CLARIFICATION

CLARIFICATION

Prepared by G R E Lionnet

Study Text 1

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North , 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright ® 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

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This text or any part thereof must not be reproduced in any form without the
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This text forms part of a sugar technology study programme. The complete list
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For availability, new study units and other information, please write to G R E Lionnet,
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 GUSH LUSH

TO DIFFUSER TO MUD MIXER

 1. INTRODUCTION

The cane juice extracted by milling or by diffusion is a turbid, Objectives

greyish/green liquid containing impurities present as insoluble,

colloidal and soluble matter. The main purpose of the general
clarification process is to produce a clear juice of the correct pH
value, free of suspended or colloidal matter; this must be done with
the minimum loss of sucrose, glucose and fructose. The efficiency of
the purification process will affect the quality of the sugar produced
and its recovery Clarification represents perhaps the only opportunity
that a process manager has of improving the cane juice.

Traditionally and universally in the cane industry, heat and lime have Heat WW lime

been at the heart of clarification, and the basic concepts have not
changed over the years. Heat and lime cause the flocculation and
coagulation of many impurities which are then separated from the
clear juice by settling. Air is an impurity in juice and must be removed
by flashing, since it will prevent proper settling of the flocculated
particles_

The use of heat and lime, followed by flashing and settling is called Dereeadon

defecation in the cane sugar industry and is found in many raw cane
sugar factories. There are other clarification processes, the most
important being sulphitation, carbonatation and phospho-defecation.
They are more costly than the simple defecation process but are
important when mill-white sugar, instead of raw sugar, is produced.
 2. THE CHEMISTRY

Clarification deals with the impurities in the juice, with the important
proviso that sucrose, fructose and glucose must not be affected.
Although the distinction may not always be clear, it is useful to divide
the impurities into those that are in suspension and those that are in
solution. Thus has been done in Table i for some important juice
constituents.

Table 1
Some constituents of juice

2.1 Sucrose

This is the most important constituent and it must not be lost. Apart
sucrose
from physical losses (spillage, overflows, etc.) sucrose can be lost
through two processes, namely by the action of microorganisms as
discussed later, and by chemical inversion. Inversion is an hydrolysis InverMon

reaction through which sucrose is broken into glucose and fructose,

the reaction being promoted by low pH values and high temperatures.
These two factors affect the rate at which sucrose inverts while the pa, um p
erst,re a,a thm
amount o£ sucrose lost depends on the time available for the reaction.
The reaction is shown chemically as

Ct2H220 iI + H2O --':* C6Hi206 + C6H,2Os

where sucrose reacts with water to form glucose and fructose. This
is probably the most important chemical property of sucrose from a
sugar technology point of view and is the reason why the pH,
temperature and residence time of solutions containing sucrose
receive much attention in sugar factories.

2.2 Fructose and glucose

Fructose and glucose are the two main other sugars in cane juice.
Reduce the sotneoky °rmrr°"
They impact in two different ways on the process. Firstly they
decrease the solubility of sucrose in water and will thus help the
recovery of sucrose by crystallisation. The natural concentration of
these two sugars must therefore be preserved. Secondly they Decompme to pmdaee coloor
decompose under the action of heat and of high alkalinity, to form
highly coloured organic compounds. Again high temperatures and pH, temperature and tit„e

high pH levels will increase the rate of the decomposition while the
amount of fructose and glucose lost will depend on the time available
for the decomposition.

2.3 Organic acids

Acidky of juke
Aconitic, oxalic, malic, tannic, citric and tartaric acids are some ofthe
organic acids found in sugar cane juice. Acidic organic phosphates are
also present. These are responsible for most of the acidity of cane
juice, which shows a pH of 5,2 to 5,5 normally.

It is generally agreed that the principal reaction of clarification by

liming is the formation ofinsoluble calcium phosphates. The minimum
effect of the organic acids is to compete for the time and increase the Aconitlc acid
amount required to reach the final clear juice pH. Trans-aconitic acid
is the most abundant organic acid in cane juice and must be the
principal competitor of phosphoric acid. Its concentration may even
be higher than that of phosphoric acid in many juices. Many of the
organic acids present in cane juice are quite strong acids when
compared to phosphoric acid, as shown by the acid ionisation
constants in Table 2.

Table 2
Acid ionisation constants (25°C) for polyprotic acids Acid ztrrnpths

ionisation constants:

Oxalic 6,5x10"' 6,1x10" 5

x, co, -1, H- + Hco;

Trans-aconitic 1,0x 10'3 6,6x10" 7.8x10-'

HCo= r H' + Co,,-

Malic 4,0x14` 7,5x10- 6 then x, = 1 IHCO - 1

[H,C0,I
Phosphoric 7,1x14" ; 6,3xi0-' 4,5x10-'3

Although the first H+ of aconitic acid is about one seventh as highly

ionised as that of phosphoric acid, the other two H' are much
stronger acids. In fact aconitic acid may be the most important buffer
present in normal cane juice and it has been suggested that it may
account for most of the lime needed for neutralisation.

Cane juice clarification does not depend only on the neutralisation of Precipitate or cakimn phosphates
the acidity of the juice. The formation of a voluminous precipitate is
essential. This precipitate is formed by the reaction between lime and
the phosphates in the juice and is believed to be an amorphous
calcium phosphate, which precipitates as octa-calcium phosphate and
hydroxyapatite. The phosphate content of the juice is an important
consideration. In cane juice phosphates are both organic and Coaceatraflon of phosphatn
inorganic, and it has been said that if the inorganic phosphate In the jdce

concentration is below about 300mg per litre of juice then

clarification will not proceed satisfactorily and phosphoric acid
should be added.

2.4 Other organic species

Pectins are gelatinous carbohydrates which can exist as colloids or as

soluble matter. They increase viscosity but are precipitated during
Pecdns
clarification. Gums is the name given to colloidal or soluble, high
molecular weight carbohydrates, which are determined analytically
by precipitation through the addition of alcohol to the juice. Some of Gtow

the gums originate from the cane plant itself, but most of the
problems caused by gums are due to those formed by microbiological
activity in the juice. These gums which include the dextrans, increase
ncrtrans
viscosity, slow the crystallisation rate of sucrose and cause crystal
deformation. Gums are only poorly removed (10 to 20%) by
defecation. Proteins originate £torn the cane plant. They are denatured Proteins
and precipitated by heat and lime.

Colour bodies include saccharetin, a yellow pigment found in the

Colour bodies
fibre, as well as chlorophyll, anthocyanins and polyphenols. Phenolic
compounds are normally present in tops, rind and younger shoots and
form dark-coloured soluble compounds when they are acted upon by
enzymes, by chemical oxidation and by reaction with iron.
Chlorophylls and other plant pigments are removed or destroyed
during clarification.

Starch is present as granules in the cold juice but is solubilised above saran
74°C. In its soluble form it is not removed by defecation. It has a
severe negative impact on sugar quality since it is incorporated into
the raw sugar crystal during crystallisation and causes serious
filtration problems in refineries using carbonatation. Its removal from
the cane juice is however relatively easy since it is degraded by the
enzyme a-amylase, commercially available in a thermally stable form
which can be added to the third effect evaporator.

Cane wax is found on the nodes of the cane stalk and in the rind. It is War
physically removed with the muds during clarification.

2.5 Heat

The heating of the juice during clarification has the following main
effects. -

• Heating the juice to 75°C and above prevents the

microbiological and enzymatic destruction of sucrose. Microbiology

• Heat causes the coagulation of some of the organic Conguladon

constituents, for example proteins and albumins, This
facilitates the removal of those impurities by the settling
process.
 Reaction rate!
• The reactions between li me and the acids in the juice have
rates which are very slow at low temperatures. Heating to
boiling and above greatly increases these rates.

• By heating to above the boiling point of the juice, flashing Flashing

can occur. This removes air as the solubility of air in water
decreases with temperature, and allows settling to take
place. A further advantage of flashing is its regulatory effect steady temperature

on the flashed juice temperature; the juice feed to the

clarifier is thus at a constant temperature and this reduces
thermal currents.

2.6 Lime

Lime is used universally in the cane sugar industry to change the pH

ofthe juice from slightly acidic to neutral/slightly alkaline. This causes
the coagulation of colloidal matter, and the time reacts with acidic main reactions of lbm
phosphates to form a heavy precipitate ofcomplex composition which
traps the coagulated impurities. This precipitate carves with it most
of the finely suspended material left in the juice. Finally, the change
of pH to neutral/slightly alkaline reduces inversion and the alkaline
degradation of the monosaccharides.

Before its addition to the juice the lime undergoes a slaking process
Mak of ume
to produce the milk of lime used in industry. The raw product
received by most factories is quicklime (CaO), which is slaked with
water at the factory. The reaction is exothermic:

CaO + H2O =~' Ca(OH)2 + 63,40

and produces calcium hydroxide (Ca(OH)z) and heat. As calcium calcium hydreAde
hydroxide is only very slightly soluble in water (I gam dissolves in
790 grams of water), it is dispersed as a fine suspension of very small
particles in water.

The quality of the lime used in the clarification process is important. Avaftbk CaO content
Its most pertinent criterion is its content of CaO which will be
available for reaction with the juice; this is normally expressed as a
percentage and should be between 80 and 90°Io. This property of the
li me should be checked regularly by analysis.

Lime may be obtained by burning limestone (CaCO 3) and coke (C) in Lhne idins
lime kilns where the following reactions take place

C + 02 =~ C02 + Heat

CaC03 + Heat ~ CaO + C02

Lime may also be obtained commercially as lumps and this is often the Qukutme dodo
case at many factories. It should be noted that CaO has a strong
amity for moisture and for carbon dioxide from the atmosphere.
Stocks should therefore be kept low and protected from the
environment.

Quick lime (CaO) is never added directly to the juice because this
would cause localised regions of extremely high pH and temperature,
as the slaking process takes place. This would cause the destruction
of fructose and glucose.

When calcium hydroxide is added to the juice, it reacts with the acidic
phosphates to form complex mixtures of calcium phosphates; it has Reacdom hctnccn dme
been suggested that tricalcium phosphate and hydroxy-apatite are and phosphates
formed:

Cal' + K2HP04 =~ Cal-W04 + 2K'

Calcium phosphates

2CaBP0 4 + Cap+ =~ Cal(P04) 2 + 2H+

3Ca3(PO4 )z + Ca(OH) x =~ 2Ca5OH(PO4)3

Dicalcium phosphate (CaB P04) is first formed and this reacts further
to form the tricalcium phosphate, liberating free hydrogen ions.
Finally the tricalcium phosphate reacts further to form hydroxy-
apatite. The rates of these reactions are greatly accelerated by heat.
It should also be noted that the formation of H' causes the pH of the
reacting medium to drop, and this is seen when the pH values of
limed and clear juices are compared.

7-
The chemical reactions shown above are obvious simplifications of SLmpitnaxnoo of reactlo=

reality; water of hydration, for example, has not been taken in

consideration. Tricalcium phosphate is often shown as
water or hydration
Ca3(PO4).nH20, indicating the uncertainty about the number of
molecules o£ water of hydration. Finally, it is certain that the situation
in impure sugar solutions must be much more complex than shown
above.

2.7 pH

The pH concept is central in the chemistry of sucrose, glucose and Importance of pH

fructose. It has been shown that it affects inversion and the
destruction of the two monosaccharides. In both cases temperature
and time play important roles, but it is not always possible to control
these two factors. Thus the need to have effective pH control.

The first factor for effective pH control is to limit fluctuations in juice

flow and in the milk of lime or saccharate concentrations. To achieve
this, sufficient buffer capacity should be provided in the juice stream Capacity and flow control

and in the lime preparation stage, before the addition point. In all
cases juice flow control should be provided to ensure that flow
variations are within the accepted limits.

Although heat greatly accelerates the reaction rates found during

li ming, it is necessary to allow a time interval between lime addition
Measurement of pH
and the actual pH measurement, at the pH electrode. At 100°C a time
interval of 3 to 4 seconds is required, Generally the limed juice ofd
take, to the electrode, should be about 8m downstream of the point
of lime addition.

In chemical terms, pH is a complex concept but it is important to

understand it. It is possible to make simplifying assumptions to help pH

in the understanding, as will be done here.

Water has the ability to behave both as an acid and as a base. The
chemical reaction describing this is:-

H20 + H2O ~ H 30 . + OR
Equilibrium in water

where one water molecule is considered to be the acid, donating a

proton to the other, the base. The process is chemically reversible and
the equilibrium position is very much to the left.
At 25°C and after making some simplifying assumptions, the product
of the concentrations of H3 0* and OH- , which is called K„, is found
to be equal to 1x10"'.Thus, in an aqueous system at 25°C, if the
value of either the concentration of H3O+ or that of OH" is known, the
other can be calculated, since
,
Kw = [ H30 ] x [OH"] = 1 x 10-14

The concentration of H30' can vary over a considerable range and,

in order to avoid cumbersome numbers such as 10" and 10 -4 , a
logarithmic scale is used, where

pH ^ -log, o[H30 j
DetiddoR of pH

thus if the concentration of H 30- is 10 -'moles per litre, the pH is u UH,o-1 - W moi"A
given by -loglo (10') or 4.
Own pH --lap,j1V`I-4

1t is also noted that, from the above,

pH+pOH= 14
At 250C.-
where pOH is the same concept as pH, but applies to the OH'
pH + poll - 14
concentration rather than to the H 30' concentration. This means that
pH and pOH can have any value, but their sum must be 14, at 25°C.

.
At 25°C, since [H30 ] and [OH- ] are equal because o£ the electrical
neutrality of water, and Ka. is equal to 1x10", then

[H30'] = [OH"] = V 1 x 10' 14

that is [ H30'] = [OH"] = 1x10''

pH - poll - 7
or pH = POH = 7

This value corresponds to neutrality, in the acid/base sense, at 25°C.

Since pH represents a concentration, resulting from an equilibrium

which is influenced by temperature, it is expected that pH will change Effect of temperature on p1i

as the temperature changes. This is found to be the case. At 45°C

1,„ is now equal to 4,02x10-14. Then pH is equal to 6,70 which
corresponds to neutrality at 45°C.

At 25°C, the pH of acidic solutions is less than 7, while that of basic

solutions is greater than 7.

2.8 Sulphitation, carbonatation and phospbodefecation

These three clarification systems have been and are still used in cane
sugar factories, particularly when producing "mill white" sugar. The
main reactions are:-

Ca(OH) 2 + 50i =* CaS03 1 +H20

Ca(OH)2 + C0 2 =~ CaC03 l + H2O

Ca(0H)2 + H3P04 ~--* Various calcium phosphates 1

3. THE MICROBIOLOGY

Cane and cane juices always contain microorganisms which consume

sucrose. The measures taken in the factory to control the activity of
microorganisms depend on wether the extraction plant consist of
milling or of diffusion. If diffusion is used then the shredded cane is
in contact with scalding juice (90°C) as it enters the diffuser and
temperatures throughout the extraction plant should be above 75°C.
The mixed juice temperature should also be high and microorganisms
should not be a problem. llewatering mills and equipment treating
press water must however be monitored carefully.

The situation is different with milling. Although high temperatures

favour extraction by denaturing the cell walls, caution is necessary
with milling because of cane wax. Temperatures above about 66°C
cause the wax to melt and this results in slippage and feeding
problems at the mills. The tendency is therefore not to use hot
(>75°C) water for imbibition and thus temperatures across the mills
may favour microbial activity. Mixed juice temperatures are relatively
low (50-60°C) and the juice must be sent to the heaters as quickly as

- 1 0-
possible. Heavy microbial infestations are possible in the extraction nrin aanitntion
plant and mill sanitation is required. This involves the use of hot water
or steam for regular cleaning of miUs, gutters, screens, etc., and, if
necessary, the application of bactericides. Juice screens are notorious
for harbouring microorganisms, particularly leuconostoc species.

Long retention of juice in vessels where soil/sand can be deposited

must be avoided. These systems respond poorly to heat or
bactericides and the soillsand act as continuous sources of
microorganisms. Sucrose losses will then be unavoidable. Apart from
direct losses of sucrose, the microbial activity results in the formation
of many byproducts, such as polysaccharides, acids, etc., which are
known to be detrimental to downstream processes.

A useful technique to measure microbiological activity is to analyse

I Acdc acid In mixed juice
the mixed juice for lactic acid, a byproduct of sucrose degrading
bacteria. A concentration of lactic acid above 40Omglkg of brix is
regarded as the limit that can be tolerated. If the concentration is
higher then sanitation steps must be taken, after ensuring that the acid
did not enter the extraction plant with the cane.

Microbiological activity can also be found in clarifiers, in mud

compartments. Mud, sand, soil, etc., can compact in stagnant zones,
cool and provide regions where microbial activity can take place.
Lactic acid can again be used to test for this. An example of lactic Lactic acid snerey
acid concentrations is shown in Table 3.

Table 3
Lactic acid concentrations
The results shown in Table 3 indicate no problems at the extraction
stage but severe microbiological activity in the mud and in the filter
station.

4. THE MACHINERY

4.1 Screens

A common type of static screen in the cane industry is the DSM DSM screens

(Dutch State Mine) screen. It is fed over a weir box, tangentially

downwards, onto a curved screen. The screen itself is of the wedge
wire type, the horizontal wires being wedged shaped in section, the
broad edge of the wedge facing the inlet of the screen. The screen
aperture varies from 0,5mm to 1 mrn, with 0,75mm being a common
size. The screen area required has been found by experience to be
about 0,1 m2 per ton cane per hour, in the South African industry. The
distribution of the juice across the width of the DSM screen is very
important. The best method appears to be a fan shaped trough above
the screen, followed by a large radius sill on the weir feeding the
screen. Frequent cleaning of the weir is necessary.

Another type of screen which is used in the cane industry is the rotary Rotary screens
screen. This is a cylindrical drum which rotates on its axis. Juice is fed
i nto one end over a small weir, so that it meets the screen as
tangentially as possible. The fibre is carried out to the outlet by means
of flow diverters.

Finally, vibratory screens are also used, but are now fairly rare.

4.2 Juice heaters

There are basically three types of juice heaters which are fairly Tube and plate

common. The first, and the most common, is the shell and tube,
horizontal or vertical, juice heater. It consists of a cylindrical vessel
with tube bundles inside, with tube plates at each ends. A tube
diameter of 38mm and length of 3 to 5m are common. At each end,
baffles are arranged so that the juice circulates through a number of

- 12-
passes in succession. The juice flows inside the tubes while the
heating medium is outside the tubes. Incondensible gas vents,
condensate outlets, main doors at both sides and temperature gauges
are some of the requirements. The juice velocity ranges from 1,5 to
2,2m/s and the vapour velocity is about 30m/s. The juice side of the
tubes needs regular cleaning, which can be either mechanical or
chemical.

The second type is the plate juice heater. This consists of a pack of Plate juice heater
corrugated metal plates with ports for the passage of fluids; special
gaskets seal the plates. The juice and vapour move in a counter
current way. They have been used for both mixed and clear juice and
can show high heat transfer coefficients. Choking by fibre can
however be a serious problem. The "wide-gap" plate heat exchanger
is becoming popular, with a juice side gap of about l2mm. Heat
transfer is claimed to be high.

A newcomer in the cane sugar industry is the platular, all welded, Platular heater
gasket free heat exchanger. It offers a choice of plates gaps widths of
S to 40mm, with 18mm having been used successfully, Cleaning must
be by chemical means.

4.3 Liming equipment

The most common method for mills of lime preparation is to slake

rock-lime with water. Some factories operate lime kilns while others
have replaced rock lime with powdered lime. A typical lime plant is
shown schematically below.

H(7L FAUM FA[7URV

r A lime giant
wu
SFuR.U3E

nrsrPmllnox
01

MUS,
F~
D-FACFURI' T

-13-
Milk of lime or saccharate, which will be discussed later, can be
added to the juice either in special liming tanks, sometimes called
Sufic mizers
Perry tanks, or through the use of static in-line mixers. The latter is
the more modern option, and is in the form of a U-leg installed
between the final juice heater and the flash tank. Static mixers are
commercially available and create high turbulence and effective
mixing. NEW of lime is pumped in at about one metre ahead o f t h e
mixer using a variable speed dosing pump. The limed juice sample for
the pH control is then situated about lm after the static mixer. The
mixer needs to be cleaned regularly.

4.4 Flash tanks

Unless juice is flashed properly, air bubbles will be released in the

clarifier thus negatively affecting settling. Lamusse (1977) gives
sizing
formulae to size flash tanks, so that flashing takes place effectively at
atmospheric pressure without entrainment ofjuice. The area, A, (m)
required is given by

Area

4,186W (I; -- T2
A
L

and the vent pipe diameter, D, (mm) is given by

i"
n,183W(TI - T2 )V Vent diameter

D = 1D~~
L

where W is the mass of juice in tons per hour, T, and T 2 are the juice
inlet and flashing temperatures, in °C, respectively, L is the latent heat
of steam in kcal per kg and V is the specific volume of steam at T 2,
in in' per kg.

4.5 Clarifiers

The floc is separated from the juice by settling in special vessels called
clarifiers. Settling theory shows that the settling rate of particles

- 1 4-
depends on three factors: the densities of the particle and of the
Factors affecting the settling rate
liquid, the size, shape and diameter of the particles, and finally the
viscosity of the liquid. Not much can be done about the density and
viscosity of the juice, since these are controlled by the addition of
water at the extraction plant. Thus only the size/shape ofthe particles
can be controlled and this highlights the need to avoid all damage to
the floc.

In studies on the area required for the settling of cane mud particles Thickening versus settling
it was found that the area for mud thickening was half that required
for settling the mud; this is the basis for the Rapi-Doer design which
provides one mud thickening compartment for two juice trays.

The clarifiers found in the cane industry are generally the Dorr type Types of clarifiers
and the trayless clarifiers designed by the Sugar Research Institute of
Queensland, in Australia- The Rapi-Dory is operated on the counter- Rapi-Dory
flow principle- The juice is admitted at the top centre and moves out
towards the periphery where it is extracted at the point of lowest
velocity. The separated mud is collected on the trays and is scraped
until it falls into a thickening chamber where it compacts before being
withdrawn. Many modifications have been carried out to optimise the
operation ofthese clarifiers and to increase their capacity. The use of
flocculants has contributed greatly but it is still felt that progress is
possible, particularly in terms of capacity, thus reducing the retention
time. A schematic representation of a Rapi-Dory is shown below.

. - L04M n tct

Schematic diagram of a Rapi-Dory

rawr
 Mer
Work carried out in Australia, particularly by D J Hale and E The trayle' cI
The need for process control
Whayman, showed that solid-liquid separations and thickening
achieved in a pilot plant, trayless, clarifier were far greater than those AAvautageo of the uAyless cWrider
acheived in commercial units. It became apparent that, in spite ofthe
many trays available in commercial clarifiers, these could not reach
the loadings obtained with the simple pilot plant design. A full scale
trayless clarifier was designed and tested in 1959, and proved highly
successful. The design involved the minimisation of cross flows. The
clarifier is made up of a cylindrical tank in which circumferential
launders are fitted. The feed well extends downwards for about lm.
Beneath the feed well there is a deflector plate that directs the
descending juice towards the centre and the periphery. A zone of
separation is established in which the clear juice travels up to the
outlets and the solids to the bottom. The basic design of the clarifier
is to minimise cross flow and to approach a vertical upward path for
juice and a downward one for mud. The muds are continuously
removed from the slopping bottom compartment.

The short residence time clarifier requires good process control for
satisfactory operation. Juice flow control, constant liquid temperature
and brix, and the use of flocculants are essential. The main advantage
of the clarifier are the smaller volume of material they contain, which
facilitates liquidation procedures and reduces sucrose losses. The
simpler less cluttered design is better suited to plug flow and prevents
the accumulation of muds in stagnant pockets. A schematic diagram
is shown below. Schematic diagram of the short
residence time ctarifler

u
cum
 5. THE TECHNOLOGY

5.1 Screening

Raw juice from milling tandems contains a considerable amount of Fibre in juice from mills
suspended matter, mostly fibrous material. These cause many
problems in the downstream processes; they choke scales, pumps and
heaters; they overload flash tanks, clarifiers and filtration equipment;
they form colour and increase the concentration of soluble silica at
high pH values. Without screening it is possible for fine fibre to be
found in the clear juice; this may then require the screening of this
material. The amount of fine fibre particles may be a function of the
pith to hard fibre ratio of the cane, which itself depends on the
variety, the growing conditions and other agronomic factors. The
suspended matter must be screened out of the raw juice, and is
returned to the mill, usually in a flume using recirculating juice. It is
normally returned to the bagasse leaving the first mill.

It has been found that juice leaving a cane diffuser is already

Fibre in juice [ram difmrs
effectively strained by the bagasse blanket in the diffuser, and further
screen may not be necessary. In South Africa all the milling tandems
screen the juice; five factories with diffusers do not screen the juice
but four others do. In the same country, mixed juice from milling
tandems has been found to contain about 1% of suspended matter;
juice from diffusers show only about 0,3%. Fine fibre present in clear
juice will finally find its way into the raw sugar where it can cause
deterioration problems. Again it can get caught by the backing
screens of the batch A-centrifugals, reducing molasses drainage.

Conventional juice screening has little effect on the soillsand content loll in juice from mills
of juice. With a milling tandem the soil remains in the juice and is
finally removed with the filter cake. Some soil inevitably settles out
in tanks, whenever the velocity is low. This soil must be physically
removed. Soil removal systems have been proposed but these always
increase the retention time ofthe juice and will result in sucrose losses
from microbiological activity. Trials with hydrocyclones have been
done but with very limited success. The separation was poor and the
underflow still needed further treatment in order to reduce sucrose
l osses.

In the case of diffusion most of the soil stays with the bagasse and
ends up in the boiler. Ash in bagasse ranges from 1 to 2% in milling swiainainier bagasse
tandems but reaches 3% and more in diffuser bagasse. At levels above

-17-
5°/n bagasse does not burn well and fires may be put out. Sand and
soil in bagasse cause severe erosion problems with fans, tubes, ducts,
etc.

5.2 Juice now control

In order to obtain effective pH and temperature control it is essential

to limit fluctuations in juice flow. Control of steam and of milk of lime The effects of Ruchutions
to Juice [law
will generally be unable to cope with large fluctuations in demand.
These will therefore inevitably result in temperature and pH variations
which are unacceptable as far as the clarification process is
concerned.

Variations in juice flow also affect the clarifier in another way. They
cause physical flow disturbances in the vessel and mud is entrained
with the clear juice, a result called carryover. This problem is more
severe in short residence time clarifiers which contain relatively
Carryover
smaller volumes of juice and are thus more susceptible to flow
disturbances.

Diffusers, because of their dependence on percolation rates and the

fact that they hold a large amount of fibre, can cause large
fluctuations in juice flow, as cane quality changes.

Juice flow control in a modern factory is essential. Various systems

are available and are normally installed at the mixed juice tank, after
the scales. Some of the common systems include flow control itself,
gap action controllers and cascade control. A schematic juice flow
control system is shown below.

Mncr n iun - P

schematic diagram of a
Row coat" system

TO PROCFSS

l8
_
5.3 Juice heating

Efficient juice heaters must be able to raise the temperature of the

incoming juice to the required level. Temperature gauges are essential
on both the inlet and outlet streams. In many cases heating is done in
two stages, a primary one using vapour 2 and a secondary one with
vapour 1.

Although there is no concentration effect, that is water is not

evaporated during juice heating and thus there is no increase in the
concentrations ofthe soluble solids, scale is formed in the tubes. This
Sc9i" of heaters
is due to the effect of heat on some of the organic species and to
changes in solubilities as temperature rises. The scale reduces the heat
transfer considerably and has to be removed, by regular cleaning. This
can be done mechanically or chemically.

Mechanical cleaning for tube heaters involves the use of rotating

brushes/cleaning heads. Chemical cleaning maybe done by circulating
a solution of sodium hydroxide (caustic soda) through the units, at cog
about 8U°C. The time and concentration cycles depend on local
conditions, mainly the scale composition, which however is less
variable than that found in the evaporators. Often the solution used
can be that left from the cleaning of the evaporators.

Plate and platular juice heaters cannot usually be cleaned

mechanically and chemical cleaning must be used. This requires care
with respect to the concentration, temperature, retention times and
complete plate coverage. Final washes with water are required. It
should be noted that the disposal of spent sodium hydroxide solutions
can be an environmental problem.

5.4 Liming

Whatever the clarification process used, lime is the main clarifying

agent; it was first mentioned as a defecant in 1585, The addition of
lime to juice is done either as calcium hydroxide in milk of lime or as
lime saccharate.

Milk of lime is a slurry of calcium hydroxide in water. The

concentration of lime is often expressed in degrees BeaumeBaurne,
on old (1870 and earlier) scale for the concentration of dissolved
solids. The term is still used extensively for milk of lime. Table 4 Beams

gives data relevant to the Beaume scale.

_1g_
 Table 4
Degrees Beaume and more usual concentration units

4 1,029 36 3,50

10 1,075 94 8,74
15 1,116 148 13,26
20 1,162 206 17,72

Since milk of lime is a slurry it must be kept in motion to prevent

settling and choking of equipment.

Calcium hydroxide and sucrose react in aqueous solution to form

mono-, di-, and tri-calciurn saccharates, depending on the conditions
under which the reaction takes place. For mixed juice liming it is the
most soluble, namely the mono-calcium saccharate, which is Cddam Wcharates
required. It is formed according to the reaction

C12H220ii + Ca(DH)2 r Cr2HzODi 1Ca + 2H20

The two reaction conditions that are required to produce the mono-
calcium saccharate are an excess of sucrose and a temperature below
58°C. In practice the required ratio of sucrose to calcium oxide is 7:1
and is obtained by using evaporator syrup (68 brix) and 15Beaume Preparation ofsnccharate
milk oflime. The pH value ofthe resulting saccharate is between 11,0
and 11,2. Practically the saccharate formation may be controlled by
using the pH, ensuring a value of 11,0,

The advantages of saccharate liming are stated to be the use of a

soluble liming agent, which does not settle in equipment. It may be
left standing during week-end shut downs, and is immediately
available on start up. The use of saccharate is seen as resulting in aav=fta and d6"ra"gp

much lower turbidity in clear juice when compared to the result with
milk of lime. This has been a major claim as to the superiority of
saccharate. It has been shown however that the lower turbidity may
not necessarily persist in syrup and in sugar. It has also been well
established that saccharate liming causes the muds to be lighter and

-20-
more voluminous. Finally the use of a sucrose stream, usually syrup,
to prepare it means that a significant quantity of sucrose needs to be
recirculated. Furthermore most or all the monosaccharides in the
stream will be destroyed at the high pH. This is the reason for lime
saccharate solution to be wine red in colour.

Saccharate liming is used extensively in many cane sugar producing

countries but this is not so in South Africa. A schematic arrangement
for its preparation is shown below.

Plant for preparing saccharate

~CUON r~

940L swum

79LV~Q

Australian workers have shown that sucrose was not lost when
saccharate is prepared. Both fructose and glucose, as expected, were
lost, and a number of organic acids, including lactic acid, showed
i ncreases in concentration. Increasing either the temperature or the
concentration of the lime resulted in more acid being formed.

Milk of lime or saccharate may be introduced in the juice stream

-21-
either before or after the flash tank. When the point of addition is Point of addition

before the flash tank, an in-line mixer is usually installed after the
input point. If added after the flash tank the application is done in a
special tank normally called the "Terry" tank. Liming can also be done
in the flash tank itself.

5.5 Flashing

Juice must be heated to a temperature higher than its local boiling

point. A practical point of relevance here is that if the last heater is
situated far from the flash tank, it is the temperature at the flash tank,
not at the heater outlet, which is important. Furthermore if milk of
Tetaperatan for flub g
lime is added before the flash tank, a similar comment about
temperature must be made. It may then be necessary to heat the juice
somewhat more to compensate for any cooling. A similar situation
arises if filtrate from the mud filters is returned after the juice heaters.

The purpose of flashing is to force out the air present in the juice, to
cause the bagacillo particles to burst and then sink with the floc, and
to ensure constant flashed juice temperature. A practical check on
flashing is to observe the vapour coming out of the flash tank vent; if
there is little or no vapour then flashing is not taking place.

5.6 Flocculants

A number of synthetic water soluble polymers, bearing various trade

names, have come into general factory use. The action of these
polyelectrolytes is to produce a secondary flocculation. Generally a
good flocculant should improve flocculation, increase settling rate,
Properdea of ROCCUIMts
reduce mud volumes, and most importantly, increase the clarity ofthe
clear juice. It is normally found that a flocculant which is particularly
efficient as far as increasing the settling rate is concerned, will be less
efficient in terms of juice clarity, and vice versa. Some compromise
is necessary.

The most successful flocculating materials for the raw sugar industry
are the partially hydrolysed polyacrylamides, shown below.

_22-
The molecule is a combination of acrylamide and sodium acrylate, and
an important property is its degree of hydrolysis given by the ratio
IOOYI(X+Y), as a percentage, where X and Y are the mass
percentages of the two components. crst~x cell c r
I
CONHZ COo- Hi
Studies in Australia have shown that the mud particles attach
themselves to the active sites of the long chain polymer and form a
floc structure. These two processes are shown schematically below.

Mud particle attached to

Rocculant chain

MUD PARTICLE

Build up of ft" erucdtre

Polymers vary in their degree of hydrolysis and as far as their

molecular weight is concerned. The properties of the floc vary
according to cane quality, local conditions and probably because of
many other factors. Thus it is impossible to predict the best flocculant
for a particular application. The traditional approach has been to test

-23-
a number of flocculants on site, using a settling kit.

The preparation of flocculant solutions requires great care if the rnparanoo of floccuLmt sohalon
maximum benefits are to be obtained. Two tanks should be used, one
for adding and dispersing the flocculant, usually in powder form, and
the other for aging the solution, Fibreglass or stainless steel are
recommended since flocculants can attack iron and cause it to be
present in the solution. A clean, suspended matter free, water must be
used, at a temperature below 55°C. It has been suggested that the pH
of the water should be about 9. The powder is usually dispersed by
means of an eductor or it may be added in a spray of water. A slow
speed paddle should be used for mixing; air sparging is not
recommended since small air bubbles may be trapped into the viscous
liquid and thus enter the flashed juice. The solution should be allowed
to stand for about two hours to allow complete hydration of the
polymer. Addition into the juice requires attention. Although good
mixing with the juice is necessary, excessive turbulence will destroy
the polymer chains. A low shear dosing pump may be used and
piping should not have sharp bends or restrictions.

5.7 Settling

The complex precipitate is separated from the juice by settling in

special vessels called clarifiers. The theory of settling shows that the
settling rate of particles depends on the densities ofthe liquid and that
of the particle, the physical characteristics of the particles, namely
their shape, size, etc., and the viscosity of the liquid. The settling rate
may be measured as a velocity, V, which can be calculated for
spherical particles as

D2 (d, - d2 )g
Y=
18U

where V is the settling velocity in cm/s, D the diameter of the

particles in crn, g the gravity constant in cm/s', d, and d 2 the densities
of the particle and of the liquid respectively and U the viscosity ofthe
liquid in poises. The importance of the particle size and of the

_2q_
differences in density are clearly apparent. The density of the liquid is
really a function ofthe amount ofimbibition water added. The density
of the particles will vary with their size and it is thus important to
avoid damage to the floc formed after liming and conditioned by the
use of flocculants.

Settling rates in the cane sugar industry have been measured by using
settling kits, as shown.

Sea" rat

settling curve

The level of the mud interface is recorded at different times, as it falls

through the juice, to produce a settling curve. This technique has
been used extensively to study the effect of different flocculants, of
different liming procedures, etc. It is also possible to use the curve to
calculate various parameters such as the initial settling rate and the
final mud volume, which characterise the type of settling.

5.8 Other clarification processes

Carbonic acid, sulphurous acid and phosphates have been used in the
cane sugar industry since 1843. The juice sulphitation process is still
Sulphludon
used in Colombia, India and Pakistan, for example, to produce mill
white sugar. It was used in South Africa, prior to the introduction of
simple lime defecation, in the nvd 1960's. The main reaction is the
formation ofa calcium sulphite precipitate. The reaction is carried out
at 70°C to minimise the post-precipitation of calcium sulphite which
would cause a high level of scaling in the evaporators. Juice is limed
to a pH not exceeding 7,5 with simultaneous gassing, using SD z, to
a pH of 7,2, in a sulphur tower. Sulphur is burned in a sulphur burner

_2$_
with a controlled amount of dry air, at a temperature of about 250°C,
when the minimum amount of sulphur trioxide is formed. The
presence of S0 3 is undesirable as it dissolves in the juice to form
calcium sulphate, which increases evaporator scaling and gives poor
quality massecuites. It can also form the highly corrosive sulphuric
acid.

The increase in scaling in juice heaters and in the evaporators, due in

a large part to poor pH control during sulphitation, led to the
replacement of this process by a simple lime defecation.

Recently, liquid sulphur dioxide has been made available LAq,dd sulphur dloslde
commercially, at costs which are competitive with those of burning
elemental sulphur. Finally, commercially available solutions of Ammoninm b.olphMe
ammonium bisulphite, containing 40-50°/o available S02 have also
been considered as a source of sulphur dioxide.

Raw juice carbonatation seems to have been introduced in the cane

Carbonatadou
sugar industry in lava, around 1880, where it was standard practice
for many years. Outside Java, it was not utilised much, but as a
refining process it is very important.

Finally, although phosphoric acid is added to juices which clarify

poorly, the phosphodefecation process is not normally used in raw
juice processing. As is the case with sulphitation and carbonatation,
it is an important refining process.

5.9 Syrup clarification

Clarification of evaporator syrup by settling is not possible because

of its high density and viscosity. Flotation clarification however, is
well established in sugar refining. Rein et al., in 1972, developed a
successful syrup clarification process and most of the information
given here is based on this work and on subsequent results in South
African factories using the process and producing raw sugar of the
very high pol (VHP) type.

Extensive laboratory work showed that the addition of phosphoric

acid and of lime did not improve the removal of impurities or of smP thnifeffoa
colour, and actually gave worse turbidity removals. A simple
conditions
clarification, involving the addition of heat, air and polyelectrolyte,
was found to be the optimum process. The flocculant dosage was
found to be about 10 to 15mglkg brix; a polyelectrolyte with a higher

_26_
degree of hydrolysis did improve the turbidity removal. Temperature
was found to have a significant effect on turbidity removal and 85°C
is recommended. Retention time was found to be optimum at 1 0 to
15 minutes. Finally turbidity removal was found to be independent of
syrup brix and viscosity.

A simple syrup aeration procedure, classified as dispersed air Arratlon

flotation, was used. Air is injected into the suction of a pump
operating at high speed.

A schematic diagram is shown below.

Syrup clarl&r

AIR FLOCCULAI+IT

As usual in clarification processes, flow variations and disturbances

must be avoided. Syrup clarification has been found to result in
turbidity removals of 65 to 70%. Sugar quality was improved, with
colour, gums and ash being reduced. Massecuite viscosities were also
found to be lower. It is also expected that the process will remove
bagacillo, if it is present in the syrup.

_27_
 BIBLIOGRAPHY

Currie A F (1986), The use of a wide gap plate juice exchanger on mixed juice heating. S Afr Sug
Technol Assoc 60, 37-39.

Hale D J and Whayman E (1972). Juice flow control. Proc Queensland Soc Sug Cane Technol, 39,
293-302.

Hale D J and Whayman E (1972), Developments in clarifier design. Int Sug J, 74,6-10,40-45,72-75.

Hartman E M (1974). The calcium saccharate process. Sugar Technology Review 2, (3), 213-252.

Koster K, Vermeulen P L M, Getaz M A and Lionnet G R E (1992). Some notes on abnormal

processing difficulties during spring. S Afr Sug Technol Assoc 66, 127-130.

Lionnet G R E and Ravno A B (1976). Flocculant assessment using a portable batch settling kit.
S Afr Sug Technol Assoc 50, 176-177.

MacNaughton M (1995). The use of powdered lime at Maidstone. S Aft Sug Technol Assoc 69,173-
176.

Meadows D M (1996). Raw juice flow control, screening, heating and liming. S Afr Sug Technol
Assoc 70, 272-276.

Munsamy S (1982). Assessment of a plate heat exchanger on process juice heating, S Afr Sug
Technol Assoc 56, 41- 43.

MurrayJ P and Shephard G S (1975). Some aspects of flocculant use in clarification and filtration.
S Aft Sug Technot Assoc 49, 53-59.

North-Coombes S, Taylor K and Koster K C (1981). The practical development and application of
saccharate liming at the Pongola sugar mill. S Afr Sug Technol Assoc 54, 71-74.

Rein P W, Cox M G S, and Montocchio G (1987). Syrup clarification in raw sugar mills. S Afr Sug
Technol Assoc 61, 22-31.

Scott R P (1988). Modifications to and experiences with Rapidorr clarifiers including saccharate
liming at Amatikulu. S Afr Sug Technot Assoc 62, 32-35.

Simpson R (1996). The chemistry of clarification. S Aft Sug Technol Assoc 70, 267-271.

Whayman E and Crees G L (1974). Mechanistic studies on cane mud flocculation. Proc Int Soc Sug
Cane Technol Ass 15, 1175-1182.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control

In preparation:-

Evaporation
Diffusion
Crystallisation
Pan boiling
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
CANE AND JUICE
 Sugar Technology For Students

CHEMISTRY OF CANE AND JUICES

Prepared by G R E Lior2rrei

Study Text 3

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright 0 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-23543-8

This text or any part thereof must not be reproduced in any farm without the
written permission of the publisher.

This text forms part of a sugar technology study progranune. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 UNTRODUCTION

Sugar cane is a giant grass of the genus Saccharum, which is thought o

to have evolved in the Burma/ChinalIndia region of Asia. The cane
then spread to other areas, with S. Offacinarum evolving in the New
Guinea region. The accepted view is that S Offrcinarum was
developed through selection by aboriginals to yield a sweet, soft and
juicy cane propagated for chewing.

The earliest record dealing with sugar cane in the Hindu literature is Hhtory
about 3000 years old and crude sugar was developed by 400BC.
Sugar was introduced in Egypt by 710AD, where clarification,
crystallisation and refuting were developed. Sugar cane reached
Madeira in 1420 and Columbus introduced it to the New World in
1493. During the 1500's it reached Mexico and Brazil, and in the
1700's it arrived in Mauritius, Reunion and Hawaii. Finally it reached
Australia, Fiji and South Africa in the 1800's.

The success of sugar cane in apiculture is due to the development of

new cane varieties. Different varieties were distributed from the
Indian sub-continent to the West, and from Polynesia to Mauritius
and the West Indies. A variety called Otaheit caused a revolution in
sugar cane agriculture and made sugar production the driving force
in tropical America. Cane breeding, in research institutions, was
started on a scientific basis in Java and Barbados, over the period
1880 to 1889. This resulted in many commercially successful varieties
and breeding stations developed around the world.

In South Africa, the South African Experiment Station started its Hr"akg
breeding programme in 1925. Many world wide successes have been
achieved and it has been stated that no imported variety has yielded
more than 90% of the South African bred NCo376 variety. In 1992
monetary terms the 10% advantage given by NCo376 was worth
about two hundred million rand per annum. Newer and better
varieties, such as NI2, give particular benefits estimated at 17m rand
per annum.
 ITHE CANE

2.1 The stalk

The clean cane stalk consists oflong internodes, with soft centres and
an external hard rind, with nodes in between. The ideal material that
the miller would like to receive is the clean stalk, namely that part of
the plant above the root level to below the immature top, with all
materials which are not part of the stalk removed during the
harvesting process.

The eane stalk

WP
Industrially the cane consists of varying quantities of non-stalk
materials, of which the immature taps and the trash (green or dead) rnawaw CMMOM
form the major part. When dealing with the composition of cane it is
therefore necessary to consider not only the stalk itself but also tops
and trash.

Apart from the extraneous matter content, the composition of the Fnetora whieh influence can
cane depends on many other factors. Cane variety, the region where 4uWky

it is grown, climatic conditions, agricultural practices such as

fertilisation, irrigation, burning or trashing, the use of ripeners, etc.,
the degree of maturity, and pests and diseases will all influence the
quality of the cane. In South Africa the cane contains about 13 °Io
sucrose, 15% fibre and 69°/o moisture. The other constituents of cane
are the monosaccharides, inorganic materials, for example potassium
salts, nitrogenous substances, gums, waxes, organic acids and other
organic species such as phenolic compounds which are associated
with colour.

Work done in South Africa showed that the region where the cane Impuritiea hm cape
grows and its variety have important effects on its colour and the
levels of soluble ash, silica and phosphate in the cane. The effects
were quite significant, the concentration of impurity more than
doubling in some cases. Colour, because of its impact on sugar
quality, has been well investigated. Time of harvest and variety
showed clear effects, with differences of up to 3d°Io. The different
constituents of the cane have marked effects on colour. Some results
are shown in Table 1.

Table 1

Colour in various parts of the stalk

Colour
Finally, it can be shown that cane variety and physical parameters
such as stalk thickness associated with it, can impact on extraction at
the mills. In South Africa for example it could be shown that N24 and
N21 behaved differently with respect to the extraction of brix in a
cane press.

2.2Vegetable extraneous matter

Trash in cane can be defined as all leaves, dead or green, attached or Definitions
free, including sheaths, found with the cane below the natural Tmh

breaking point of the stalk.

Tops are defined as that portion of the stalk above the natural Tops
breaking point of the stalk.

The natural breaking point of the stalk is that point where the stalk Nab" brraWng pob!
will break, fairly easily, when bent manually. Generally it is
surprisingly consistent, being located at the base of the 5' or b' fully
opened green leaf, counting from the top of the stalk.

The impact of tops and trash on cane quality must not be Tops and fruh in cane
underestimated. Measurements made in South Africa have shown
levels of 2 and 5% (mass/mass) in manually cut, wholestalk cane. On
an annual crop of say 20 million tons of cane, this represents 440 000
and 1 000 000 tons of tops and trash respectively.

The main factors which influence the contents of tops and trash in
cane are the harvesting practices and the cane itself Burning for
example will reduce the trash content, and different mechanical
harvesting techniques will impact on tops and trash.

Representative analyses of the clean stalk, immature tops and trash

are given in Table 2.
 Table 2

Analyses of clean stalks, tops and trash

ana]ysls of tops sad trash
Brix (0/0) purity Fibre ("tn) ..,

Clean stalk 15-17 86-89 12-13

Tops 6-9 21-37 12-17

Trash 7-9 -28 49 -59

L19

Apart from the low quality of tops and trash in terms of sucrose
content, these materials contain much ash and colour. Thus the
addition of 15% trash by mass to cane increases the colour by about
50%.

2.3Fibre

By definition, the dry insoluble matter in cane is called fibre. It should Definition
be noted that, according to this definition, cane consists of brix, Flhre

moisture and fibre. Cane fibre essentially consists oftwo constituents,

pith and hard fibre. The pith exists as relatively small, fluffy particles pith
Hard fibre
while the hard fibre tends to be long and stringy. An analytical
method has been developed to analyse cane fibre for its pith to hard
fibre ratio.

Although fibre tends to be seen as chemically inert, this is not the

chemlral Lapact of fibre
case. The hemicellulose in fibre reacts with lime to form acetic acid
and this can be a problem in diffusion, if local over liming takes
place; the acetic acid causes severe corrosion problems later in the
process. Silica is associated to cane fibre, from which it can be
leached, particularly if the pH is alkaline. Silica can cause severe
scaling problems in evaporators. Finally fibre contains a dye called
saccharetin, which turns yellow when in contact with lime, this can
therefore add colour to the juice.

Pith can also cause processing problems. Since it is light, it does not processing problems w'Nh pith
settle well, efficient flashing is required to remove the air trapped
inside it. The pith content of cane seems to be high when tropical
climatic conditions exist and the cane grows rapidly, to produce thick
and soft stalks. Under those conditions it is often necessary to sieve
clear juice, thus removing large quantities of pith. Pith left in juice
will find its way in A-massecuite. This will cause two problems.
Firstly, it will accumulate inside the backing screens of the
centrifugals, reducing the flow of molasses. The screens will therefore
need cleaning. Secondly, some of the pith will remain with the sugar.
Drying will be impaired and sugar quality will be affected, sometimes
seriously. In South Africa, syrup clarifiers have been found to remove
pith from the syrup.

In the cane industry, fibre, in the form of bagasse, is valuable as fuel

for the factory. The amount of fibre brought into the mill can be
greatly increased by including tops, and more particularly trash, in the
cane. This allows more electricity than used in the factory, to be
produced and made available for the grid. This process is called
cogeneration and is important in countries which do not have fossil
fuels. Bagasse can also be used for by-products such as paper,
particle board, cattle feed or chemicals such as furfural. Tests done
i n South Africa have shown that, if the extraneous matter goes with
the cane through the extraction plant, juice quality is reduced to an
extent where the present South African sugar quality standards
cannot be met. It should also be noted that the inclusion of the
extraneous matter with the cane reduces transport payloads. The
trend in a number of countries is to dry clean the cane before the
extraction plant, routing the tops and trash directly to the boilers.
 MHE JUICE

Cane juice is a foaming turbid liquid, ranging in colour from light Juice
grey to dark green. It is acidic and, because of its colloidal matter
content, it doe not filter well.

Cane juice, as extracted by milling or by diffusion, contains materials In Solution

in solution and in suspension. Although the distinction is not always
very clear, these will be considered in turn. The materials in solution
include sugars, mainly sucrose, glucose and fructose, which will be
considered in detail later; inorganic salts and acids; proteins; gums
and other polysaccharides; colour bodies and minor constituents.

In suspension one finds fibre and pith, sand and soil, clay, In X"Penflon
chlorophyll , waxes and air. A summary of this basic juice
composition is shown in Table 3.

Table 3

Some constituents of juice

3.1 Sucrose, glucose and fructose

Sucrose is obviously the major component present in the juice. The

three sugars account for SO - 90°/a (mass/mass) of the soluble matter
present in the juice and will be discussed later.

3.2 Inorganic species

The inorganic species in the cane sugar industry are referred to as Ash

ash. This terminology probably reflects the analytical procedure used

to yield an inorganic residue after ashing under specified conditions
in the laboratory. In most cases and unless stated otherwise it can be
assumed that the ash is a sulphated ash, again reflecting a specific
analytical technique.

The inorganic species in cane juice consist of potassium, sodium, Inorganic specin
calcium, sulphate and chloride. Iron, because of its involvement with
colour forming reactions, is important. High concentrations of
inorganic constituents tend to hinderthe crystallisation of sucrose and
are thus undesirable. Phosphates, silica, calcium and magnesium are
also present in the juice. Some typical concentrations are shown in
Table

Table 4

Concentrations of inorganic constituents in raw cane juice

The total inorganic content of juice may be given in terms of
sulphated ash. In South Africa mixed juice shows sulphated ash levels A* In n&ed JWce

of about 0,45% (masstmass) or 3 - 4% on brix. The inorganic content

of cane is influenced by the cane variety, its age, the region where it
grows, the use of fertilisers, the soil type and the presence of tops and
trash, which can be overriding. It should be noted that this section
deals with soluble ash in cane, and not with soil/sand in cane. The
latter, which unfortunately tends to be called ash in cane in South
Africa, will be covered later.

3.4 Organic acids

Many organic acids exist naturally in the cane plant; they are
ncKs In casm juice
responsible for most of the acidity of the juice. Of these aconitic acid
is a major constituent but glycollic, malic, oxalic, citric, tartaric and
others are also present. Many acids occur in trace quantities. Acetic
and lactic acids are not natural constituents of cane but are formed by
microbial infection. Amino acids are also present. Many acids form
sparingly soluble salts during clarification and are therefore not
removed by this process. Others form salts which are deposited as
Evaporator wale
scale in the evaporators; oxalic acid for example reacts with lime to
form calcium oxalates which are precipitated at higher brixes in the
evaporators.

Trans aconitic acid, an unsaturated, tribasic acid, is the most Aconftlc "
abundant organic acid in cane juice. This acid is the subject of
research at the Sugar Milling Research Institute; it is implicated in
evaporator fouling, it increases lime consumption during
clarification, and results in the formation of aconitate crystals in low
purity streams. Its formula is shown below.

HOOC - -H
C =C

HOOCH2C' ` COON
The concentrations of three organic acids present in cane juice are
shown in Table 5.

Table 5

Concentration of organic acids in juice

Acid Concentration (mglkg brix)

Malic 600-900
Citric 700-1000

Aconitic 4000 -5000

3.5 Other organic species

Pectins are gelatinous carbohydrates generally in colloidal form. They Peons

increase the viscosity but are removed during clarification.

Gums are soluble or colloidal, high molecular weight polysaccharides.

They can be present as part of the cane plant itself, but by far the
more important gums are those formed by microbiological activity.
These gums, which include dextrans, cause severe processing
problems. Unfortunately the impact of the conventional clarification
process on the removal of gums is not very clear; a removal of about
10 - 20% has been measured, mostly through the action of heat and
pH, but other, unknown, factors were involved.

Proteins originate mainly from cane tops. They are coagulated by Protelm

heat and lime, and thus removed at clarification. Amino acids can link
together to form proteins.

Starch is a polysaccharide of high molecular weight and its presence sunk

in the juice is affected by the cane variety. It tends to be found more
in the immature tops. Cane starch is present as granules in the juice
and is solubilised at temperatures around 70°C; it is then not removed
by the clarification process and thus is present in syrup. Investigations
of the crystallisation process have shown that starch is highly
incorporated into the sugar crystal. It is released during the
corbonatation process in refining and causes very severe filtration
problems. Starch levels are controlled by the addition of thermally c.-amyia9e 'Yme
stable o-amylase enzymes, which are added to the third effect

- 1 0-
evaporator, in the raw house. A concentration of starch of about 120 Stanh !hilt €n raw =gar
mg per kg of sugar is acceptable.

Cane wax originates from the nodes and from the rind. It is physically Cane wax
removed with the clarifier muds and leaves the factory with the filter
cake. Cane wax has been recovered commercially from filter cake, by
a solvent extraction process, from time to time in the past. The
process does not seem to be financially viable now.

Colony bodies
The familiar green and yellow plant pigments (chlorophyll, carotene,
xanthophyll) are all present in cane and readily extracted into the
juice. Most are removed or destroyed by the clarification process.
Sugar colourants, which cause the colour of raw and refined sugar,
consist of four main groups. The first group contains colour bodies
from the cane plant itself, mostly phenolic, polyphenolic and PI"t colour
flavonoid compounds; many of those are yellow to brown in colour,
or can exist in the plant as non coloured compounds which are
oxidised to a coloured state in the juice, either by enzymes or through
chemical oxidation. The second group consists of caramels which are caramel

formed by the action ofheat on sucrose, glucose or fructose. Thirdly, c~no~ aRd a W'. „"e„
glucose can react with amino nitrogen to produce brown coloured
compounds, often of high molecular weights. Finally, fructose and Alkal6,r degradation of F and G
glucose degrade under alkaline conditions to yield highly coloured
products.
 4.THE SUGARS

Sugars are carbohydrates, that is they are composed of carbon, Carbohydrate

hydrogen and oxygen; hydrogen and oxygen are usually present in the
same ratio (2:1) as found in water.

Glucose and fructose are monosaccharides, that is they cannot be lionosacchaides

hydrolysed to smaller carbohydrate molecules. Monosaccharides
usually have 5 to b carbon atoms.

Sucrose is a disaccharide. It can be hydrolysed into its two Disaccharide

monosaccharides, glucose and fructose.

Spatial representations of glucose, fructose and sucrose are shown

below.

Chain Torn
H- C- OH C- O
ON - 1 H
OH- C- H
H-C-- -Ol"i H - ON
H -C--OH
H-C-OH
H -C-ON
H .-. C.__ ON

GLUCOSE FRUCTOSE

CFI,l7H
I
Ring Torn

=COSE TRUCrOSE

_ 1 2_
 CH,CH

O o O
H
- I F
~ C

IH O J - CHzOH
off CI CH

SUCROSE

In the leaf of plants the simple compounds C0 2 and water are

combined to form the sugar glucose. Because of its special role in
biological processes glucose is by far the most important and
abundant monosaccharide in nature.

Fructose occurs widely in fruits and combines with glucose to form

sucrose. Of all organic chemicals sucrose is the one produced in the
largest amounts in pure form.

Glucose and fructose reduce Fehling's solution, an alkaline solution atd-lng

of cupric ions complexed with tartrate ions; the deep blue colour is
discharged and red cuprous oxide precipitates. This is the reason
behind the name reducing sugars for glucose and fructose. Sucrose
does not reduce Fehling's solution and is thus a non reducing sugar.

4.1 Sucrose

Sucrose has the molecular formula C 12H,2a,,, with a molecular or ~~

weight of 342. The melting point of pure sucrose is 186°C at which ~`~~" '
temperature no destruction of sucrose takes place. Raising the
temperature above the melting point results in destruction and a dark Car&= [

coloured product, caramel, is formed. In the presence of very little

moisture, sucrose decomposes between 154 and 16TC to form
caramel.

An aqueous solution of sucrose rotates the plane of polarised light to Polarlaation

the right. This dextrorotatory property is used in analytical chemistry
and is the basis of the pot analysis.

Sucrose is very soluble in water and its solubility increases with solubiuer
temperature. There is no certainty as to the exact solubility of
sucrose in water and various authors give slightly different values.
Following a recommendation by Peacock, the data of Vavrinecz have

-13-
been chosen here. This is shown in Table b.

Table 6

The solubility of sucrose in water

Temperature . Mass of sucrose (g) dissolved

(°C) in 100 grams of solution (brix)
20 66,8

30 68,6

40 70,4

50 72,5
60 74,6

70 76,8

80 79,1

90 81,5

Solubility and saturation concepts are central to the recovery of

neffida~
sucrose by the crystallisation process. Some definitions are required.

Solubility
The composition of a solution may be expressed in many different SaUbMr
ways, for example mass solute per unit mass of solvent, mass solute
per unit mass of solution (brix), mass solute per unit volume of
solvent, and so on. It is therefore meaningless not to specify the units. 79.3 s In 1408 solution at 88°C

Since solubility is often temperature dependent, as is the case for

sucrose, the temperature must be quoted. Thus the correct way to
quote a solubility for sucrose would be 79,1g of sucrose in IOOg of
solution, at 80°C.

Saturation
sabiranon
A saturated solution is in thermodynamic equilibrium with the solid
phase, at a specified temperature. In simpler, but less exact, terms it
contains the maximum amount of solute in solution, at that
temperature.

- 1 4-
Supersaturation Saperaatrumtlon
It is often possible, for example by cooling, to prepare solutions
containing more solute than represented by the equilibrium saturation.
Such solutions are said to be supersaturated, at the specified
temperature. Again there are a number of ways in which
supersaturation can be expressed; considerable confusion results if
the units are not clearly stated. The temperature must also be given.
Two common expressions are the concentration driving force, Ac,
and the supersaturation ratio, S. They are defined as follows.
Ac
,&C=C-C
S
S = CIC

where c is the solution concentration, and c' is the equilibrium

saturation at the given temperature. The units used must obviously be
consistent. The following data are used as example. For sucrose at
20°C, c' = 2040g/kg of water; let c = 2450g/kg water. Then

E 5-c3?r~tfrfrf :. ~~ j :1~.

gikg water 2450 2040 410 1,20

The state of supersaturation is essential for crystallisation to occur. Crystallisation zones

Early in the 1900'x, the term "labile" and "metastable" were
introduced to classify crystallising systems. In the sugar industry the
relationships between the saturation/supersaturation of sucrose in
water and temperature are divided into four zones.

• The stable, undersaturated zone, in which no nucleation or crystal Stable

growth takes place. Any added crystals will dissolve.

Metastable
• The metastable, supersaturated zone, in which added crystals will
grow.

• The intermediate zone, where new crystals will form, if crystals lntermedlate
already exist.

• The labile zone, where new crystals will form spontaneously. Labile

These zones are shown schematically in the following diagram.

_ 1 5-
 C ation ygne3
5U4

340

300

740

43 AS

FEh1PEA:17URE VC)

The properties o£ sucrose as far as its solubility in water is concerned, Properties required for
eryatanbation
are quite special. It is highly soluble in water and can form highly
supersaturated solutions. Yet it is capable of crystallising, that is of
moving out of solution, to deposit itself in a controllable manner on
existing crystals. This is the basis of its recovery in industry. Fructose
and glucose are highly soluble in water but do not possess all the
other properties required for recovery by crystallisation. This is why
it is difficult to produce crystalline fructose or glucose.

Possibly the single most important chemical reaction of sucrose is its Hydrotysh of suerm
hydrolysis to yield equimolar amounts of glucose and fructose. This
is the " inversion " reaction, producing " invert ", In the chemical Inreraion
sense "inversion" means the changing of the dextrorotatory optical
activity to laevorotatory, or the converse. When a solution of
sucrose, which is dextrorotatory, is hydrolysed the equimolar
solution of glucose and fructose is laevorotatory, and this is the
reason behind the name inversion.

The hydrolysis (or inversion) of sucrose is either enzymatic, through

the enzyme invertase, or is brought about by acidic conditions. The
rate at which sucrose is hydrolysed depends on the degree of acidity,
pH, temperatarV, tlme
that is the pH, and on the temperature. The amount of sucrose which
will be inverted depends on the above two factors and on the time
available for the hydrolysis to occur.
When the pH is 5,8 and the temperature 120°C, for example,
inversion reduces the concentration of sucrose at the rate of 2% per
hour. At a pH of 4,6 and a temperature of 90°C, sucrose will be lost
at the same rate.

The hydrolysis or inversion of sucrose is represented by the following

equation.

~
C 1 2H220 ! 1 + H20 C6141206 + C6H1206

A small change in the molecular mass of the sugars takes place. Thus
3428 of sucrose produce 360g of fructose and glucose. This is due to
one molecule of water being taken up to form glucose and fructose.

4,2 Glucose and fructose

Glucose is metabolically the most important sugar in plants and

animals; it is also known as corn sugar, gape sugar and blood sugar.

Fructose is sweeter than sucrose or glucose and is the least abundant

of the three sugars in cane. Like glucose it is a reducing sugar.

Both fructose and glucose are relatively stable at low pH values, the Decomposition or F and G

maximum stability being at about pH 3. In alkaline solutions both

sugars decompose to form coloured products, the rate ofthe reaction
Pm temperatam and than
being controlled by the pH and by the temperature, while the amount
lost is a function of time. This decomposition creates a colour
problem and reduces the concentrations of these sugars. It will be
shown later that fructose and glucose increase the recovery o£ sugar.
Their destruction must therefore be kept as low as possible.

Finally, it is accepted that fructose is less heat stable than glucose; Effect or heat
fructose is destroyed more than glucose during evaporation. Glucose
on the other hand reacts with amino nitrogen, through Maillard type Mom" type rawtlons
reactions, to form coloured products, small gas bubbles and other
viscous products. The reactions normally occur in high brix, low
purity products, such as C-massecuites.

A major difference between beet and cane is that beet contains little Beet md cam
to no glucose and fructose. Thus all the steps which are required in
cane processing to avoid destroying these two sugars are not
necessary with beet. On the other hand the positive effect of these

-17_
sugars on molasses exhaustion is absent in beet, and beet molasses
contain more sucrose than cane molasses.
 5. THE TECHNOLOGY

It is usually accepted that cane quality has important effects on

factory performance and on sugar quality. These effects are well
illustrated in South Africa where cane originates from a relatively dry
and warm coastal area, an inland region with cold winters including
frost, and finally a more tropical region, in the North, where irrigation
is applied. This diversity in climatic and agronomic aspects has
resulted in the use ofdifferent cane varieties, different cane harvesting
practices, such as burning and trashing, and many other agricultural
aspects, which all affect cane quality.

In South Africa cane quality data, at the mills, are obtained through Analysis or cam and Jsilce
fairly sophisticated sampling and analytical systems. These involve the
weighing, sampling and direct analysis of the cane (DAC), the
weighing, sampling and analysis of mixed juice, and finally the
sampling and analysis of final bagasse. It should be noted that South
Africa measures the true sucrose (by gas chromatography or high
pressure liquid chromatography) and not only the pol in juice.

Several parameters are available to gauge cane quality. The estimated ERC,CCS
recoverable crystal (ERC) in cane was introduced by van Hengel in
1974. It is a simple formula which estimates the contribution of each
cane consignment towards the total industrial production of a
standard sugar. In Australia the commercial cane sugar (CCS)
concept is used. Purities, the concentrations of reducing sugars, of
ash and of a number of impurities, including colour, are also relevant.

The presence of sand or soil in the cane delivered at the mill can sand I soil In cam
cause serious problems. The content of suspended solids in the mixed
juice gives an indication of the amount of soil in cane, but the direct
measurement of sand or soil in cane yields a better measure. This
analysis was introduced in 1979, in South Africa; it involves the
ashing of a sample of cane in a furnace, and its result was
unfortunately called ash °Io cane; it must not be confused with the
soluble ash content of cane or juice.

Extraneous vegetable matter is the subject of much work, Cargill

(1976) describes sampling and analytical procedures.

In 1978, Schaffler and Smith compared the pol measurement to true Pot Versus sucrvx
sucrose, in mixed juice. Their results confirmed the superiority ofthe
sucrose based data; variable and large discrepancies found when poi

_l9_
is used were completely efnvnated. The analytical procedures are not
simple and the analyses are done routinely in a large central
laboratory, in South Africa.

Some specific aspects will now be considered.

5.1 Extraction

Rein (1975) investigated the effects of pol and fibre °Io cane on the Corrected reduced eitracdon
extraction achieved by milling. He showed that the extraction is (CRE)

adversely affected by high fibre levels but improves as pol °Io cane
rises. A corrected reduced extraction (CRE) formula was derived to
calculate an extraction independent of cane quality. Pith to hard fibre
ratio is believed to have an impact on extraction; similarly, sucrose to
fibre ratios have been showed to correlate positively with extraction
both for milling tandems and for diffusers.

Scott in 1977 carried out full scale tests to measure the effect of fibre Fibre and trash versos extraction
°Io cane and of tops and trash, on throughput in milling tandems. He
obtained two statistically significant regressions

Tons cane per hour = 203 - 5,3 x fibre % cane

Tons cane per hour = 134 - 3,0 x trash °/s cane

indicating that fibre and trash reduce the crushing rate.

5.ZTops and trash

Scott et al. (1978) and Lionnet (1980), among others, investigated Tops and trash versus cane and
the effect of tops and trash on cane and juice qualities. One percent Juice q-J*
by mass of tops or trash in cane was found to add 0,22 and 0,28 units
of soluble ash in cane, respectively. The same proportions oftops and
trash reduced the juice purity by 0,45, increased the juice colour by
1 to 4°/n, increased the juice sulphated ash by 1,2°Io and increased the
reducing sugar content by about 1%.

Lamusse (1979) measured the levels of fops and trash in the cane
delivered to mills in South Africa. On average the cane contained Tops and mash in cane

2,1°Io of tops and 5,3°/0 of trash, both on a mass basis.

Cargill (1976) investigated the effects of tops and trash on milling

capacity, on the recovery of sucrose and on transport costs.

-20-
Reid et al. (1989) investigated the milling of cane which had been
Tops .W i.mh veram nM[ng
subjected to four different type of harvesting systems, from burning
and topping, to no cleaning at all. Sorne results are in Table 6.

Table 6

Full scale milling of four types of cane

Stalks 88,4 1 4,4 I 1,13 87,6 1 4970

only

Stalks + 86,4 14,7 2,11 1 86,2 15040

tops

Stalks + 84,6 21,2 2,48 1 85,3 22090

trash

Stalks + 80,4 21,6 2,76 1 82,5 1 30730

tops +
trash

Another test but involving a diffuser, showed similar results. Further

calculations showed that recovery would drop by about 5% when
tops and trash are left in the cane; sugar quality, in terms of the usual
South African standards, would not be acceptable.

5.3 Sand or soil

As mechanisation replaces hand labour for the harvesting ofcane, the

sand content of the cane delivered at the mill increases. This has been
a worldwide trend. The sand/soil causes severe processing problems. efrecb or sMd WM Hdans RrA
With milling tandems the sand exits with the juice, it settles in juice ditfusioo
tanks, in clarifiers and in filter boots and must be removed. With
diffusion most of the sand leaves the extraction plant in the bagasse.
It then causes serious problems in the boilers because of erosion of
fans, tubes, etc., and because of high ash levels in the furnaces.

Apart from disrupting the process and damaging equipment, sand McrubloloV

promotes microbiological growth by providing a support on which

-21-
the microorganisms thrive.

5.4 Soluble ash and the monosaccharides

Cane and juice contain various inorganic species, usually quantified Sulphated. ash
by an ashing technique, which gives the sulphated ash content. This
is the soluble ash content which must not be confused with the sand
or soil content of the cane. The soluble ash content of the cane is
influenced by many factors, such as the variety, the locality where the
cane grows, the fertilisation practices, etc. Some results obtained in
South Africa are shown in Table 7.

Table 7

The effect of locality, month cut and cane variety

on soluble ash in cane

Tact or Sulphated ash 'fe brix

Locality A B C
1,8 3,7 5,7

Month cut June/July Aug/Sept Oct/Nov

4,5 3,1 3,4

Variety A B C
2,6 3,6 4,1

Soluble ash in juice has been shown to increase the solubility of Effects or ash and of F and G on the
sucrose in water, and thus to hinder the exhaustion of molasses. solubility of sucrose to water

Glucose and fructose on the other hand, reduce the solubility of

sucrose in water. It has been possible to quantify these two effects,
by experimentation. Rein and Smith (1981) and Smith in 1995
developed a target purity for final molasses given by the formula
shown below.

-0,74(F+G) Target purky formula

Molasses target purity= 43,1- 17,51- e 'A

-22-
where F is the fructose, G the glucose and A the sulphated ash
concentrations in the molasses. The formula was obtained by the
experimental exhaustion of many samples of final molasses under
specific conditions. It shows that as the sulphated ash increases the
purity of molasses increases; as the monosaccharides increase, the
molasses purity decreases.

In South Africa the formula has been used for many years and the
final molasses produced at the factories normally show purities
which are 2 to 4 units above the calculated target purity. This is
expected since wash water is used during centrifuging.

In 1998 Sahadeo and Lionnet showed that the formula applied to

cane molasses from 15 different cane processing countries. This
confirms the universality of this simple formula.

The difference between the actual purity of the molasses produced at

TPD
the factory and the purity calculated by the formula is called the
target purity difference, often abbreviated as TPD. This is possibly
the best indicator of backend performance. Abnormally high
viscosities have however been shown (Koster et al., 1992) to cause
TPD values to rise considerably.

5.5 Colour

Colour is an important sugar quality parameter. Raw sugar in South

Africa., which conforms to the very high pot (VHP) quality, must
meet a colour standard. Colour is also very important as far as refined
sugar quality is concerned.

Much work has been done in South Africa to investigate colour, both
in the rawhouse and in refineries. Two main results have emerged.
Under normal processing conditions, the colour of the raw sugar is Raw m g ar colour Is 6% or
V-p `o[Mr
determined by the colour entering with the cane. There is little change
between the colour in the cane and that of the syrup, and the raw
sugar colour is about 6% that of the syrup. Thus the only way to
reduce raw sugar colour significantly, without additional chemical
treatment, is to reduce the colour of the cane entering the factory. In
refining it has been well established that the colour of the refined
sugar is a function of liquor colours, which, for a given colour
removal cost, are in turn dependent on the colour o£ the raw sugar
feed. The colour of the cane is thus highly relevant.

-23-
Cane variety has an effect on colour; the range of colours in sixteen Variety and colour
South African varieties was from about 9080 to 19600 ICUMSA
units, a maximum difference of 54%. The geographical locality from Locality and colour
which the cane was grown also had a large effect, with a maximum
difference of about 55%. As shown in Table 1, tops, and more Tops and trash
particularly trash, contain large quantities of colour. Thus burning
and trashing will impact on cane colour-

5.6 Maillard type reactions

Maillard type reactions can cause severe problems in raw sugar

Glucose + andno nitrogen
manufacture. They involve reactions between glucose and certain
types of amino-nitrogen. Little is known about the reactions
themselves and about the amino compounds that trigger them.

The occurrence of these reactions causes much glucose, 40% or Products :-

more, to be lost. The reactions are exothermic, liberate gases, form Heat
Gas"
colour bodies and produce high viscosity, polymeric by-products. As Colour
a result massecuites swell and overflow, and temperatures rise thus
decreasing exhaustions. In addition massecuite handling and
centrifuging become difficult.

The occurrence of Maillard type reactions cannot generally be

predicted, but cane quality, particularly in terms of the region where
it grows, impacts on it. The reactions normally occur in low purity,
high brix streams, and are promoted by high temperatures,
particularly local overheating.

The results of severe Mailiard type reactions can be catastrophic, MaMrd and molasses storage
particularly in molasses storage tanks. Tanks have collapsed, leaving
their contents as dark porous masses, resembling carbonised sugar.
It is recommended that final molasses be cooled to below 40°C
before storage, and air sparging should be used in the tank to prevent
hot spots.

Cooling, by spraying water, is one ofthe few available defences, once Cooling
Maillard reactions have started. Massecuite brix should be reduced
and purity increased. The addition of sodium sulphite or
hydrosulphite, at concentrations of between 200 and 400 mg/kg of Addition or sdphiles

massecuite, has helped, but this is not always the case.

-24-
5.7 Post harvest deterioration

It is accepted that cane starts deteriorating immediately after it has

been burnt or cut. This deterioration is caused by two processes; one Natural enaymea aad
m1croort
involves the inversion of sucrose by enzymes naturally present in the
plant, while the second, which predominates in wet, warm weather
and can cause rapid and serious loses of sucrose, involves the
infection of the cane by microorganisms which secrete sucrose
inverting enzymes.

Work done in Australia shows that microorganisms are always

present in cane and reinfestation, by insect, rain, wind or direct soil
contamination, occurs rapidly after burning. Many different
organisms were isolated on the surface of burnt cane, some as early
as ten minutes after the burn. Burning may in fact facilitate infection Burning

by causing splitting of the stalk and seepage of juice. Tests on cane

wax show that it has some bacteriostatic activity; its removal by heat
may thus allow organisms to grow more freely. Organisms can enter
the cut stalk through the vascular bundles and massive infections have
been found up to 15cm from the cut end after 94 minutes.

The rate at which harvested cane deteriorates is influenced primarily

by temperature, the state of the stalk (whole/chopped, burnt/trashed), Temperature and state of stalk
the humidity and the cane variety. For a given cane quality and
agricultural practices, temperature is recognised as being a major
factor.

Work done in South Africa clearly demonstrate the effect of

The ear of temperature on h
temperature on the change in purity as cane deteriorated at 19 and
34°C, other conditions being similar; the trends are shown below.

b-
CL .

UTo -

iao tao
TIME (hours)

_2$_
Under industrial conditions cane purity is not an ideal parameter to
gauge deterioration, since the original, or non deteriorated, purity is
Ethanol in cane as an hidtcMor of
unknown. An independent chemical index is needed. Work at the deterloratlna
Sugar Milling Research Institute, over the period 1985 to 1990,
shows that the concentration of ethanol in the burnt cane is a good
indicator of cane deterioration. No ethanol is found in fresh, healthy
cane, under normal growing condition, and the rate of ethanol
formation as the burnt cane deteriorates is rapid. Furthermore the
determination of ethanol by gas chromatography is relatively simple.

It has also been shown that significant relationships exist between the
in burnt, whoiestalic cane:-
amount of sucrose lost and the ethanol formed. For burnt, wholestalk
cane, laid in windrows, about 1 % of the mass of pol in the fresh cane x% of the pol nsW6 Inmt for each
Frou an bris
is lost for every 1000mglkg brix of ethanol formed. The relationship 1"MP°'n
is different for bundled or green cane.

The effect of temperature on the formation of ethanol as cane Effect of temperance on ETON
deteriorates is well marked. Some results for wholestalk, burnt cane
laid in windrows, are shown in the figure below.

moo a
e000
_
Y

-J 3000
2000

Lu 1000

0 30 100 160 2ff0 250

TIME (hours)

Experimental work to investigate cane deterioration has shown that Mass km. 1% per day

cane loses mass as it deteriorates, mostly through dehydration, since

the mass of fibre was found to stay constant. Wholestalk, burnt cane
in windrows was found to lose about 1% of its mass per day, under
summer conditions in South Africa. The loss was linear with time.

Since the pol °Iu cane and the cane mass decrease as cane Lown
deteriorates, the mass of pol in the cane decreases with deterioration
ti me. This is a direct loss for the industry; it is however not the only
loss. As the microorganisms consume sucrose, they secrete a number
of impurities which cause processing problems in the factory and

-26-
these inevitably result in more sucrose being lost, mostly through rnmpactorkn
lower molasses exhaustion. It has been well established that the
concentrations of impurities such as gums and dextran increase
exponentially with cane deterioration time. These cause severe
viscosity problems, slow the crystallisation rate of sucrose and cause
crystal deformation.

The deterioration of chopped cane has been investigated extensively

°et`rio' °aor buletea cane
in Australia, during the mid 70's. Chopping the stalks into billets
obviously results in more exposed areas for microbiological
infestation and the deterioration is two to four times faster than with
wholestalk cane, under the same conditions. The results of
deterioration can therefore be extremely severe as illustrated by the
loss in recoverable sugar in the cane, expressed in commercial cane
sugar (CCS) units, reported by Vitale and Domanti, representing an Low of wcrose In cane

average from a number of Australian publications.

x
--a
to

3
ar
"2
d
ai

o s 10 is so za
TIME (hours)

Within a few hours the loss of sucrose has reached percentage levels.
As a result of these high potential losses the Australian industry
operates with cane delays of about 16 hours at most.

5.8 Climatic effects

Like any crop, sugarcane is affected by climatic disasters. Apart from

mechanical damage, for example due to gales, hail, etc., droughts,
frost and floods impact on cane quality.

Droughts reduce cane tonnage by slowing growth down and because nvonght

of high stalk mortality. Cane quality is lowered and this is aggravated Tonnage

_ 27_
 Colour
by accidental fires which accelerate cane deterioration. Drought also
increase the colour in the cane and thus sugar colour.

Floods cause purities to drop as flooded cane deteriorates, and the

soil content increases. Transport is disrupted and time efficiencies
reduced.

In South Africa frost occurs in the Midlands. Severe frost destroys

the growing point in the cane stalk which thus dies. An immediate but
relatively small purity drop is usually noted as the frosted cane is
crushed. If the weather becomes hot and humid, the frosted cane
deteriorates extremely rapidly and purities plummet. Severe
processing problems are experienced with deteriorated, frosted cane.

Some effects of major climatic disasters over a period of 20 years in

South Africa, are shown below The effects or floods and
droughts on :-

C 82

i 80
W
078--
LL
W 76 Time efSciendes.

F- 74

172
w
7
0 70
1 2 3 4 3 6 7 8 9 1011121314131617181920
YEARS

87

Puiities
185
W
V
84

81
1 2 3 4 5 8 7 8 9 1011121314151617191920
YEARS

-28-
where the solid bars represent normal seasons; year 9 was affected by
a flood while all the other clear bars represent draughts. There is no
doubt that time efficiencies are reduced and juice purity decreased.
 BIBLIOGRAPHY

Bacci J C and Guichard V (1994). Cane deterioration in Reunion island. S Afr Sug Technol Assoc
68,97-100.

Brokensha M A, Niemeyer R H and Schafle K J (1978). A comparison of the estimation of

sucrose in sugar cane mixed juice by poiarimetric and gas chromatographic methods. S Afr Sug
Technol Assoc 52, 54-58,

Carol J M (1976). Stop-Hulett's "Stalk only please" programme. S Aft Sug Technol Assoc 50,
18-24.

Cox M G S and Sahadeo P (1992). Post harvest deterioration of burnt cane in bundles. S Afr Sug
Technol Assoc 66, 224-223.

de Robillard P M, Vawda A and Lionnet G R E (1990). The measurements of losses associated

with cane delays. S Afr Sug Technol Assoc 64, 5-7.

Henderson C S (1972). Cane deterioration and its effects in the Racecourse area- 1971 season.
Proc Queensland Sugar Cane Technol 39, 267-273.

Ivin P C (1972). The effect of billet size on the rate of cane deterioration. Proc Queensland Sugar
Cane Technol 39, 279-280,

Ivin P C and Bevan D (1973). Further measurments of chopped cane deterioration. Proc
Queensland Sugar Cane Technol 40, 31-38.

Koster K C, Vermeulen P L M, Getaz M A and Lionnet G R E (1992). Some notes on abnormal

processing difficulties during Spring. S Afr Sug Technol Assoc 66, 127-130.

Lamusse J P and Munsamy S (1979). Extraneous matte in cane and its effects on the extraction
plant. S Afr Sug Technol Assoc 53, 84-89.

Lionnet G R E (1992). The effects of some selected factors on the colour in cane. S Afr Sug
Technol Assoc 66, 121-126.

Lionnet G R E and Pillay J V (1988). Ethanol as an indicator of cane delays under industrial
conditions. S Afr Sug Technol Assoc 62, 6-8.

Lionnet G R E and Pillay J V (1987). Ethanol as an indicator of bum to crush delay. S Afr Sug
Technol Assoc 61, 5-7.
Lionnet G R E (1986). Post harvest deterioration of wholestalk sugarcane. S Afr Sug Technol
Assoc 60, 52-57.

Morel du Boil P G and Schafer K J (1978). Application of gas chromatography in a preliminary

investigation into changes in some non-sucrose constituents during sugar-boiling. S Aft Sug
Technol Assoc 52, 96-105.

Peacock S (1995). Selected physical properties of sucrose solutions. Int Sug J, 97, 571-577.

Reid M J and Lionnet G R E (1989). The effects of tops and trash on cane milling based on trials
at Maidstone. S Afr Sug Technoi Assoc 63, 3-6.

Rein P W (1975). A statistical analysis of the effect of cane quality on extraction performance. S
Afr Sug Technol Assoc 49,43-47.

Rein P W and Smith I A (1981). Molasses exhaustibility studies based on sugars by gas
chromatography. S Afr Sug Technol Assoc 59, 85-91.

Schifler K J and Smith I A (1978). True sucrose versus pol- The effects on cane quality and
factory balance data. S Afr Sug Technol Assoc 52, 59-63.

Scott R P, Falconer D and Lionnet G R E (1978). A laboratory investigation of the effects of tops
and trash on extraction, juice quality and clarification. S Afr Sug Technol Assoc 52, 51-53.

Scott R P (1977). The limitations imposed on crushing rate by tops and trash. S Afr Sug Technol
Assoc 51, 164-166.

Smith I A (1995). Exhaustibility of molasses with low reducing sugar levels. S Afr Sug Technol
Assoc 69, 163-165.

Smith I A (1990). A survey of colour input and formation in process. S Afr Sug Technol Assoc
64, 213-216.

Vickers R P (1968). The Tully area cane deterioration investigation. Proc Queensland Sugar Cane
Techno135, 19-29.

Vitale M M and Domanti S A (1997). An investigation into the optimal length of sugar cane
billets. Proc Aust Soc Sugar Cane Technol 19, 170-178.

Watford S N (1996). Composition of cane juice. S Afr Sug Technol Assoc 70, 265-366.

Wood R A (1976). Cane deterioration as affected by billet size, delay in milling and other factors.
S Aft Sug technol Assoc 50, 12-17,
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

T Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control

In preparation:-

Evaporation
Diffusion
Crystallisation
Pan boiling
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
 Sri'

CHEMICAL CONTROL
 Sugar Technology For Students

CHEMICAL CONTROL

Prepared by G R E Lionnet

Study Text 4

Published by G R E Lionnet
Published by G R E Lioanet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright ® 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-23541-1

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For arrahability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban No* 4051, KZN, RSA.
 INPUTS
CANE PAYMENT
T
S[IC I3ISTRIBll"I~IDN I

I EXTRACTION
I I

I I

f 1

I
ouTPUTSi
RECOVERIES
! TIME ACCOUNT LOSSES
I I

T
STOCK I
I

f
V
 1. INTRODUCTION

Flourishing cane sugar industries are known to have existed in the

Mediterranean region during the 13 n' and I4''' centuries. As
colonisation of many parts of the world proceeded, cane sugar was
introduced and industries established in America and in West Indies
islands, to then move to most other tropical regions of the world.

In these early days cane quality, cane payment, and general measures
of control or performance were of little importance. In many cases,
a single concern owned both the plantation and the mill, and
economic considerations were limited to the sale of sugar and of by-
products.

As industry and commerce became more sophisticated, the growing

of cane and the manufacture of sugar became more independent of
each other; many cane sugar industries today are structured on the
basis of two separate but interdependent entities, the growing sector
and the milling sector. The revenue, however, arises from the
proceeds derived from the sale of the sugar and by-products. It
therefore became necessary to devise methods for the distribution of
these proceeds between the two parties. Furthermore, to increase the
competitiveness of the industry the methods should provide
incentives for growers to produce high quality cane, and for millers
to reach high sugar recoveries. As a results of these needs, systems
of measurements and controls were developed. These are generally
referred to as chemical control.

As the need for chemical control increased, other areas, such as

sampling, analytical techniques, and data handling also developed,
and this is still going on today. Chemical control is thus a many
faceted and dynamic aspect of sugar technology.
 2. MEASUREMENTS

2.1 Basic concepts

Measurements involve three components: a system, some properties

ofwhich is being measured; an instrument; and a human being. Errors
originate in all three components. As far as the system itself is
concerned, sampling for example is a crucial step; it must not affect
the system but must be representative. The instrument and method
used impact on concepts such as precision and accuracy. A simple
definition is that accuracy expresses the correctness of the
measurement and precision its reproducibility. Accuracy without Acs rnd pred4m
precision is improbable while precision does not guarantee accuracy.
It must be noted that, theoretically, it is impossible to obtain the exact
value of a physical measurement. Finally, people make errors due to
inexperience, carelessness, prejudice, or through some forms of
i nability, for example being unable to judge a colour change exactly
in a titration.

There are many sections of statistics which are available to deal with
measurements, as will be found in relevant textbooks.

2.2 Sampling

As was the case with measurements, many textbooks are available on

sampling. Some points particular to the sugar industry will be
stressed here.

Sucrose, the component of greatest importance in most samples, is

chemically labile and is degraded microbiologically. Thus, extreme
s,croft
care is needed to preserve its concentration during sampling, sample
handling, storage, compositing, etc. Very often the rapidity with
which changes occur is underestimated. Fructose and glucose are
also degraded microbiologically, but are somewhat more stable Fraclow rod Zrcose

chemically than sucrose. Nevertheless, the same extreme care is

needed. All samples, up to syrup, are liable to be affected by
microbiological or enzymatic activity. The use of juice preservatives
is essential, and the recommended procedures must be adhered to
rigorously. It should be noted that no preservative is capable of
providing an absolute guarantee that no deterioration will take place.
Rapid freezing is effective but thawing may be a problem. In all
cases, tested and recommended techniques must be adhered to.
Many streams in sugar factories are at high temperatures. Evaporation
Evaporation is thus always possible and, since it will affect
concentrations, needs to be prevented during sampling. This is often
not easy, but special techniques and equipment are available for many
applications.

Many streams in sugar factories contain suspended matter; some like suspended matter
sand settle quickly, while others like bagacillo, tend to float. This
impacts on the representativeness of the sample and of the sub-
sample. Again special techniques are available to cope with these
problems.

Sample contamination from fine bagasse particles or dust, in the air, Air borne contaminants
is always possible in a cane sugar factory, Apart from these impurities
themselves, there is the possibility of introducing microorganisms in
the sample.
 3. SOME FUNDAMENTAL CONCEPTS

3.1 Polarisation

3.1.1 Definitions DEFINITION'S

• POL • The pol of a solution is the concentration of sucrose in Pal

water (g per 1008 of solution) which has the same optical rotation
as the solution, under the same, specified, conditions. With pure
sucrose, pol gives the exact concentration of sucrose; in solutions
containing other optically active materials, pol is the algebraic sum of
all the rotations. In many practical cases pal thus yields an apparent
concentration of sucrose. The term is used as if pol was a real
substance.

• OPTICALLY ACTIVE • A substance is optically active if it can Optima actnity

rotate the plane of polarised light.

• DEXTROROTATORY • Dextrorotatory substances rotate the Deztrorotatory

plane of polarised light to the right. (Latin dexterldextra: right).

• LAEVOROTATORY • A laevorotatory substance rotates the Laevorotatory

plane of polarisation to the left. (Latin laevus: left).

• SPECIFIC ROTATION • The specific rotatory power [a] is the spccfc rotation

calculated angular rotation, in degrees, which a solution of lg of the

substance in I ml of solution, in a 1 dm path, gives to the plane of
polarised light, under specified conditions.

• POLARDAETER • An apparatus which measures the change in Pa]arhneter

direction of vibration of polarised light when it interacts with
optically active materials. It is one ofthe oldest instrumental methods
of analysis, it was used already in 1812.

• SACCHARIMETER • A polarimeter designed specifically for use saccharhneter

only with sucrose solutions.

• NORMAL WEIGHT • The weight of pure sucrose which, when Normal welaht
dissolved in water to a volume of 100nil at 20°C, gives a solution
reading 100 degrees of scale when read in a saccharimeter, in a tube
200mm long, at 20°C and with light of the specified wavelength. This
weight is 26,000g for most modern saccharimeters.
• °S • International sugar scale used until June 1988, as calibration in cs

saccharimeters.

• °Z • A new international sugar scale in use since I July 1988, as °z

official calibration of saccharimeters. The change to °Z was due to a
small correction, found experimentally, for the optical rotation of the
normal sugar solution (wavelength of the green mercury isotope
'98Hg
at 20°C in a 200mm tube), from 40,765° (°S) to a more correct
40,777°. To avoid confusion a new name was chosen, namely °Z.

3.1.2 The concepts

Ordinary light vibrates in all directions at right angles to the direction Plan, pomAmd upht
of the beam of light. Optical devices may be used to cause a beam of
light to vibrate in one plane only. Such light is said to be polarised or
more specifically to be plane polarised.

Many optically active substances, such as sugars, have the power to

rotate the plane of polarised light. The specific rotation [a] of the
optically active substance depends on the wavelength of the light and
on the temperature. If the sodium D line is used at 20°C, then the
specific rotation is denoted [a ] fl . This quantity for sucrose is
+66,5°, for glucose +52,5° and for fructose -92,5'-

When polarised light is passed through a sucrose solution, the amount

Basis of poi Analysh
of rotation will depend on the concentration of sucrose, the length of
the path, the wavelength used, and the temperature. If the last three
parameters are kept at fixed, standard values, then the rotation
becomes a function of the concentration of sucrose only. This is the
basis of the poi analysis.

Returning to the definition of [a], two equations can be derived:

eg unflon I

where a is the angular rotation in degrees, c the concentration of the

optically active substance in g1100m] of solution and 1 the path length
in decimeters, and
 100a Equation

pdl

where p is now the percentage of the optically active substance in

solution that is its parts by weight in 100 parts of the solution, and d
is the true density of the solution; thus pxd = c.

For the determination of pol, under the analytical conditions used to

obtain f a ]o for sucrose (+66,5), the two equations shown above can
be rewritten to yield concentrations:

100a
Equation 3
a 121
C} f 1D

100a
P ld[Q']za
d
Equation

Equation 3 is used when a known weight of substance is made up to

a known volume and read.

Equation 4 is used when a solution is read directly. Then d is needed.

In 1966 an international sugar scale was adopted, with 26,0008 as the

normal weight. Thus if 26,0008 of a material are dissolved in water Normal wet& nu*od
and the solution made to 100ml at 20°C and read at 20°C, in a
200mm tube, in a saccharimeter calibrated as required, the reading
gives the pol % material directly. This is the normal weight method
of pol determination, The pal result is the percentage by mass of pol
in the material.

In 1880 Schmita gave a procedure which does not require weighing,

and which is particularly useful with juices. The pol % is calculated
from the saccharimeter reading using the equation
 reading x 26,000
sebmitz'a metMd
Pyre/a = 99,718
x SG20120

where 99,718 is the weight in grams of I00ml of water at 20°C and

SG20120 is the specific gravity ofthe solution, a function of its Brix.
The weight of 100ml of water multiplied by the SG give the weight
of 100ml of the solution. This again applies to a saccharirneter
calibrated as required for the normal weight method.

It is clear that pol is exactly equivalent to sucrose only in pure

Appareotaucroa coactatradoa
solutions. Whenever other optically active substances are present, it
will measure the overall rotation and thus give an apparent
concentration for sucrose. Cane materials contain sucrose, fructose
and glucose, and often other optically active substances. As the
purities of the materials decrease, in molasses for example, pol
becomes less and less meaningful as an approximation for sucrose.

3.1.3 Pollsucrose ratio

This ratio is an indication of the difference between the pol and

PIS ratio
sucrose contents ofd material. In pure sucrose solutions the ratio will
be 1. In South African mixed juices it ranges from about 0,98 to 1,00;
but in molasses it varies from about 0,80 to 0,97. This illustrates the
difEculty in interpreting pol balances in a factory.

3.1.4 Pol derived

For 26g of sample dissolved in 100ml of solution at 20°C, in a

200mm tube, with the sodium D line, read in a saccharimeter
Pol derive d
calibrated as required, it is possible to calculate (Morel du Boil and
Schaffler, 1978) a pol value based on the assumption that the only
optically active species present are sucrose, glucose and fructose.
This is called the pol derived, Pola and is given by

20
Pold =o%oS+0,015 [a]x °IaG+Ia)DFX%F

where %S, °IsG and °IoF are the concentrations {mass / 100 mass
material) of sucrose, glucose and fructose, respectively; [a DG
 20
and [a ]DF are given by

[a I" = 52,50 + 0,0198 x %G + 0,00517 x %G 2

[a]") = - (88,12 + 0,260 x %FJ

Thus, if the concentrations of sucrose, glucose and fructose are

known, it is possible to calculate Pol l and to compare it to the pol
measured on the solution. Good agreement indicates that the only
major optically active impurities present are sucrose, glucose and
fructose. Disagreement, for example pal measured being numerically
greater than Poly, indicates the presence ofdextrorotatory substances
such as dextrans.

3.2 Brix

3.2.1 Definition
DEMITIONS

• BRIX -The Brix of a solution is the concentration, in grams solute

per 100 grams of solution, of a solution of pure sucrose in water, sru
having the same density or refractive index as the solution under
study, at the same temperature. When the refractive index is used, the
value should be called the refractometer Brix.

- SPECIFIC GRAVITY • A number indicating how much heavier a SG

substance or a solution is than an equal volume ofwater. It is defined
as the ratio of the density of the substance or solution to the density
of water, a temperature must be specified. Apparent specific gravity
is the specific gravity based on weights in air as opposed to weights
in vacuum.

-REFRACTIVE INDEX - A beam of light falling at an inclined angle Refraefive lades

upon the surface of a second medium will be found to be bent or
deflected. The ratio of the sine ofthe angle of incidence to the sine of
the angle ofrefraction, at a given temperature, is the refractive index.

- DRY SUBSTANCE - or dry solids, is the weight of material

Dry aobstma
remainin g after drying a product, under specified conditions,
expressed as a percentage of the original weight. The weight of dry
substance may also be found by deducting from the weight ofproduct
the weight of water, as determined in a specified manner.

3.2.2 The concepts

In the 1800`s, the scientist A F W Brix was involved with the

measurement of solids in sugar solutions; his name has been given to
the soluble solids found in sugar streams.

There are two basic physical parameters which are extensively used specific gravity and refractive index
to measure the concentration ofsoluble solids in sugar streams. These
are specific gravity and refractive index; the values obtained are
normally referred to as hydrometer Brix and refractometer Brix,
respectively.

Specific gravities in the sugar industry have been determined using

hydrometers, more commonly called Brix spindles. The applicability
of specific gravity arises from the fact that solutions of many different
sugars ofequal concentrations have almost identical specific gravities-,
this is illustrated below, for 10°/a solutions

Fructose 1,0385

Sucrose 1,0381

Arabinose 1,0379

Galactose 1,0379

Thus, in solutions of mixtures of sugars, specific gravity works well.

This is not the case however, when other dissolved substances, such
as salts, are present.

Specific gravities and the corresponding concentrations of sucrose,

expressed in mass sucrose per 100 mass of solution, or the Brix of
the solution, are given in tables found in many sugar technology
books. In expressing specific gravities it is usual to indicate the
temperature of the solution above that of the water; for example
2a° 20,
20'
or 4`
One ofthe disadvantages found with Brix hydrometers is the need for ntaadvaataVis orthe hydro.necer
large samples; this makes temperature control difficult. Reading the
hydrometer scale is also not easy.

Refractive index is now used extensively for the Brix determination.

Many modern refractometers, of varying degrees of sophistication,
are available. As was the case with specific gravity, many sugars,
when present at the same concentration, have nearly the same
refractive index. The refractive index is affected by the wavelength of
the light and by the temperature.

The refractometer is very suitable for the determination of the Advanta=es o[ the refl-aetowtrtc
concentrations of sugars in aqueous solution. It has many advantages sru
over the densimetric method. It is relatively easy to use; it requires a
small sample, sometimes a few drops only; it is rapid and lends itself
to automation.

For pure solutions of sucrose in water the Brix value, whether by

densimetry or refractometry, is exactly equal to the concentration of
sucrose. As the concentrations of impurities increase, Brix becomes
less and less meaningful.

3.2.3 Dry substance

The quantity of dissolved solids in a clear or filtered solution can be

Dry sunfawe or ary sanas
determined by actual evaporation of all the water and weighing ofthe
residue. The vacuum oven drying technique is based on this principle.
Specific analytical techniques have been developed and are used for
low purity streams such as final molasses. The results are often called
dry solids, and are expressed in mass per 100 mass of sample.It is
also possible to analyse the sample for its water content, for example
by the Karl Fischer method. The dry solids are then given by
subtracting the water, expressed as mass per 100 mass sample, from
100.

The two methods may not yield the same answer. Vacuum oven
drying will also expel the volatiles in the sample, while constituents
other than water in the sample may react with the reagent. Generally
Brix and dry solids will be numerically very different in final molasses.

_ 10_
3.3 The sugars

Sucrose, glucose and fructose in cane products are determined by F, G and s

specific, sophisticated analytical techniques such as gas
chromatography (GC), high pressure liquid chromatography (HPLC),
etc. These methods yield the concentration ofthe sugar itself, and not
an empirical result.

As shown previously, pol can only approximate sucrose in impure

solutions, the approximation becoming less and less meaningful as the
purity decreases. In cane sugar factories, mixed juice is usually the
process input stream, while the output streams are the filter cake, Pol versos sucrose
sugar and molasses. The quantity of sucrose in filter cake is usually
small and any difference between pol and sucrose is negligible. Due
to the high purity of sugar, pol and sucrose are virtually the same.
This leaves rnixed juice and molasses, which vary considerably in
terms of their impurity contents. Schafller (1976,1978), Morel du
Boil and Schaffler (1978) and Brokensha et al. (1978) show clearly
that the pollsucrose ratio in mixed juice can vary both within and
between factories; furthermore, the polarising properties of the non
sucrose component of the streams in the factory do change as
processing proceeds. From these observations, the above mentioned
workers show that the pol balance is incapable of providing
meaningful results, not only for internal control but also for
comparisons between factories. Recovery and performance data are
distorted by the use of pol; these inaccuracies are eliminated by the
use of sucrose in mixed juice and in final molasses.

The terra reducing sugars is used when the reducing substances in Reducing sullan versus F and G

cane products are determined using techniques such as the Lane and
Eynon titration. As expected it can be shown (Ravno and Lionnet,
1982) that these techniques are less specific than the true glucose
and fructose analyses mentioned above.

3.4 Other species

A number of specific components are important as far as chemical

control is concerned, because they impact on particular aspects o£
throughput or performance. Some of these are considered below.
3.4.1 Non-sucrose

The non-sucrose content of a material is the difference between the

total dissolved solids and the sucrose contents. In mixed juice it is non-sucrese %

given by {Brix°/o - sucrose %}; in final molasses it is the difference

between dry solids % and sucrose °Io. It impacts on throughput and
is used in mass balances.

3.4.2 Fibre De finltlon : Fibre

Fibre is defined as the dry, water insoluble matter in the cane. In

terms of the mass balance in South Africa, fibre is all the insoluble
solids in cane, that is it includes the vegetable fibre but also the soil,
sand, etc. in the cane. Fibre % cane, Brix % cane and moisture °Io
cane add to 104 exactly.

3.4.3 Ash

Sulphated ash is a measure of the content of inorganic matter in a

material. In cane sugar factories the inorganic species include
potassium, calcium, magnesium, chloride, etc. Unfortunately the term
ash °Ia cane, in South Africa, is widespread as a measure of soil or
sand in the cane.

3.4.4 Suspended solids

The term suspended solids in South Africa is used mostly as a

measure of insoluble solids in mixed juice. It is an important quantity
as it impacts on the mass balance at the extraction plant, which is
used to calculate the sucrose input into the factory.

3.4.5 Moisture

The water content of materials can have an impact on performance

or on quality, The term moisture is used. Thus moisture % bagasse
is an indication of milling performance; it also impact on the quality
of the bagasse as a fuel. Moisture °Io sugar is an indication of sugar
quality.
 4. THE TECHNOLOGY

4.1 Cane

Two main aspects relevant to the cane itself will be considered here.
The first is cane payment and the second deals with cane quality.

4.1.1 Cane payment

Some forrn of sampling and of analysis for cane payment purposes,

is found in all modern factories. Two distinct methods exist.

• Indirect methods, involving the sampling of first expressed or Indirect moo&

crusher juice. The juice is analysed, usually for poi and Brix, and a
method developed to relate these results to poi, Brix and some form
of recoverable sugar in the cane delivered by the individual growers.
The CC S (commercial cane sugar) determination in Australia and the
"Java ratio"method used in South Africa are based on these relatively
simple, but limited, indirect methods.

Direct methods
• Direct cane analysis methods, which involve sampling and analysing
the cane itself, Two main cane sampling methods are used, the core
Core
sampler, which produces a sample of cane taken directly from the
vehicle, at the weighbridge, and the hatch sampler, giving a sample
HAtch
of prepared cane, from the main carrier, just before the first mill or
the difuser. The sample of cane, produced by the corer or from the
hatch, is analysed by one of two methods. It can be mixed with a
known quantity of water and disintegrated in a mechanical digester; Digestion

the liquid extract is then analysed for poi and Brix, while some of the
cane is analysed for its moisture content. The second approach is to
subject the cane to high pressure in a cane press, under controlled
Pressing
conditions; the expressed juice is then analysed for poi and Brix,
while fibre is estimated from the weight of the press cake.

In South Africa, the DAC (direct analysis of cane) method involves DAC

a sample of prepared cane from the hatch, followed by the

disintegrator technique, where l OOOg ofcane and 20OOg of water are
used . The cane is also analysed for moisture by oven drying. The
extract from the digester is analysed for poi (p%) and Brix (b%). The
following calculations are then used.

-13-
 am=pflom:
Let M be the moisture °lo cane, F the fibre % cane and B the Brix %
cane. By definition M+F+B=100. It is assumed that the digester M+F+B -100
Exttteilon -100
technique results in complete extraction of pot and Brix from the
cane. Then

mass of Brix in the extract = 1000 x (100 - F - M)1100

mass of water in the extract =

1000 x M 1000 x F x 25
2000+ --
100 10O X 100
where the amount of brix free water, equal to 25% of the fibre, has
been subtracted, since it is not available for dilution, as discussed
later.

Then,

10(100- F - M) x 100 b-
b (mass Beix) x 100 / cum sekadon
10(100- F - M) + 2000+ IOM- 2,5F

It is easy to show that

100-- M - 3b
1- 0,0125b F1brrc % cane

The calculations for Brix and pot % cane follow.

1000x B
Mass Brix in cane =
100

b
Mass Brix in extract = mass extract x 100

- 14-
 100O X M Man extract -
Mass extract = 2000 + 100 - 2,5F + 10B water added + water la rune - 6rix
free water+ Brix in cane

hi+F+B-200
= 3000 - 12,5F

Then

IOB = (3000 - 12,5F)b1100 111 an Brix in cone=

mass Brix in extract
It is now easy to show that

Brix % cane = b(3 - 0,0125F) Brio "fin cane

The calculation for poi % cane is exactly the same but with pal
instead of Brix.

The three basic concepts involved in those calculations need more Basic concepts
comments.

• F + M + B = 100 • This is a basic definition and it shows that cane

consists of fibre, of water (measured by drying) and of Brix.

• Extraction = 100% • It is assumed that the disintegrator technique

yields poi and Brix extractions of 100%. There is independent
experimental support (Lionnet, 1986) for that.

• Brix free water • Brix free water is associated with the fibre in the
cane and is not available for dilution. It is bound water which cannot
be freed by mechanical means. It does however leave the fibre when
the cane is dried, and is thus included in M. Thus when the moisture
% cane is used to calculate the mass of water available for mixing
with the added water, brix free water must be removed. Based on
past work, the amount of brix free water is assumed to be equal to
25% of the fibre.

The DAC method used in South Africa thus yields poi, Brix and fibre Cane psymert requirements
in somrh afHea
% cane, for each consignment delivered at the factory. The
consignments are also weighed. In addition, mixed juice is weighed
and analysed for poi, Brix and insoluble solids. Bagasse is analysed,
by the disintegration technique, for Brix, and by oven drying for
moisture; fibre % bagasse can therefore be calculated. The following
procedures are then used.

-15-
Tons fibre in bagasse
tons fibre in cane by DAC - tons insoluble solids in mixed juice. Correction for Ne solkis
edtin; to mixed juke

This corrects the mass of fibre in the bagasse for that amount of
insoluble solids which was removed in the mixed juice and thus will
not be found as fibre in the bagasse.

Tons bagasse = tons fibre in ba asse x 100

fibre °/u bagasse

Tons pot in mixed juice uncorrected for insoluble solids =

tons mixed juice weighed x poi % mixed juice

100

Tons poi in mixed juice = Correction for the effect of salable

wlids on the pal % tutted Jake

tons pot in mixed juice uncorrected for insoluble solids x (100

i nsoluble solids vIa mixed juice)/1 00

The determination of the pot in the mixed juice is not done by the
normal weight method. The measured pot % value therefore applies
to a solution with no insoluble solids; thus the need to correct the
tons pot in mixed juice. The correction could be applied to the mass
of mixed juice. Legal considerations in connection with the massing
of juice for cane payment do not allow the mass of mixed juice to be
altered. Thus the need to correct the mass of pot and not of juice.
Either correction obviously yields in the same result.

Tons pal in bagasse = tons bagasse x poi vIo bagasse

loo

Tons pal in cane = tons pot in mixed juice + tons pot in bagasse Total tons pal h< trine

which is the official mass of pal entering the factory in the cane
delivered by the growers. It takes no cognisance of the individual
consignments. Tons pal far each row3pument

This amount of pot is now distributed among the individual cane

suppliers pro rata to their DAC analyses. DAC provides the pot v/o
cane for each consignment, and this together with the mass of the
consignment, allows the calculation of the mass of pal present in the
consignment.

-16-
It is evident that the South African method allows the determination
of the pol in cane by two independent approaches, one based on
mixed juice and bagasse, and on based on the pol % by the DAC Pot factor
method. This therefore allows a check to be made and the "poi
factor " is defined as

Poi factor = mass pol in cane from mixed_ juice and bagasse x 100
mass pol in cane by DAC

Thus is an important figure which has legal implications. Should the

pol factor decrease to levels below those considered acceptable, legal
action can be taken and financial compensations claimed. Tons pol by mass batancc

Traditionally the tonnage of pol in cane based on mixed juice and

bagasse has been called the tons pol in cane by mass balance.

The classical mass balance, cane plus imbibition water is equal to Cam + Imbibition smtrr-
mixed juice plus bagasse, cannot be used with cane diffusion. This is mixed Juke + bn=ane
due to a high degree of evaporation in the diffuser, which operates at
high temperatures. This loss of water cannot be measured and renders
the classical balance meaningless. When the balance can be used,
cane, imbibition water and nixed juice are weighed, and the tonnage
of bagasse then calculated.

The South African DAC system yields good data and has built-in
safeguards against inaccuracies. It is however sophisticated and
costly.

Cane payment systems vary from country to country, but, in all cases
they have an important impact on the economics and growth of the
i ndustry. Saranin (1975) gives an extensive review of cane payment
in the cane sugar industry. Finally, cane payment has also been
discussed in detail during the 1974 ISSCT congress.
4.1.2 Cane quality

The sampling and analytical systems installed for cane payment

purposes provide cane quality parameters such as pal, Brix and
purity. Fibre °Io cane impacts on the extraction plant. The poVfibre
ratio has been found to influence extraction. Fibre also impacts on
energy considerations.

Sand and soil in cane are quantified by an ashing procedure in South

Africa, which yields ash % cane. This is an important cane quality
parameter as it affects the boilers if diffusers are used, or the process
with mulling.

Estimated recoverable crystal (ERC) in cane is a simple concept ERC •.c cane
which allows the contribution of a given tonnage ofcane towards the
total production of a standard sugar to be calculated. Its basic
formula is

ERC=aS-bN-cF

where S is the sucrose % cane, N the non-sucrose % cane and F the

fibre % cane; a is a unit recovery, b a sucrose loss in molasses per
unit non-sucrose in cane, and c a pol loss in bagasse per unit of fibre
in cane. This concept, which has been discussed in detail by van
Hengel (1974), can give a good indication of cane quality.

4.2 Extraction

Pol, or sucrose, extraction given by

tons pol in mixed juice x 100

tons pol in cane

is a simple, widely used parameter to gauge the performance of the

milling tandem or diffuser. It has obvious financial implications.

The effects of cane quality, in terms of pol and fibre, were

i nvestigated by Rein (1975), in South Africa, who derived a corrected
reduced extraction, CRE, which allows the extraction to be corrected
to standard values of pol °Io cane (13) and fibre % cane (15, 15). This
makes the comparison of performances more meaningful.

-1 S-
The concept of absolute juice is important in milling, This is a
hypothetical juice of mass equal to the difference between the mass
of cane and that of fibre.

4.3 Mixed juice

Traditionally the process in many sugar factories is seen as starting

with mixed juice. This material is central to the mass balance concept
and is thus weighed and sampled as accurately as possible. In South
Africa it is analysed routinely for Brix, pol, sucrose, fructose,
glucose, sulphated ash and insoluble solids.

The true purity (sucrose °l0 1 Brix %) of mixed juice is a good

indication of cane quality and of potential recovery.

Its soluble ash content, expressed as sulphated ash °Io mixed juice,
together with its monosaccharide content, namely fructose % mixed
juice plus glucose % mixed juice, can be used to predict exhaustion
performances, as will be discussed later.

4.4 Stock

The chemical control of any process usually involves material

balances, that is a statement of the quantity of a material entering the
process and of the same material leaving the process. In the sugar
factory, the sucrose balance is the most important material balance;
sucrose enters in the cane only and leaves mainly in the bagasse, filter sucrox lwimee
cake, molasses and sugar. The total quantity of sucrose leaving will
normally be less than that entering, due to physical losses, chemical
destruction in the process, and errors in measurements, analyses and
techniques. These losses are grouped under the title "undetermined
losses".

Material balances in a cane sugar factory are complicated by the fact

that some ofthe material involved in the balance is only partly treated materials In stock

and held in stock, in the process. Such material will then be entered
i n the balance under the heading "in stock". For the purpose of the
sucrose balance it is assumed that all the sucrose in stock will leave
the factory in the sugar or in the molasses, Recovery formulae are
then used to estimate the percentage of the sucrose in stock that will

- 1 9-
exit later in the sugar; if this is x, then 100-x will leave in molasses.

Stock tacking is carried periodically, usually weekly, by physically

measuring the quantities of materials present in the factory and by
sampling and analysing each material for pol and Brix.

A simplified stock calculation is shown belo-, . The following

Important concepts
concepts are important.

Errors, such as the use of pol rather than sucrose, are largely
compensated for because the calculations involve differences rather
than absolute values.

• Traditionally the values for the period under study, usually a week,
are obtained by subtracting values applying to the previous to-date,
(namely to-date tonnages at the end of the previous week) from the
values applying to the present to-date, (that is to-date tonnages at the
end of this week).

• The important concept of "made" and of "made and estimated" is

involved. In stock taking made is synonymous with weighed, thus
sugar made means sugar that has passed over the scales and been
weig hed during the period. The word estimated applies to materials
in stock which are expected to be recovered later. Made and
estimated is the sum of these two quantities. All recovery parameters
and all losses are calculated using the made and estimated tonnages.

The following table is drawn.

Materials in stock

-20-
The values in column 4, tons Brix per m3, are available in most sugar
technology textbooks. The table is then completed and the tots] tons
Brix, tons pot and tons sugar in bins calculated. The following is now
needed.

Stock purity = 100 x 10161 1583 = 64,2

The SIM formula (see section 4.5.3) is used to estimate the

percentage (R) of the pot in stock recovered in sugar

R - = 75,9
J(S - M)

where S = 99,5 the purity o£ the sugar to be produced

7 = 64,2 the measured purity of the stock material
M = 30,3 the purity of the molasses made during the week

the estimated tons of recoverable pot = 75,91100x1016 = 771

the estimated tons of recoverable sugar = 771x100199,4 = 776

where 99,4 is the pol % sugar for the week.

The tons of pol that will be found in the molasses are 1016 - 771 or
245 tons.

Po! % molasses during the week was 26,98, then the estimated tons
of molasses in stock are

245 x 100/ 26,98 = 908

Thus for the week:

Estimated tons recoverable sugar = 55 + 776 =831
Estimated tons molasses = 908

Made (i.e. weighed) during the week:

Tons sugar = 4938,274
Tons molasses = 1492,000

It is traditional to use the difference between the to-date value and To-0 ate values

the previous to-date value to calculate the period value.

Tons sugar made previous to-date = 24557,683
Tons sugar made this week = 4938,274

Thus tons sugar made to-date = 29495,957

Estimated tons recoverable sugar in stock = 831

Thus tons sugar made and estimated to-date = 30326,957

Tons sugar made and estimated previous to-date = 25362,294

Tons sugar made and estimated this week = 4964,663 sugar nI & E far e
p riod

The calculation is similar for the molasses made and estimated for the
period.

Since the analytical results for the sugar and molasses are available,
it is possible to calculate tons of material, for example poi, sucrose,
dry solids, etc, in sugar and molasses made and estimated.
Recoveries, ratios and other performance parameters can now be
calculated by using the relevant torinages of materials in cane or in
mixed juice.

4.5 Recoveries and losses

The sucrose balance is used to calculate recoveries and losses in the

factory. The following quantities form the basis of all recovery/loss
calculations:

• Mass of sucrose in cane or in mixed juice

• Mass of poi in sugar made and estimated

• Mass of poi in bagasse

• Mass of poi in filter cake

• Mass of sucrose in molasses made and estimated.

The mass of sucrose in "undetermined" is the residual, calculated by ud,,.r.h,,,a I..: by dW, .
difference.

-22-
4.5.1 Overall recovery

Overall recovery (OR) is given by

mass of sucrose in sugar M& E

OR= 1100
mass of sucrose in cane

4.5.2 Boiling house recovery

Boiling house recovery (BHR) is given by

$HR = mass of sucrose in sugar M& E

x 100
mass of sucrose in mixed juice

This is a recovery based on sucrose entering the process. BHR is

influenced to a large degree by the quality of the cane; the impact of
mixed juice purity (sucroseBrix) on BHR in the South African
industry, over 15 seasons, is shown below.

BUR rs mixed juice purity

89

88

z 87
m

86

85
83 83.5 84 84.5 85 85.5 86 86.5
MIXED JUICE PURITY (SUCBRIX)

Many attempts have been made to derive recovery formulae which

would be independent of cane or juice quality. Lionnet and Koster CRB
(1986) reviewed some of the work done and proposed a corrected
reduced boiling house recovery (CRB) which is reasonably

-23-
independent of mixed juice quality. The derivation does include some
important assumptions described in detail in the above mentioned
reference.

4.5.3 SJM recovery

The SJM formula was introduced by Deer in 1904 and is one of the
most widely used concept to calculate the percentage of the total pol
or sucrose, in an initial material, which will be recovered in the sugar.
This percentage is given by

1 OOS(J - M) S J ht ramuutla
Rs~:~i - J(S - M)

where Rs,m is the recoverable sucrose (%), S the sugar purity, J the
purity of the initial material and M the purity of the molasses.

The formula divides the amount of sucrose in the original material

between the sugar and the molasses. No other loss (for example in
filter cake or as undetermined loss) is considered.

Its derivation is as follows.

Dcrirarion of SJM formula :-

Let Q be the mass of Brix in sugar, per ton of Brix in the initial
material, J the purity of the initial material, 5 that of the sugar or final
product, and M that of the final molasses. The initial material will be
indicated by i, sugar by s and final molasses by fm.

A sucrose balance then yields

tons sucrose in i = tons sucrose in s + tons sucrose in fin

or

sue % 1 x tons i = sue % s x tons s + sue % fin x tons fm

Purity is given by I00xsucolo/Brixolo. Substituting for suc °Io

purixBrix%ixtons i=pursxBrix%sxtons s
+purfmxBrix%finxtons fin

or

-24-
 pur i x tons Brix in i = pur s x tons Brix in s
pur fin x tons Brix in fm

For 1 ton Brix in i :-

purity i = purity s x Q + purity fin x (I -Q)

or
J=SxQ+M(1-Q)
J=SQ+M-MQ
J - M = Q(S-M)

_ J-M
S-M

Multiplying both sides by S/J gives

S J-M S
Qx_J_S-M x_
J

Q x5
is equal to (tons Brix in sugar x sugar purity) / (tons Brix in
1XJ
initial material x initial material purity). This is in turn equal to (tons
sucrose in sugar) / (tons sucrose in initial material). Thus

tons sucrose in sugar J-M S

x
tons sucrose in initial material S-M J

and

S (J - M) S J ]I formwa

% recoverable sucrose in sugar = x 100

J(S - M)

Taking an example. The mixed juice purity is 85,0; that of the VHP
sugar 99,5 and that of the expected final molasses 35. Then one can
expect an SJM recovery of

-25-
 995(85- 35)
RUM _ _ 85(99,5- 35) x 100

= 90,7%

Assuming a loss of poi of 0,2% in filter calve and an undetermined

Actual BHR
l oss of 2%, the actual boiling house recovery in the factory will be

BHR = 90,7 - 0,2 - 2,0 = 88,5%

4.4.5 Massecuite exhaustion and crystal content

Massecuite exhaustion is a measure of the recovery of sucrose in P arom krs for mn.wcuf n
crystalline sugar from the massecuite.

100(mc pur - mot pur)

PUT) x 100
Mc exh = me pur(100 - mol

Apparent purities are adequate for comparison purposes.

The crystal content of massecuites is useful to optimise boiling

systems and check operations, it is given by

(mc pur - mot pur) x Bx °%o me

Crystal % me =
(100 - mot pur)

4.5.5 Losses

Sucrose losses are obviously the most important ones in the

factory. The loss in bagasse is usually expressed as pol lost in Pol lost in Lapse and to filter cake

bagasse % sucrose in cane. It is given by

tans pol in bagasse x 100

Lost in bagasse °Io in cane =
tons sucrose in cane

The loss in filter cake is calculated similarly. The loss in molasses is

given by Lam in AnW molasses

tons suc in f mot M& E x 100

Loss in f mot =
tans suc in cane

The sucrose balance shows that the mass of sucrose in the cane
exits in the bagasse, in the filter cake, in the molasses made and
estimated and in the sugar made and estimated. Any residual

_27_
sucrose tonnage, calculated by the difference between the tonnage Undetermined loss
in the cane and the above exit tonnages falls under the name
"undetermined". A typical example for a South African factory is
given below, for a given period.

Cgeuludon of the undetermined

1059

T sue in cane 4875,000 100

T pol in filter cake 12,188 0,25

T pol in bagasse 146,254 3,04

T sue in f mol M&E 511,875 10,50

T poi in sugar M&E 4144,012 84,39

Total accounted for 4784,325 98,14

Calc tons lost in and 90,675 1,86

Since theundetermined loss is calculated by difference, thisparameter

Sucrose versus pol
will be affected by any inaccuracies in the system. The use of pal
instead of sucrose in minced juice and in final molasses has been
shown to cause severe errors in this parameter.

4.6 Molasses exhaustion

The loss of sucrose in final molasses is the single largest loss in cane Loss hl MO1MW3
sugar factories. It is therefore given special attention and a number of
parameters have been developed to investigate molasses exhaustion.

4.6.1 Molasses at 85 Brix °Io cane

This is a simple parameter which converts the molasses to a standard

Brix and expresses this amount as a percentage of the cane tonnage.
It allows straightforward comparisons

4.6.2 Molasses purities

The limitations of pol and Brix with materials containing high levels
of impurities have been well documented. With final molasses only
the specific parameters such as F, G and 5, dry solids, and sulphated
ash can yield meaningful results. True purities (sucldry solids) must

_28_
be used for the more fundamental measurements. Apparent purities
are used for short terns, comparative results in the factories.

4.6.3 Molasses factor

This is a measure of the melassigenic (molasses making) property of Meisssigenic properties

the impurities in the cane or mixed juice. It is well established that
impurities present with sucrose, in the process, will unavoidably
cause sucrose to exit with them, in the molasses. The molasses factor
is an attempt to quantify the melassigenic properties ofthe impurities
in the mixed juice, It is given by

tans sucrose in final mol M& E

MF -
tons non - sucrose in mixed juice

In South Africa the molasses factor ranges from 0,45 to 0,65; thus
I part of non-sucrose in mixed juice will remove about 0,5 parts of
sucrose.

Recent work at the Sugar Milling Research Institute (Sahadeo,

1998) has shown that the melassigenic properties of metal ions of
importance to the industry follow the trend
Melassiger& properties or metsl
Na>Ca/Mg>K ions

which is contrary to the trend found with beet. This work is

continuing.

4.6.4 Target purity

The production o£ standards for molasses exhaustion has received

considerable attention from sugar technologists, over the years.
Formulae have been proposed in Australia, Hawaii, India, Mauritius,
Puerto Rico and Taiwan. Most workers have attempted to correlate
the final molasses equilibrium purity with its composition, as
expressed by individual constituents or groups of constituents.

This concept was introduced in South Africa in 1949, by Douwes-

Dekker, using a formula which showed that the equilibrium purity
was lowered by reducing substances but increased by ash. In common

-29-
with many other formulae, Douwes-Dekker's reflects the opposing Reduef mg.n =W ash
influences which reducing sugars and ash, respectively, have on the
sucrose solubility in molasses.

This interesting and useful area of work continued in South Africa,

and culminated in 1981 with the publication (Rein and Smith) of an
equilibrium purity formula based on accurate gas-liquid
chromatographic analyses. This concept has been reviewed and used
extensively in South Africa, over a period of 20 years.

The formula (Smith, 1995) reads

FAG)
-0.74 Target P-" FO-6
Target pur = 43,1- 17,5 1- e

where F is the fructose % final molasse, G the glucose % final

molasses, and A the sulphated ash °Io molasses. The purity is the true
purity.

This formula predicts the purity of a molasses, based on its content

of monosaccharides and of ash, when exhausted in the laboratory
under specific conditions. It was derived by exhausting 133 samples
of molasses, under specific conditions, and using GLC analyses for
F, G and S. Conventional statistical techniques were then used to
relate the purities to F, G and A. Recent work (Sahadeo and Lionnet,
1999) shows that it applies to molasses produced in many countries.

4.6.5 Nutsch molasses

The terra "nutsch", or "cyclone" in Australia, usually refers to the

mother-liquor of a massecuite, extracted from the massecuite without
dilution, change oftemperature, or any operation which could change
its properties. In South Africa the nutsch filter (Munsamy, 1980) is
used to produce the nutsch molasses.

The purity of nutsch molasses at pan drop, after the last crystalliser, N parky profs
and after the reheater can be compared to gauge exhaustion work,

By comparing the purity of the final molasses to that of the nutsch

molasses at curing, one gets the purity rise across the centrifugals;

-3 0-
this is an important parameter as far as centrifugation is concerned.

4.7 Ratios

4.7.1 Cane to sugar ratio

This is the number of tons of cane needed to produce 1 ton of sugar.

It is a simple parameter which yields immediate comparisons as long
as the sugar quality is not too different.

4.7.2 Non-sucrose ratio

This is given by

tons non - suc in f mol + tons non - sue in sugar

N5R
tons non -suc in mixed juice

where the tonnages of final molasses and of sugar are made and
estimated values. The NSR is an indication whether non-sucrose has
been formed or destroyed in the process. In South Africa the value is
close to 1.

4.7.3 For G ratios

These ratios are given by

tons F (or G) in f mol M& E

F or G ratio
tons F (or G) in mixed juice

They give an indication whether F or G is produced or lost in the

process. It is assumed that the monosaccharide content of sugar is
negligibly small.

In South Africa the F ratio is about 4,90; thus on an overall basis

about 101/6 of the fructose is lost. The G ratio is smaller, namely
about 0,7. Thus about 30% of the glucose is lost, mostly through
Maillard type reactions.

-3 1-
4.7.4 Reducing sugar lash ratio

This ratio must not be confused with the reducing substance/ash

ratio. In South Africa it is usually shown as (F+G)/A, namely the
fructose plus glucose, sulphated ash ratio. It is often given on its own
as an important quality parameter for mixed juice and final molasses.
Its relevance to molasses exhaustion has been described in section
4.6.4.

4.8 Time account

The efficient utilisation of time is an obvious concern. This is

particularly important in the sugar industry, where the crushing
season is often limited by climatic conditions. In many countries
crushing has to be stopped when the summer rains prevent access to
fields or cause the cane to revert to fast growth thus lowering its
sucrose content. Seasons can range from relatively short periods of
about 100-120 days, to the whole year, in rarer cases. In South Africa
the season is relatively long at 230 to 280 days.

In all cases it is important to measure the efficiency with which time

is utilised, and to quantify and identify the reasons for stoppages.

4.8.1 Overall time efficiency

Overall time efficiency, OTE, is given by

(total gross available time in hours - hours scheduled stops - hours no

cane stops - hours other stops - hours foreign matter stops) x 1041
total gross available time in hours

An example of the calculations to obtain the time parameters will be

given later.

4.8.2 Lost time % available

L T A is given by
hours other stops x 100
gross available time in hours - H

-32-
where H is the sum of hours for scheduled stops, hours stopped for
no cane and hours stopped for foreign matter.

4.8.3 Stops

The stops are expressed as percentages of the gross available time in

hours.

°Io foreign matter stops =

hours stopped for foreign matter x 100

gross available time in hours

% scheduled stops =

hours scheduled stops x 100

gross available time in hours

% no cane stops =

hours stopped for no cane x 100

gross available time in hours

°Io other stops =

hours other stops x 100

gross available time in hours

4.8.4 Example of time calculations

For a given week: -

Cross avaflahle time for 1 week

Cross available time = 7 x 24 = 168 hours

-3 3-
Hours stopped for foreign matter = 2
hicammd swp
s ht houn
Hours scheduled stops = 16
Hours no cane stops = 12
Hours other stops = 6
co ed trm pmwmtrm
0 T E = (168-2-16-12-6) x 1001 168 = 78,6

LTA=6x 1001(168- 16-12-2)=4,35

% foreign matter stops = 2 x 1001 168 = 1,19

% scheduled stops = 16 x 1001168 = 9,52

% no cane stops = 12 x 1001 168 = 7,14

% other stops = 6 x 1001 168 = 3,57

4.8.5 Some definitions NllnMorcs for rtne rakolarfaa,

The following definitions apply to the time calculations used in South

Africa.

• FOREIGN MATTER • Any clearly identifiable foreign object,

directly and immediately causing the stop, which was delivered with
the cane.

SCHEDULED • Planned stop for maintenance at the factory.

NO CANE • A factory stop because of cane not being delivered, for

example because of roads or fields being unaccessible to transport
due to rain.

OTHER - Normally a stop due to the factory itself, for example a

mechanical breakdown or the factory being full.
 BIBLIOGRAPHY

Browne C A and Zerban F W (1948). Physical and chemical methods of sugar analysis. John
Wiley and Sons. London

Brokensha M A, King S and Lamusse J P (1976). Evaluation of the press method for cane
analysis under South African conditions. S Afr Sug Technol Assoc 54, 212-219.

Brokensha M A (1984). A trial to compare core sampling with the full width hatch method of
cane sampling. S Afr Sug Technol Assoc 58, 9-14.

Brokensha M A, Niemeyer R H and Schaftler K J (1978). A comparison of the estimation o£

sucrose in sugar cane mixed juice by polarimetric and gas liquid chromatographic methods. S Afr
Sug Technol Assoc 52, 54-58.

Brokensha M A (1979). Freeze preservation of sugarcane juice samples. S Afr Sug Technol
Assoc 53, 70-72.

Buchanan E J and Brokensha M A (1974). The application of direct cane testing to the South
African sugar industry. Proc Int Soc Sug Cane Technol 15, 1456-1469.

Day-Lewis C M J and Schafller K J (1992). Analysis of sugars in final molasses by ion

chromatography. S Afr Sug Technol Assoc 66, 131-135.

Emmerich A, Zander K and Seiler W (1991). Basic measurements for the definition of the new
ICUMSA International Sugar Scale. Zuckerind. 116 (1191) Nr. 1, S. 110-124.

Hugot E (1974). Direct analysis and evaluation of sugarcane. Proc Int Sac Sug Cane Technol 15,
1426-1436.

Landry W J (1974). Core sampler procedure and analysis as a method for cane payment. Proc Int
Soc Sug Cane Technol 15, 1444-1456.

Lionnet G R E (1992). A review of some aspects of cane quality in South Africa. Revue Agric, et
Sucriere de file Maurice. Vol 71, 2&3, Mai-Dec 1992, 79-87.

Lionnet G R E and Koster K C (1986). A boiling house recovery formula independent of mixed
juice quality. S Afr Sug Technol Assoc 60, 30-32.

Lionnet G R E (1986). An analytical approach for the determination of colour and other
impurities in cane. S Afr Sug Technol Assoc 64, 62-65.

Morel du Boil P G and Schaffler K J (1978). Application of gas chromatography in a preliminary

investigation into changes in some non-sucrose constituents, during sugar boiling. S Afr Sug
Technol Assoc 52, 96-105.

Munsamy S (1980). The new SMRI nutsch bomb. S Afr Sug Technol Assoc 54, 79-81.

Ravn6 A B and Lionnet G R E (1982). Exhaustion performance yardsticks in the South African
sugar industry. S Afr Sug Technol Assoc 56, 46-50.

Rein P W and Smith I A (1981). Molasses exhaustibility studies based on sugars analysis by gas
liquid chromatography. S Afr Sug Technol Assoc 55, 85-91.

Rein P W (1975). A statistical analysis of the effect of cane quality on extraction performance. S
Afr Sug Technol Assoc 49, 43-48.

Sahadeo P (1998). The effect of some impurities on molasses exhaustion. S Afr Sug Technol
Assoc 72, 285-289.

Sahadeo P and Lionnet G R E (1999). An analytical survey of final molasses from cane producing
countries. Proc Int Soc Sug Cane Technol, 23, in press.

Saranin A P (1975). Sugar cane payment systems. Sugar Technol Rev, 3, 155-238.

SchMer KJ and Smith I A (1978). True sucrose versus pol. The effect on cane quality and
factory balance data. S Afr Sug Technol Assoc 52, 59-63.

Schiffier K J (1976). Preliminary comparison of polarimetric and gas chromatographic methods

for the estimation of sucrose in sugarcane mixed juice and molasses. S Aft Sug Technol Assoc 50,
220-223.

Smith I A (1995). Exhaustibility of molasses with very low reducing sugar levels. S Afr Sug
Technol Assoc 69, 163-165.

van Hengel A (1974). Proposal for the evaluation of cane and sugar in identical units at
standardised factory efficiency. Proc Int Soc Sug Cane Technol 15, 1446-1455.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
Filtration
3 Chemistry of cane and juices
4 Chemical control

In preparation:-

Evaporation
Diffusion
Crystallisation
Pan boiling
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
 TUDENT S

EVAPORATION
THE FUNDAMENTALS
 5r -'

Sugar Technology For Students

EVAPORATION
THE FUNDAMENTALS

Prepared by G R E Lionnet

Study Text 5

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North , 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright ® 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-24196-9

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This test forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 1. INTRODUCTION

The purpose of clarification has been to remove impurities from the

Removal o! water
juice, as far as possible. It now remains to remove the water, which
is done by evaporation.

As evaporation proceeds, the sucrose becomes concentrated and, as

it reaches saturation, crystals will appear in the liquid. As this second
phase proceeds, the material does not behave as a liquid anymore.
kvaparatton 1 Crystallisation
Thus the evaporation/concentration process is separated in two
operations. Evaporation itself starts with clear juice and yields syrup;
it thus deals with a liquid material. This is then followed by the
crystallisation process.

In the early industry, evaporation and crystallisation were done in Multiple efe[is
open pots. A significant step forward was taken around 1830 when
Norbert Rillieux proposed multiple effect evaporation. The idea was RWleu:
to use the vapour produced from one vessel to heat another portion
of the juice. For this to work one must obtain a temperature
differential; Rillieux solved this problem by lowering the pressure in
the subsequent vessel. This solution requires vacuum equipment but Vacuum is needed
but
it optimises the use of energy and reduces the temperature at which energy is saved, attd
the more concentrated and viscous juice is handled, which is temperatures arc lrmered

beneficial in terms of losses and of colour formation in the cane sugar

i ndustry.

The evaporator station consumes much energy. Thus, considerations

based on energy will be central to the study of this operation. At the
same time, however, the chemical species in the juice will be exposed Temperature and chemical changes

to a range of temperatures which include fairly high values,

particularly when large climbing film evaporators are used. Although
the residence times are relatively short, particularly at the higher
temperatures, chemical changes can and do occur. These must
therefore be considered.

The boiling ofliquids at sub-atmospheric pressures can result in liquid

Entrainment
entrainment, and thus in losses of sugar. This aspect will also need
attention.

The changes in temperature and in concentration, during evaporation,

result in the precipitation of various chemical species. This causes Fouling
fouling problems since the species deposit themselves as scale on the
heating surface. Scale reduces the heat transfer, to the extent that the
factory has to stop, to allow the evaporators to be cleaned. In c-l"t
addition to the cost of cleaning there is a cost associated with the loss
of production. The reduction of fouling and the optimisation of
evaporator cleaning are active areas of research.

Finally, because of the impact of evaporation on energy, evaporator aeAgns.

New
design is receiving much attention in the cane sugar industry. A
number of new types of evaporators are being tested and some have
been introduced in the factories.
 2. THE CONCEPTS

2.1 Basic Principles

2.1.1 Unit of heat

In the SI system internal energy, heat and work are all measured in
TLe Jotile
the same unit, the joule (J). The joule is defined as the amount of
kinetic energy possessed by a 2kg object moving at l ms". Then

El.Cdc - 0, 5 mv,

= 0,5(2kg)(lms')2

1 kgm2 s"2

As a reference to the calorie, the joule is exactly equal to 114,184

calorie.

The joule was named after James Joule; it is a relatively small unit of
energy, each beat of the human heart consumes about 1J. In practice The .oM J/s
the kilojoule, (kJ), namely IOOOJ, is better suited_ A kW is then
I40OJs""', since the watt is in joules per second.

2.1.2 Thermal properties

The thermal properties of a substance are properties that describe its

ability to absorb or release heat, without changing chemically. Heat
capacity and specific heat are such properties.

Heat capacity is defined as the amount of heat energy required to

Heat expacfty, JI'C
raise the temperature or an object by one degree Celsius. Its unit is
JI°C.

The specific heat capacity, usually known as the specific heat, is the speeiee heat. J1 002
heat capacity per unit mass, usually for lg. It can be defined as the
treat needed to raise the temperature of one gram of the substance by
I °C. It is then the heat capacity per gam.

Specific heat = heat Maci

mass(g)
Since heat capacity is in 71°C, specific heat is in JI°Clg. For example
the specific heat of water is 4,18J1°Clg at 25°C. Expressed in
calories, the specific heat of water is IcaV°Clg.

The specific heat capacity of sucrose solutions, Cp, can be calculated

from a correlation given by Peacock (1995): sa of euerose solutions

CP = 4,1253 - U,0248d4B + 6,7x10'SBT + 1,8691x1D''T - 9,271x14

where B is the brix of the solution and T its temperature in °C. Cp is

then in kJ/kg/K.

Because phase changes occur at constant temperature and pressure,

the potential energy change associated with vaporisation can be VapatIsation
expressed as an ENTHALPY change, OH. The word enthalpy was
invented to deal with energies when the system is under constant
pressure. Enthalpy changes are often expressed on a per mole basis.
Thus the molar heat of vaporisation, OH ;., is the heat absorbed
when 1 mole of a liquid is changed to 1 mole of vapour, at a constant
temperature and pressure. In the case of water, the heat of
vaporisation is a function of pressure as shown below.

4400
Y
Heat of vaporisation of
X350 water, 11ift
a~
32300
6
m2250
a
2200
m
r
2150
0 50 100 150 200 250
Pressure (kPa)

The heat of vaporisation of water will be needed often in evaporator

calculations; it can be seen from the above figure that it will range
from about 2200 to about 2370 kJ/kg under usual operating
conditions.

A-
Boiling point elevation, BPE, is a colligative property of a solution, Boiling point elev9don
by which its boiling point will be higher than that of the pure solvent.

The term colligative means a property whose physical value depends Coltlf2ttre
on the ratio of the number of moles of solute and of solvent, and not
on their chemical identities. Normally, solutes elevate the boiling
point of solutions. The magnitude of the effect, quantified by OTb,
is proportional to the relative populations of solute and solvent
molecules. For dilute solutions

AT, = Kb.m

where m is the molality, that is the number of moles of solute in

10OOg of solvent. Kb is characteristic of the solvent only, and for
water is 0,51°Cm""'.

Peacock (1995) gives a correlation which allows the calculation of

the BPE, for sucrose solutions, when the brix and temperature are
given. This has been used to calculate BPE, at atmospheric pressure
and for brix values from 10 to 70, as shown in Table 1.

Table 1
Boiling point elevation of sucrose solutions at
atmospheric pressure, for various brix values.
BPE values for sucrose solutions

These data can be used to calculate K b, which is found to be equal to

0,69°Cm', instead of the theoretical value of 0,51 °Crf'. This is due
to the fact that the solutions in Table I are not all dilute.

Hydroatadc head
The hydrostatic head is now considered. When a pressure P is exerted
on the surface of a liquid, the pressure to which the molecules are
subjected at a given depth in the liquid is equal to P increased by the
pressure due to the column of liquid to that depth. If the liquid
temperature is equal to that needed to produce boiling at the surface,
then there will be no boiling at lower depths.

In evaporators it is considered that the transmission of heat is

sufficiently rapid to cause boiling throughout the liquid depth in the
tubes. Then, the juice at the bottom of the tube will be subjected to
a hydrostatic pressure equal to the weight of juice above it, and will
boil at a higher temperature.

In practice many complications arise. The juice is turbulent,

conditions are variable, and it is nearly impossible to measure juice
levels. It is therefore difficult to calculate the contribution of the
hydrostatic head to the juice boiling temperature, with any degree of
certainty; this effect will be ignored in the calculations presented
later. In principle, however, it must be present.

The concept of the heat transfer coefficient, HTC, is central to the

design, operation, and performance assessment of evaporators. Heat trasfer eoeMclent, HTC

HTC is defined by the following equation:-

Q=KAOT
Deflm"Z egmatlon for HT C

where Q is the heat energy transferred per unit of time, namely Js' ,or
m'kgs3. A is the heat transfer area, in m2. LET (delta T), is the
temperature difference, or the driving force, which causes the heat to
flow.

The proportionality constant, K, is called the heat transfer coefficient.

A unit analysis shows that the units of K are m xkgs31m2°C. Since the
watt has units of rn kgs3, it is clear that K is in Wni s°C-'. It is thus uau, of]ErrC
in watts per square metre of surface area, per degree of temperature
difference. Note that the watt is in fact equivalent to joules per
seconds. The HTC is thus the amount of heat energy transferred per
second, per unit area, per degree of temperature driving force.
Let us assume that we want to measure the HTC for an evaporator
vessel. We need the following:-
Cakolation of ITTC :•
Q, the heat provided by the steam or vapour

A, the heat transfer area

AT, the temperature difference.

Q, the amount o£ heat transferred, can be calculated in a number of

ways. A material balance over the evaporator can yield the amount
of water evaporated; if the juice feed was not at its boiling point, then
a correction is needed. The vapour produced may be condensed and
measured; again if the feed was not at its boiling point a correction is
needed. Finally condensate from the heating steam or vapour can be
measured and the heat input calculated.

A, the heat transfer area, is obtained by a physical measurement. This

is relatively straightforward.

AT, this is the most troublesome quantity for measurement.

Furthermore, since it is usually numerically small, large errors can
occur. It is generally assumed that the temperature of the heating
steam will be uniform and known. The difficulty is in estimating the
juice temperature. This varies along the heating surface of the tube,
and juice levels are very difficult to measure. A number of
appro)dmations are necessary:-

The juice temperature may be assumed to be equal to that

corresponding to the vapour pressure, to which the boiling point
elevation must be added.

If the hydrostatic head is considered, then one can estimate

this pressure, adding it to the vapour pressure and then reading the
corresponding temperature. SPE is then added. This is the
temperature of the juice bailing at the bottom of the tube. That for
the top of the tube is as calculated above. The juice temperature is
now an average of the top and bottom values.

In other cases, a log mean temperature is taken. Then

 At, -Ot x
T= In(Ot, / et2 )
where At, is the difference between the steam temperature and the
feed temperature, while Ot 2 is the difference between the steam
temperature and the boiling point of the juice.

The SPE needs the brix, to be used in the correlation from Peacock;
again there is a problem in deciding which value to use. An average
equal to the arithmetic average of inlet and outlet brixes is often used.

It is important in HTC calculations to show clearly what assumptions

have been made and what values have been taken. This gives meaning
to the results and allows comparisons.

2.1.3 Multiple effect evaporation

al 30
M120
x110
U-100
0
~- 90 Boilkg point aiwater rs prenurt
0 S0

m 5p ! a f i +

0 50 100 150 200 250

PRESSURE (kPa)

It is well known that the bailing point of water decreases as the

pressure decreases. This fundamental relationship is shown above.

The multiple effect evaporator then follows the principle shown in the
diagram below.
 TO VACUUM
V APL7IIR

hfultlpie effect principle

STEAM

SYRUP

In this way the necessary temperature difference is obtained and it is Triple, quwl and quin
possible to utilise the vapour produced by a previous effect to heat
the next. In the cane sugar industry the approach is used with three
(a triple), four (a quadruple) or five (a quintuple) vessels.

2.1.3.1 Temperature limits Temperature range

The temperature limits for a multiple effect are now considered. From
a theoretical point of view, the highest temperature would be that at
which sucrose decomposes; this can be taken as 130°C. The lowest
theoretical temperature would depend on the vacuum reached in the
last vessel; taking 12 to 14kPa as the lowest attainable pressures, one
would boil at 49 to 53°C. This gives a maximum theoretical range of
130-49 or 81 °C. There are of course many practical problems with
this maximum range.

Firstly, it would be dangerous to assume that variations in the Practically

operating conditions would never cause the temperature to rise above
130°C; as a measure of precaution the recommended maximum Higher limit 12I°C
temperature is usually given as 121°C.

Secondly, high vacuum levels increase entrainment, low syrup

temperatures may not be desirable for good pan feed quality, and
more importantly, it can be shown that heat transfer coefficients are Lower 11=11 SS°C

reduced, due to viscosity effects, at low temperatures. A value of

55°C is usually quoted as an acceptable lower limit.

R=P "0C
The practical temperature range in the cane industry is thus 66°C.

Multiple effect evaporation needs vacuum equipment, which can be

seen as a disadvantage. This is, however, more than compensated by
all its advantages. It optimises the use of energy; it allows
evaporation of the more concentrated and viscous cane juice to be
done at lower temperatures. This reduces inversion and the
degradation ofmonosaccharides, and is an important advantage in the
cane industry.

2.1.3.2 Vapour bleeding

In the simplest case, all the vessels in a multiple effect may be of the
same size, and each then supplies vapour to the following vessel.

It is possible, however, even with the same size of vessels to

withdraw, or bleed, some vapour from the vessels, to use in the juice
heaters or in the pans. This operation is advantageous with respect to
heat economy, in that the steam used in the heater or pan is now
replaced by vapour from one ofthe evaporator vessels. The economy
achieved increases as vapour is bled from vessels further on down the
set. If the vapour is bled from the last vessel then the economy is
complete since that vapour and its energy would otherwise have been
lost.

Since the vapour bled is at a lower temperature than the exhaust

steam it replaces, a larger heating area is required. Obviously a
vapour will not be able to raise the temperature of a material above
its own.

Theoretically vapour can be bled from any vessel in a set of vi aad V2

evaporators. In South Africa vapour bleeding is usually restricted to
vapour from the first and second effects. These vapours are called
vapour 1 (V I) and vapour 2 (V2) respectively.

Theoretical calculations of the steam savings with vapour bleeding

are now considered.

-10-
Without vapour bleeding the heaters and pans need R tons of steam.
The evaporators need Q tons of steam. Then, the total steam needed,
D is

D=R+Q

We now assume that we will bleed from a quad, and that each unit
Assumptions
bled will be equivalent to one unit of steam (the latent heats are
approximately the same). It is also assumed that the temperature
profile allows the use of all the vapours.

Say we take P, from vessel 1, P2 from vessel 2, and so on; the

vapours bled then account for all the demand from the heaters and
pans. Then

PI +P2+P3+P4=R

The evaporators now need a new steam supply, D b, and

Db =X+Pi+Pz+P3+P4

Sham and vapour for bleeds

where X is the vapour going into the condenser from the 4 h vessel.

Assumptions
The following assumptions are now needed:-
 In each vessel 1 unit of mass of inlet vapour evaporates 1
mass unit of water.

Bleeding P, from vessel 1, P 2 from vessel 2, etc., does not

modify equilibria or performances in the vessels.

X is equal to the mass of vapour to the condenser.

Then, the last vessel evaporates a mass of water equal to (X+P 4 ).The
third vessel evaporates (X+P 4+P 3), the second (X+P 4+P3+P2 ), and the
first (X+p 4+p 3+px+p i )

The total evaporation by the multiple effect, E, is the sum of the

above

E = 4X+4P4+3P3+2P2+P,

but
Db = X +p 4+P3 +p2 +p l

We eliminate X. Then

Db =E14+P)4+p212+3P,14

But D, the steam demand without bleeding, is

D =E14+P4 +P3 +P2 +P,

which is the total vapour bled plus one quarter of the evaporation.

The steam economy is then (D - D b) or

4P+2 P2 +4 P3+P4

In general the economy, e, will be

I 2 3 EP n-1
e= -P+-P+-P3+.....+ +.....+ +P„
n n n n a n

-1 2-
for an evaporator station with n effects.

Generally though, one will bleed from the first and second effects
only. Then

2 m wvtng or a team
eracflc,
1
e= -P, + - P2
n n

2.1.3.3 Condensates

The steam or vapour transmits heat which corresponds to its latent

heat of vaporisation (i.e. its enthalpy of vaporisation). All the steam Candensate
used will therefore be transformed into the liquid form, called
condensate. It is necessary to remove this water, whose mass is
equal to the mass of steam or vapour used. If the condensate is not
removed, the calandria will fill up with water and the heat transfer
will decrease.

Condensates contain heat energy, which should in principle be ums of condensate

recovered. furthermore, they should provide a source of hot, good
quality, water for use in the factory.

If condensate is removed and sent away as is, it takes with it all its
sensible heat. If it is directed to a lower pressure environment it will
spontaneously evaporate, or flash, as it readjusts to the new
conditions of pressure and temperature. The quantity of water
evaporated will correspond to the quantity of heat given up, and one
recovers a smakl quantity of vapour which can be added to that
feeding the next calandria. It can be calculated that, in a quad, 5%
more evaporation can be obtained if the maximum amount of
condensate is circulated.

2.1.3.4 incondensable gases

The vapour which arrives in each calandria contains air and foreign Source of gases
gases. These originate from air and gases dissolved in the juice, which
are released on boiling; with cane this is essentially air. Leaks in
vessels or in calandrias, lines, etc., allow air into the system. This can
be the largest source of gas.

_1 3_
 Effect of air In cnlandrW
If these gases are not removed, they accumulate in the calandria and
evaporation will stop, in a matter of minutes in a 3" ° or 4' effect. It
should also be noted that a little air in the calandria can cause the
temperature to drop significantly.

2.1.4 The vacuum system

As noted in section 2.1.3 the multiple effect evaporator operates

under vacuum. A common system is shown below.

Schnnatic diagram or water

and vacuum system

2.1.4.1 Central vs. individual vacuum

For reasons of simplicity and economy a factory may use only one
large, central condenser, one air pump, and one injection water pump.
From a mechanical point of view this is a practical arrangement, but Disadvantage or central System
it has one major disadvantage. Some of the units on the vacuum
system, such as batch pans, can and do cause large fluctuations in the
central vacuum system. Since a steady vacuum, at the correct level,

_ 14_
is essential to the proper operation of multiple effect evaporators, the
central vacuum system is not recommended.

The only completely satisfactory solution to vacuum fluctuations

caused by the use of a central system is to use separate vacuum
systems for each pan and for the evaporator. The disadvantages
include cost; a multiplicity of pipes, pumps, etc.; a higher power
consumption, and more cooling water. The advantages are, however,
considerable. The large vacuum piping of the central system is Advantages of the Indfrldual system

avoided; each condenser is much smaller, and can be located close to

the vessel it serves. A breakdown of one unit does not require the
shutdown ofthe whole factory. The most important advantage is that
the evaporator and each pan can regulate its own vacuum and thus
operate optimally without interfering with each other. A steady and
adequate vacuum remains the most important requirement of
evaporators and pans.

It is possible to obtain very high vacuum levels industrially. In cane Level of vacuum to factorks

sugar factories the vacuum used for evaporators is usually between

15 and 20kPa absolute. Often vacuum is limited by the temperature
of the incoming injection water, which can be high due to high
ambient temperatures, poor water cooling facilities, and lack of
water.

The vacuum is maintained by continually removing the gasses mixed

with the vapour. If air pumping stops, the vacuum will drop
inevitably, in spite of the condensation o£ the vapour.
Amount ortncondtimaNt gas
Lengthy calculations may be done to estimate the amount of air or of per 4of vapour

incondensable gases, to be removed. The basic data needed is at best

doubtful. A useful approximation is 10 to 15 grams of air per
kilogram of vapour produced, or 0,15m3 of air per kg of vapour.

2.1.4.2 Condensers

The condenser is a closed vessel in which the vapour to be condensed

and the cooling water are brought into contact.

In the cane sugar industry, direct contact condensers are used. In this nlerct contact condenarers

system steam, or vapour, is condensed by direct contact with the

cooling water. This type of condenser is efficient and of a reasonable
cost.

- 15-
Direct contact condensers can be further classified. In co-current
condensers, steam or vapour, and the cooling water, travel in the
same direction. In counter-current condensers, the steam or vapour
and the cooling water travel in opposite directions. The counter- Cocmrrent ra. counter-current
current condenser is more efficient, for the same vacuum it uses less
water and requires a smaller air pump. The air is removed from the
coolest part of the condenser and thus has a lower specific volume.

The only real advantage of the co-current condenser is its design

simplicity and thus its lower construction cost. This is, however,
heavily outweighed by the cost of larger air and water pumps.

The distribution of the cooling water in the condenser may be

through spray nozzles, water curtains, or perforated trays.

The amount of inlet water needed per kilogram of vapour can be Calculation or condenarr water
calculated as follows. needed per anit mans of vapour

WATER

MM W
Tang 1,

VAPOUR

MM I
Temp

TAIL PIPE WATER

Mm W•i
Temp t,

An amount of vapour of 1 unit of mass, at a temperature of t, Bask conditions " =nmpdom

requires W units of mass of inlet water, at t l . The tail-pipe water exits
at t2 . Any effect due to the gas removed is ignored in this calculation.
The heat gained by the water is

WXSI-1, x(t2 -tO

Heat babin«
The heat lost by the vapour is

1 x Ll-1, + l x SH„ x (t„ - t2)

The specific heat of water is taken as 4,18kJlkg. The enthalpy of

vaporisation, over a temperature range of 47 to 62°C, is taken as
2380kJlkg. Then

W x 4,18 x (t2 - ti) = 1 x 2380 + l x 4,18 x (tv - t2)

and

569+t,,-t2
W-
t2 - ti

Assuming (t„ - t2 ) to be small, say 5°C, an approximation for W is

574
W= Approxhoation for W
t2 -
ti

We can also fix the following conditions:-

Vacuum of l6kPa absolute, thus tr is 55°C, the inlet condenser water Given set of con&tiam
temperature is 30°C.

Then

W - 569 + 55 - t2

t2 -1 1

or
W - 624-- t 2
t2 - t]

-1 7-
It is now possible to plot W, the amount of inlet water needed per
unit mass of vapour, versus the temperature difference, t 2-tl . This is
shown below.

120 Maw Inlet water 1 weft maw vapoar

100 -
2 .
?80 -
36o .
........ aP-11-zkr............
40
RANGE t
20 ............................ ..............
0
5 10 15 20 25 30 35
Temp. dif. (water out-water in) °C

The quantity of condenser water needed increases rapidly as (t,-t,) Pradlcai mate 1-r 02-tl)
decreases, that is as the injection water temperature increases. On the
other hand it decreases only slowly for high (t 2-t,} values. It is
advantageous to keep a moderate value for (t2-t,}, say 15°C; and
especially not to let it fall below about 10°C.

The temperature profile across a condenser is now considered. t2 will

be lower, or at most, equal to t„. The condenser is a heat exchanger, TemperRture pronk

whose aim is to absorb all the heat of the vapour to be condensed,

using the minimum amount of water. Its efficiency will thus improve
as t2 approaches tri the maximum efficiency will be when t2 is equal
to tr.

The difference (t,-t.) therefore represents the margin by which the

condenser performance is away from its maximum, or, the degree to The Approach

which it approaches this efficiency. The difference (t„-t 2) is known as

the approach. For counter-current condensers this varies between 3 For eommter-curreat condensers
S°C
and I 0°C. A value of 5°C is normally taken for design purposes.

A co-current condenser shows poorer performance with an approach

of 5 to I 1 0C.

-1 a-
The air temperature, t„ will be between t E and t2. In a counter-current
Air temperature
condenser t, will be close to t l; while in a co-current, t, will be closer
to t2.

Finally, the inlet water temperature can vary widely, depending on

weather conditions, on the efficiency of the cooling system, on the
amount of water, etc.

2.1.4.3 Entrainment

As the juice boils and water evaporates, fine droplets of juice are
projected into the vapour space of the vessel, by the turbulence from Fxt,aiRmnt and vapoar v
the boiling process. The droplets also include small bubbles ofvapour
enclosed in a film of juice. The droplets are entrained by the current
of vapour, and are carried away. The faster the vapour moves, that
is the faster the vapour velocity, the higher the entrainment.

Entrainment causes many problems. It results in losses of sugar and

thus contributes to the undetermined loss in the factory. The presence PmWnm orentralameat
of sucrose in condensates routed to the boilers can cause very severe
damage. Sugar entrained in the tail-pipe water promotes
microbiological activity and the formation of acidic by-products. This
affects equipment and/or pollution of the environment.

Entrainment separators are vital accessories to evaporators. They

ERtratmneut repuatom
separate the juice particles from the vapour and return them back to
the juice. They are usually situated inside the top part of intermediate
vessels, but may be found in the vapour line to the condenser, from
the last effect.

The separation of the droplets from the vapour is based on three Separation mechanfgas
processes. Firstly, abrupt changes in direction and/or speed of flow
are used. Secondly, centrifugal force is used, and thirdly,
impingement against baffles can be used.

Finally, the concept of vapour velocity is central to the entrainment

process and to its control. This will be illustrated in detail later. Apart Comm orentrabment
from vapour velocity, unsteady evaporator operations, particularly
vacuum fluctuations, are the main causes of entrainment.

_1 9-
2.2 Calculations

2.2.1 Pressure

Pressure is central to calculations dealing with evaporators. The

concept can also be confusing since there are a multiplicity of
units, and because pressure can be quoted in different ways.

The unit of pressure in the SI system is the pascal (Pa), which is The id (M,kr-2)
defined as 1 newton per square metre:

1 Pa=INm x

Unfortunately pressure is still quoted in non SI units in many cases,

particularly in tables needed to link pressures, temperatures, and
thermal properties required in calculations. The following conversions
will help.

1 bar= 105 Pa = 100 kPa exactly The Gar

1 atmosphere = 101,325 kPa exactly The atmosphere, atm

The difference between gauge and absolute pressure must also be Gauge and absolute presiurrs
understood. A pressure gauge usually measures the amount by which
the pressure being measured exceeds the atmospheric pressure. This
is indicated by adding "g" after the value. The real or absolute
pressure is the gauge pressure plus the atmospheric pressure. A
gauge pressure of 100 kPa (100 kPag) is in fact a pressure of 201,3 25
kPa absolute. Similarly a gauge pressure of -85 kPag is an absolute
pressure of 16,325 kPa.

2.2.2 Quad, no vapour bleeding

We will now look at a quad and do some material balances. This will
introduce a number of basic concepts relevant to evaporator
calculations.

When a vapour is at a temperature corresponding to the boiling point

appropriate to its pressure, it is said to be saturated. Then, once the
saturated steam
steam or vapour pressure has been given, the temperature of the
steam or vapour is defined, or vice versa. Tables dealing with the
properties of saturated steam will then be used.

-20-
In our example we assume that the exhaust steam feed to the first Pressam and tcmperatare rank or quad
effect is at a pressure of 170 kPa (all pressures are absolute). Then its
temperature is 115°C. The pressure in the last effect is 12 kPa; the
vapour will be at 49°C.

There are 4 vessels and the average pressure drop will be

Pressure drop over quad
170-12
= 39,5 kPa
4

We can now calculate the pressures and temperatures in all the

vessels:-

The following schematic diagram can now be drawn

4
Tem perntarea and prMares tP the quad
1 2 3
12 kPa
130,5 91 51,5
49"C
107 97 82
-1• y y
170kPa

11S°C

Clear Jake and syrup

We assume a clear juice brix of 16, a clear juice tonnage of 154 tons
per hour, and a syrup brix of 70.

-2 1-
We calculate the following mass balances.
Mm baLmets
Tons brix in CJ per hour = 154x161100 = 24,64

Tons water in CJ per hour = 154 - 24,64 = 129,36

Tons syrup per hour = 24,64x100170 = 35,2

Tons water in syrup per hour = 35,2 - 24,64 = 10,56

Then,

tons water evaporated per hour = 129,36 - 10,56 = 118,8

This answer can be obtained directly by using the formula

brix CJ
tons water evap 1 hr = tons CJ 1 hr 1-
brix syrup

The amount of water evaporated by each effect is

Evap
oratiom per effect
tons water evaporated per hour per effect = 118,8/4 = 29,7

The amount of exhaust steam needed per hour is thus 29,7 tons, but steam needed
a safety margin of 5 to 10°/o should be added.

The heat transfer coefficients, lc, for each effect may be taken as
follows..-
HTC In each effect

Each effect evaporates 29,7 tons of water per hour; the quantity of

-22-
heat in the vapour in each vessel is given by the product of the mass
of water evaporated and the heat of vaporisation.

Considering the 1' l vessel:-

Heat in vapour, Q, = 29,7 x 1000 x Ofd, at 107°C

= 29,7 x 1000 x 2238

= 66468600 kJ /hr

18464 k lls

The temperature difference, AT, is 115 - 107 = 8°C

The HTC defining formula is Q = k A AT

and therefore

18464 = 2,6 x A x 8

which shows that a heating surface area of 888 or 900m 2 will be

required.

The calculation proceeds in exactly the same way for the other Fadmation of surface am needed
vessels, and it is found that 935, 975 and 1000e, are needed in the
2~°, 3d and 4~' effects, respectively.

2.2.3 Quad, with vapour bleeding

Again a set of calculations will be done to illustrate the procedures

with vapour bleeding. The following conditions apply.

data WMch h avacable

Tons clear juice per hour is 187,5
Clear juice brix is 15
Mixed juice temperature 29°C
Syrup brix is 65

Also available are the evaporation rates for each effect, namely 34,
29, 29, and 29 kg/m 2/hr, for the 1", 2nd, 3"' and 4`s effects,
respectively.

- 23-
The calculation of the specific heat of the mixed juice is done using
a formula given by Peacock (1995):

Cp = 4,1253 - 0,02480413 + 6,7x10 -5BT + 1.8691x 10 -1- 9,27 Ix I0~ sped& heat

where B is the brix and T the temperature in °C. Then Cp is

3,8kJlkgl°C.

The evaporator station, vapour bleeding and juice heaters are shown
schematically below.

Schematic representation of evaporator

The following information can be obtained from steam tables.

steam and vapour data
Exhaust steam: pressure 150kPa, temperature 1 i I °C.
Vapour l : pressure 120kPa, temperature 105°C
Vapour 2 ; pressure 80kPa, temperature 94°C

We can now calculate the heating requirements, given by WxSHxAT,

namely the mass of material to be heated, in kg/hr, its specific heat in unit,

kJ/kg/'C, and the temperature rise in °C. Q, the heat required will
then be in kJ/hr.

-24-
Heater 1:

Q = 187,5 x 1000 x 3,8 x (54-29)

= 178125000lhr

Using vapour 2 at 94°C, 80kPa and 2273 kJlkg, we will need

17812500 / 2273 or 7836kglhr of the vapour per hour.

The calculation proceeds in the same way to show that 8147kgflu of

vapour 1, and 8205kg/hr of exhaust are needed in heaters 2 and 3
respectively. The SH of the juice has been recalculated for 54 and steam m the ors
79°C. It can be argued that it would be more correct to take an
average temperature in each heater, for example (29+54)12 or
41,5°C, rather than 29°C. Although rigorously more correct, it is ,
doubtful whether the difference would have practical implications.

The total evaporation is calculated using the formula in section 2.2.2

mass water evaporated = 187,5(1 - 15165) Water evaporated

= 144 tons per hour

It was shown in section 2.1.3.2 that the total evaporation, with

vapour bleeding, is equal to 4X + 4P, + 3P 3 + 2P2 + P,. Thus

4X+4P 4 +3P3 +2Pz +P,=144

and we know that P4 = 0, P3 = 0, P2 = 7836 and P, = 8147kglhr. Thus

144x1000 = 4X + 2x7836 + 8147

and

X = 30045kglhr Mw of vapour to the condemer

where X is the mass of vapour going to the condenser.

The clear juice feed to the I'll effect is at 93°C. It needs to be heated
to 105°C, the temperature of ebullition in the vessel. The heat needed
is given by

heat needed = 187,5 x 1000 x 3,9 x (105 - 93)

-2 5-
 = 87750OOkJlhr

This heat is provided by exhaust steam at 1500a, 111 -C and Eshaost to beg ca reed
2228kJlkg. Thus the mass of exhaust needed is

mass exhaust needed to heat the clear juice = 877500012228

= 3938kglhr

We can now calculate the total exhaust requirement to the 1" vessel,
namely

Total exhaust required

F

Vapour to condenser 30045

Exhaust to heat CJ feed 3938

Exhaust to H3 8205

V 1 to H2 8147

V2 to H1 7835

The total requirement is 58171kglhr, say 54 tons per hour.

We can now consider the amount of heating surface needed in each

vessel.

First effect : In the first effect the clear juice needs to be heated and
Approxsnafan far heath= area
then evaporated. The area for heating is approximated through the in first effect
formula

area {ml} = 0,1 x mass CJ(tonsllu) x (t z - tly

then

area= 0,1 x 187,5 x(105-93 )

= 225m2

The evaporation rate was given earlier, at 34kglm~lhr. The total Area for evaporation ilrst effect

evaporation needed from the first effect is 30045kglhr, plus

-25-
8147kg/hr, plus 7836kglhr, a total of 46028kg/hr. Thus the area
needed will be

225 + 46028134 = 1579m2 Total area first effect

For the second effect the area is (30045 + 7836)129 or 1306rr Z . Area second effect

The areas are equal for the third and fourth effects, and each is Area third and fourth effects

30045/29, or 1036rn.

2.2.4 Calculations involving the heat transfer coefficient

The heat transfer coefficient concept (HTC) is often used when

evaporators are being investigated. Three cases will be considered.

In the first case the performance of a first vessel is being measured.

The following measurements are available:-
Meawrements made far 1" effect
Flowrate of clear juice = 297 tons per hour
Temperature of clear juice = 1 I I °C
Brix of clear juice= 17,3
Exhaust steam pressure = 202kPa
Vapour 1 pressure = 145kPa
Surface area for heat transfer = 3316m'
Brix of outlet juice = 34,9

Schematic representation

C317,3 brk OMigr

111°C 34,9 triX
297 Vk
The amount of water evaporated is calculated:-

mass water evaporated = massCJ x (1 - CJ brixloutlet brix)

= 149,8 tons per hour

The quantity of heat required, Q (kJ/hr), is given by

mass water evaporated x enthalpy of evaporation

The pressure of VI is given as 145kPa, thus its temperature is

110,5°C, and the enthalpy is 2229kJlkg, from steam tables. Then

Q = 149,8 x 1000 x 2229 = 333904200kJlhr Q - 927SILY/s

= 92751kJ1s

The temperature difference, AT, is now calculated. This is given by

the difference T. - Tom . The juice temperature is equal to the
vapour temperature plus the boiling point elevation, BPE. The BPE
is calculated by a formula given by Peacock (1995) and is found to be
0,6°C. Then

Tom = 110,5 + 0,6 = 111,1°C

The exhaust steam pressure is 202kPa; its temperature will therefore

be120,5°C. Then

AT = 120,5 - 111,1 = 9,4°C AT - 9,4°C

The defining equation for the HTC is:-

Q=kAOT A-33ism'

Then

92751 = k x 3316 x 9,4

and
The HTC b 2Mkwrm=JOC
k = 2,98kWlm'l°C

-28-
This measured value far the treat transfer coefficient can now be
compared to the design value, or to values from similar vessels, to
gauge the performance of this vessel.

In a second case the condensate method is used to calculate the HTC

of another first effect. The following measurements are available.

Condensate flow = 167,0 tons per hour Mcasureratmra awae

Exhaust steam pressure = 207kPa
V 1 pressure = 136kpA
Surface area for heat transfer = 3100m?

At 207kPa, the temperature of the exhaust steam is 121,3°C, and its

enthalpy of evaporation is 2199k7/kg. Then

Q = 167,0 x 1000 x 219913600 = 10200901s Q - 1020091ail5

The temperature of the juice is again that of the vapour plus the BPE.
For a first effect the BPE can be taken as equal to 0,5°C. The
temperature of V1, at 136kPa is 108,5°C. Then

Tjww = 108,5 + 0,5 = 1090C

and T, .",., is 121,3°C. Then

12,3-C 6T -12,3°C
AT = 121,3 - 109

Using again the defining equation:-

102009 = k x 3 100 x 12,3

or
k = 2,68kWlmzl°C

and the performance of the vessel may be compared or assessed.

In case three, a different approach is taken. An existing quad is

assessed for the throughput of clear juice it can handle, with given
steam and vapour pressures, and given values of heat transfer
coefficients. The available information is given below.

-29-
 Dada for case 3

1 2 3
E7tHAUST 1tdk% %kP& 62 M 3skN
230kf
2000m' 130t+m' 1500&

v
SYRUP ss bm

In addition the HTC values were measured and found to be as shown

in the table below.

2,7
2 2,3
3 2,0
4 0,7

Two basic relationships will be used, namely

Two basic equations

Q=kAAT

Q=M.H

where Q is the quantity of heat, in kJ; k the heat transfer coefficient;

AT the temperature driving force, in °C; Mp, the mass of water
evaporated, in kg; and H the appropriate latent heat of vaporisation,
in kJ.

Eliminating Q gives

M.H=kAOT

and

-30-
 kAAT calcuLatlon of the mama

M= of-ater evaporated

"` H
and we can calculate the mass of water evaporated. For the first
vessel this proceeds as follows.

HTC in 1" vessel = 2,7kWlmzls Ic - 2,7kWJm?Is

V1 pressure 146kPa, temperature =1 10,6'C

Latent heat of vaporisation = 2228kJlkg a = 228Wnz
Exhaust steam pressure 205kPa, temperature = 121,0°C

Temperature of juice = 110,6 + BPE

We have to guess the outlet brix of the vessel, to use an average brix
for the BPE calculation from Peacock's correlation, say outlet brix
is 18,9, then the BPE is found to be 0,3°C.
AT -m,iac
Then AT= 121 - 110,9 = 10,1 °C

A - 3DOm~
Heating surface area = 3000m2

Then

27 x3000 x101
Mw = ' ' = 3G,7kg l s
222$
or the vessel will evaporate about 132 tons of water per hour.

The tonnages of water evaporated by the other vessels can be

calculated in the same way, to yield 85, 51, and 20 tons per hour, rofid evaporation - 28k18r

from the 2°°, 3', and 4' vessels respectively. The total evaporation
is then 288 tons per hour.

The formula for evaporation has been used already:-

mass water evap = mass CJ 1- Bx in

Bx out
In this case it is the mass of clear juice which is unknown, while the

-31-
total evaporation is 288 tons per hour. It is easy to calculate the feed Clinw Jake dtrmftut to be
tonnage of clear juice at 357 tons per hour. The maximum tonnage hsddled-357 Ow

of clear juice that the station can handle is thus about 360t/hr; higher
tonnages would cause the syrup brix to decrease.

2.2.5 Vapour velocity

This section deals with an aspect of evaporation related to the design

and performance of entrainment separators. The level ofthe vacuum
used in an evaporator has a marked effect of the specific volume,v g vapour velwity

( m'/kg), of the vapour, with v 8 increasing rapidly as the vacuum

increases. The evaporation rate obviously impacts on the quantity of

vapour produced. Both effects are combined in the vapour velocity
concept, which has been shown to be an important parameter as far
as entrainment is concerned.

Vapour velocity will now be calculated. The effect under study is

represented schematically below.

Schematic diagram of evaporator for the

calculation of vapour velocity

-32-
The vessel body diameter is 4,42m. The pressure of the vapour in the
evaporator body is 13,3kPa. Steam tables are used to show that, at spec Mcvohm e-rraWnZ
that pressure the specific volume of the vapour is 11,2m31kg. The
evaporation in the vessel is

40
evap = 70,2 1 _
( 65
= 27 tons of vapour per hour. Tom vapour Rar- 27

Then the volumetric flow of vapour is

27 x 1000 x 11,2
3600
= 84m3/s. m' vapour la -&1

This volume of vapour flows through a cross-sectional area of nrz

squared metre, where r is the radius of the evaporator body. Then the
vapour velocity, V, is

84
Y=
x(2,21) z
V s S,5nJs in body
= 5,5m/s

and the vapour flows through the vapour space at 5,5m/s.

Say we now have an angle iron entrainment separator fitted in the

vapour space. The separator is constructed so that L = 2x, these
quantities being as shown below.

-33-
The angle BDC is a right angle; D bisects the side of length L, and
the angle at C is a right angle. Obviously BD = DC = X. Then

Sin 45 = ABIL

and

BC -- ~F + XI)
= xF L ,l2
2
Then

L..~F2 L.~2-
AC +
2 2

Thus without the angle iron baffles, the flow of gas over AC uses a
region proportional to L ,4- ; with the baffles the region is reduced
to X, or L12. The reduction is thus

-34-
 L /2 = 1
reduction = "action tam region ror aow

LV-2- 212-

The gas velocity will now be increased by a factor of 2 [2- or 2,8.

Using the results just calculated, the vapour will move at 5,5x2,8 or
15m/s through the baffles. Experience has shown that this vapour
velocity would be too fast for this type of separator; reentrainment
would occur, and sugar would be lost.

Separators using centrifugal force have been found to perform well Vapour vdodHea: evaporators and pans
with vapour velocities below 40m/s. Velocities of 3 to 10mls have
been measured in separators placed in intermediate evaporator
vessels; 20 to 30mls and 5 to 40m/s havebeen measured in separators
placed in A- and C- massecuite pans, respectively. Tests done with
an angle iron separator, in an intermediate evaporator vessel, showed
velocities of 2 to 6m/s.
 3, THE CHEMISTRY

Although evaporation is essentially a heat transfer problem, there are

a number of chemical processes that take place. These cause changes
in the compositions and properties of the dissolved substances.
Furthermore, the condensates produced do not consist ofpure water;
this impacts on their uses in the factory, particularly as boiler feed
water.
6faih arm for sturdy
Four main areas of study can be identified:-

• chemical changes due to the concentration process,

• the decomposition of fructose and glucose,

• the inversion of sucrose, and

• the chemistry of condensates.

Each will be treated separately in this chapter.

3.1 Chemical changes due to the concentration process

A large amount of water is removed during evaporation; with clear More than 9074 of the water h<
juice and syrup brixes of 13 and 65%, respectively, about 92% ofthe Jtdct Is evaporated

water has been evaporated. The concentrations of many chemical

species increase until precipitation occurs. A second effect is that due
to the increasing sucrose concentration, which itself may promote
precipitation of a number of compounds. Finally there is a
temperature effect since the juice is exposed to relatively high
temperatures for periods of time which are not negligible,

The effect ofbrix on solubility can be considerable. Calcium sulphate, Etrec! of brix on the solubdtfes of
at 50°C, has a solubility of about 1400mg11 of a 20 brix solution; in ca(SO,) and SO,
a 60 brix solution its solubility decreases to 400mg11. Similarly silica,
at 60°C, has a solubility of 0,023% (mass/mass solution) in a 10 brix
solution, which decreases to 0,020 at 60 brix.

The following observations have been made:-

Observations rounrmhng
solubMty effects
0 When syrup is diluted to the clear juice brix, its turbidity is
usually higher than that of clear juice.

_36_
 • Those species which are most soluble are found to
precipitate in later evaporator vessels.

• Species present at low concentrations in clear juice

precipitate in later vessels.

*Higher syrup brixes tend to be associated with more scaling

in the evaporators.

Finally, pH can have a mw'iced effect on the solubility of some .ai:

_ ~nnges
species. pH changes do occur during evaporation, firstly t1u ough
chemical reactions, and secondly due to the removal of ammonia as
the juice boils.

The concentration process therefore impacts on scale formation in the

evaporators. It is not the only factor that affects scaling, but it is an
important one.

3.2 The decomposition of fructose and glucose

Although it is known that monosaccharides can be affected by heat,

there is little recent work on the thermal degradation of fructose and
glucose. The experimental conditions are difficult to set up in the
laboratory and the analyses require high accuracy.

Anumber ofbasic laboratory investigations were performed about 20

years ago, in the beet industry. In South Africa, the information
which is available is due mostly to the work of Schaffler.

3.2.1 Fundamental work

Laboratory work, with pure solutions, has shown that fructose and
Work with pure soiudow
glucose are reasonably stable under acidic conditions; some
degradation takes place above 120°C.

Fructose and glucose degrade readily under alkaline conditions;

colour is produced, and acids are formed. The exact nature of the
products is still unknown.

The following results have been established, for pH values of 4,5 and
above.

-37-
 The degradation of fructose and of glucose follows first
order kinetics, namely

First order reacfton

X MJ1-e')

where x is the fructose or glucose lost in t minutes; Mn is the original

concentration of fructose or glucose, and k is the first order rate
constant, in miri', for fructose or glucose,

o The degradation rate constants are affected by pH and by pH aad temperature

temperature.

*The value of k for glucose was found, by experimentation, v,j.,, ofn,e r„te ron,w,ts for c
to be and for F, In pure tohattow

10260 _
log. k,, = 25 310 - 0,017T + 0,77pH
T
where T is in Kelvin, and the pH is the value at T.

Similarly for fructose

8529
log,Q kf = 22,3 - - 0,017T + 0,54pH
T

It is now possible to calculate the quantities of fructose and glucose

that are lost under different conditions of temperature and pH, and
for given reaction times. This has been done in the table below.
 Loss of glucose and of fructose (% by mass) for a
reaction time of 5 minutes

Lasses of F and G with pH and

pH at the reaction temp temperahwe

Temp 6,0 6,5

(°C) %G lost alOF lost a1/OG lost °/uF lost
110 0,l 0,3 0,2 0,5
115 0,2 0,4 0,5 0,8
120 0,3 0,7 0,8 1,3
125 0,6 l,l 1,4 2,0
130 1,0 1,7 2,5 3,1
135 1,7 2,5 4,1 4,5

The impact of temperature and ofpH is clearly evident. It is also Clear Fr is more iabat than glucose
that fructose is more labile than glucose.

3.2.2 Industrial conditions

Although fructose and glucose can be destroyed during many

operations in the factory, this section will deal with evaporators only.

3.2.2.1 Loss of F and G in industrial evaporators

Investigations ofthe degradation of fructose and glucose in industrial

evaporators is difficult, and the information available in the literature
is limited. It is generally accepted that the losses of these
monosaccharides in the evaporators will be higher than those
calculated in section 3.2.1, for the same conditions.

In South Africa, Schafer (1985) carried out an extensive

investigation across an evaporator station consisting oftwo tails, both
with kestners as first effects, followed by Roberts. The following
results were obtained:-

The FIG ratio decreased from clear juice to syrup. Since

0 F I G ratio

fructose and glucose are produced in equal quantities when sucrose

_39_
inverts, fructose must be more labile than glucose. This agrees
qualitatively with the results in section 3.2.1.

*The Glbrix (or GICl, where brix or chloride is an G1brtorG1C1ratlos

unchanging base used as reference) increased from clear juice to

syrup. Thus, more glucose was formed by the inversion of sucrose
than was destroyed thermally. On average about 3,4% more glucose
was produced.

e Assuming that the loss of glucose was negligibly small, it 4,5% of F destroyed
was calculated that about 4,5% of the fructose was destroyed,
between clear juice and syrup.

0 For a retention time of 5 minutes, an operating pH value of Acton r& theoretical loam of
6,0, and a temperature of t 15°C, that is conditions similar to those FRndG

found in one of the kestners, the data in the table o£ section 3.2.1
show that 0,4% of the fructose and 0,2% of the glucose would have
been lost, according to the laboratory work. About 10 times more
fructose was found to have been destroyed in the evaporators, while
glucose was assumed not to be destroyed. These differences are large
and reflect the need for more research in that area.

3.2.2.2 Apparent purity

0 The apparent purity (pollbrix) increased from clear juice to

Decrease in apparent purfty
syrup. This is not due to the precipitation of brix (as scale), but to the
decrease in the negative rotation of polarised light, as fructose is
destroyed.

3.2.2.3 Colour
Colourfeereasa
0 Colour increased by 10 to 15%, from clear juice to syrup.
This is attributed to the degradation products of fructose.

3.2.2.4 pH

0 pH decreased from clear juice to syrup. This was the case C1un=e In pH
both for pH measured at 25°C and for the operational pH. There are
at least two reasons for the drop in pH. Firstly, ammonia is lost as the
juice boils. Secondly, the products of the thermal degradation of

-40-
fructose are generally acidic. Finally, the pH effect is fairly complex
since both brix and temperature tend to lower pH.

3.3 The inversion of sucrose

The most important chemical reaction in the evaporation process is

the inversion of sucrose. There has been much more work done on
the inversion of sucrose than was the case with the degradation of the
monosaccharides.

3.3.1 Fundamental work

Under acidic conditions sucrose hydrolyses readily to form equal

amounts of fructose and glucose. In dilute solutions the reaction
First order 13netics
follows classical first order kinetics, provided the temperature and pH
are carefully controlled.

C)2H22 0 11 + H 2 0 -* C6H12 0 6 + C6H1206

sucrose glucose fructose

The first order rate law for the consumption of sucrose is

Rate Law

d[S]
dt
where [S] is the concentration of sucrose, d[S]Idt is the rate of
change of the concentration with time, and k is the first order rate
constant. Rearranging yields

d[S]
IS] . = -k * dt

which can be integrated readily. Initially, at t=0, the concentration of

sucrose is [S]fl, and at a later time, t, it is [S], Thus

-4 1-
 E S]r d[S] = -k '
ft 5,0 S dt
f"

or

1I7[S]I [s lo - RBI a

In _ -kt
i [S]
[S''o
and

e-Ar = [S] , / [SJ O ........... I .......

(1)

Let x be the amount of sucrose (g/100g solution; molls; etc.) lost in

the time t. Then

x = IS]. - IS],

substituting in (1)

_kf - [S]p - .x
!S] o

x = [S]. - [SJae-kt

and

X = [Sjo (I - e- ") ................... (2)

-42-
Equation 2 shows that the quantity of sucrose lost in a time t, can be
calculated if the original concentration of sucrose, [S]o, and the first
order rate constant, k, are known. [S]a can be obtained by analysis;
it remains to obtain k.

It is well established by experimental work that the rate of inversion The detenoWadon or 4
of sucrose depends on pH, on temperature, and on the concentration
of sucrose in the solution. Vukov, in 1965, summarised the results
obtained by himself, and 10 other workers. He gives equation 3:-

logok=16,91+log,,,(d-c)- 5~0 -pH...... (3) Vukor's equation

where k is the first order rate constant (min'), T the temperature in

Kelvin, d the density of the solution (glcm 3) at T, and c the
concentration of sucrose (g/cm' of solution).

Equation 3 can be used to calculate k when the temperature, the pH,

and the brix of the juice are known. Let the temperature be 108°C,
the pH, at 108°C, is 5,95, and the brix is 22,0. The density at 108°C
is calculated using a formula given by Peacock (1985), namely
Con, e]ation ror density
- + B(B + 200) 1 - 0,036(T - 20)
P
54000 160 -- t

where p is the density in gJcm3; H is the brix, and T the temperature

in °C. Then the density is 1,024g1cm3. The concentration of sucrose,
in glcm3, is given by

brix x density
cone sucrose (g 1 em') =
100

= 22x 1.0241100

0,225g/cm 3

-43-
The temperature is 273+108 or 381 K. The pH at 108°C, is given as
5,95. Using Vukov's equation

log,, k =16,91 + log,o (1,024 - 0,225) -

5681 - 5.95 Calenlatlon ork

= - 4.01934

and k is equal to 9,56x10"'rniri'. If it is assumed that the solution is

kept for 5 minutes under the given conditions, then by using equation
2

e-9'564x10-sx5 )
= 100(1 -
Col.-uladon of the amount of
werox lost by inverdon

= 0,05%

and 0,05% of the sucrose present originally has been inverted.

It is possible to use equations 2 and 3 to investigate the effects of pH,

of temperature, and of brix on the percentage of sucrose inverted.
The effect of pH is calculated for an operating temperature of 110"C,
a brix of 22, and for a retention time of 5 minute. The results are in
the figure shown below.
The effect. of pH on the smomt
of mcrose Inverted

~.a

&.2
a
I-
F

-W1
1o.s

S0.4
al
0.2--

0
4.5 5 5.5 6 6.5
OPERATING pH

-44-
The effect of temperature is now investigated, with a pH of 5,95, a
prix of 22, and a retention of 5 minutes, the results are in the figure.

The effect of temperature on the

amomlt of sucrose inverted

00 95 100 105 110 115 120

OPERATING TEMP [ °O)

Finally, the effect of brix is shown below.

0 o05
The effect of boas on the amount of
sucrose inverted
Doe

p0.p55 -
W

_Z
uJ0.045
N _
O
v 0.04 -

0.033
10 20 30 40 so
JUICE BRIX

These effects can be summarised as follows:-

* For a one unit of pH drop, the amount of sucrose lost can

increase 1 0 times.

i For a temperature rise of 10 degrees, the amount of sucrose

inverted can increase 2,5 times.

0 For a doubling of the brix, the amount of sucrose inverted

-45-
decreases by 10 to 15°/0.

3.3.2 Industrial conditions

The problems associated with the measurement of the amount of

sucrose lost through inversion during evaporation are considerable. Sucrose tnrerdon in "aporaton is
monitored tadlr+ec*
5chiifller (1985) has shown that the sucrose lost cannot usually be
measured directly. The levels destroyed are small, and tend to be of
the same order of magnitude as the experimental error, Sucrose
inversion is therefore monitored indirectly. Two approaches can be
used.

3,3.2.1 The measurement of sucrose inversion in evaporators

Let us consider Vukov's equation

5670
log,,, k = 16,91 + logifl
(d - c) - T - pH

To calculate k, the rate constant for sucrose inversion, in miri', we Daft needed to r acWate x
need the following:-

d, the density of the juice, in glcm3, at the temperature in the

evaporator;

c, the concentration of sucrose, in glcm3 of juice, in the

evaporator;

T, the temperature of the juice, in Kelvin;

the juice pH, at the temperature in the evaporator.

What we can measure is shown schematically below.

 Measurements taken for
VnkOV A equalien

VAP MW I1f,2°C

H P E 0,6°C MCE OUT

am 11,26 BRIX 19,50

TPW 105T pH=, 5,&1
pE;b 6,61

105 + 111,2 + 0,6)

The juice temperature
2
= 108,4°C

11,26 + 1950
The juice brix =
2
= 15,38
pH is measured in the laboratory, usually at 25°C. A quantity called
dpHldt, measured experimentally (this will be discussed later), is
needed to convert the pH at 25°C to that at 108,4°C. In this case
dpHJdt can he taken as -0,0065. Then

6,61 + 5,84
The juice pH 25 =
2
= 6,23

The juice pH,.., = 5,23 - 0,0065(108,4 - 25)

= 5,69

The density of the juice is calculated using Peacock's correlation,

given in section 3.3.1. Then d = 1,00g/cm3.
The concentration of sucrose is given by 15,38 x 1,401 100.
Then c = 0,154 glcm3.

Substituting in Vukov's equation gives

5670
log o k =16,91 + log,, (1,00 - 0,154) - --569
108,4 + 273)

--3,7189

and
k = 1,91xl0 -4min 1

We now need the retention time, t, in the vessel, to use equation 2

X = [ S] ., (I - e - ') ................... (2)

The retention time can be measured by a tracer test, and this can be
Retention thne in vessel
checked by using the volumetric flow of juice and the vessel working
volume. It is assumed here that the retention time was found to be 9
minutes. Then

X = 100 (1 - e- 1,91-10-1 x9 )

that is 0,2°/o of the sucrose in the feed juice has been inverted.

As can be seen from this example, the procedure is not simple.

Furthermore, its usefulness depends on the validity of Vukov's
equation for the industrial conditions investigated.
The second approach
Let us now look at the inversion reaction

C 12 H 22 O il + H2 O -~ C6H12 0 6 + C6HI206

sucrose(342) glucose(180)

-48-
Clearly if amass g of glucose has been formed, then amass 3429/180 stoichtometry
of sucrose has been inverted. If the original mass of sucrose is So,
then the percentage of sucrose lost is 342gx100/(180xS O),

Luring evaporation water is removed and concentrations cannot be

expressed on juice. An unchanging reference is needed. Schaffler Glucose 1 brix and glucose 1 chloride
ratios
(1985) has shown that brix or chloride content may be used. The
amount of glucose formed may then be expressed as

(Glbx)o. - (G/bx)n,

Then, the percentage of sucrose lost, on a mass basis, is

~(G / bx).t - (G 1 bx) N I x 342 x 100

a/o Suc Lost =
180 x (S / bx).

The important assumption made here is that glucose has not been Assutnpfon
destroyed during the process. Some glucose must have been
destroyed, and this is a weakness of the approach.

Let us look at an example, for a kestner vessel. The following

analytical data are available.-
Aftabtk-al data
G°abfxo„, = 1,84
G°/obrix. = 1,77
S°abfx. --- 85,18

Then

1,84 -1,77 342 x 100

°Ia SUC lost = x
85,18 ) 1 80

= 0,2%

It is possible to investigate the effect of glucose being destroyed. If

Lopact of the assumption of no
it is assumed that the results found in pure solutions (section 3.2.1)
apply with juice, then calculations show that the degradation of
glucose will impact significantly when the sucrose loss is low. For

-49-
example, with the assumption of no glucose degradation, one may
find a sucrose loss of 0,02%, in reality this would be 0,04°/x. Both
values, however, are seen as being equal to zero, from a practical
point ofview. With a higher loss of sucrose, say 0,16%, taking a loss
ofglucose 10 times higher than calculated for a pure solution, results
in the sucrose loss increasing to 0,21 a1o. In both cases, the loss would
be reported as 0,2%, anyway.

Some sucrose inversion levels, measured in South African factories,

by both approaches are shown in the table.

sucrose [over" In evapemtoM

Vrdrov and G 1 hrlx

The advantages and disadvantages of the Vukov and Glbrix

approaches to measure inversion in evaporators are compared below.

A comparison orthe two methods

Based more on No measurements required,

measurements than on but analyses sophisticated
analyses
Retention times difficult to Sampling difficult
spa
measure

Assumes that Vukov's Assumes that glucose is not

equation applies to factory destroyed
conditions
 Clearly shows effects of pH, More representative of
temperature, brix and time actual conditions. Picks up
severe short term problems

Very dependent on pH and Glucose can be destroyed in

temperature measurements later effects due to Maillard
type reactions. This can
result in negative values

It is clear that either method can only give an estimate of sucrose

inversion.

3.3.2.2 The measurement of pH

Under industrial conditions it is nearly always impossible to measure Prwtlcal problems rrkh pH
pH at the operational conditions. It is easier to sample the material,
cool the sample and measure the pH in the laboratory at a specified
temperature. Temperature has a profound effect on pH, and the pH
values of evaporator juices at ambient temperatures are significantly
different to those at the operating temperatures. A decrease in pH is
normally experienced when cane sugar juices are at higher
temperatures.

Schaffler (1987) investigated the effect of temperature on pH, for

South African cane juices, by measuring the temperature coefficient dpFVdt
of pH, dpHldt, in the laboratory. This coefficient represents the
change in pH per unit change in temperature. Some of his results are
given below.

Valaes of dgWdt In Sovtb Afrkm

-5 1-
In all cases there was a linear drop of pH as temperature increased;
linear correlations of pH versus temperature, for each material
separately, gave excellent correlation coefficients. The value of the
slopes or dpHldt, however, varied substantially.

An equation, based on 80 juices from five South African factories,

was derived to allow the calculation of dpHldt, from the pH
measured at 25°C:-

dpH Genenal equation for dpaldt

= -0,0339 + 0,015pH - 0,0017 pH I
dt

Schaffler concludes that the equation can be used to estimate dpHldt

for evaporator juices. For very accurate work, however, it is Reservatim
necessary to measure dpFVdt experimentally for the juices under
investigation,

3.4 The chemistry of condensates

The stearn and vapour used in the evaporators give up latent heat and
are transformed into condensates. This yields a substantial amount of
hot water, for use in the factory. Condensates always contain some
impurities; these can be divided into two broad classes.-
Volatile era aortrolatlle species
volatile species, such as ethanol and ammonia, which are m cowle
distilled off,

• sucrose and other constituents of juice carried into the

vapour by physical means, such as entrainment or leaks.

4.4.1 Volatile constituents

The main volatile species in condensates are alcohols, ammonia,

aldehydes, and organic acids.

Ethanol is generally the most abundant species present, ranging from

about 300mg/l in condensates from exhaust steam, to 1500mg/l in V2

-52-
condensate, Acetaldehyde, formed by the oxidation of ethanol, has
also been found. Ethanol is formed by the anaerobic deterioration
process in beet, and by fermentation in deteriorating, burnt cane. It
therefore enters the factory with the beet or cane. Ammonia is formed Am
by reactions involving nitrogen containing compounds, which are
unstable at high temperatures under slightly alkaline conditions, such
as asparagine and glutamine. There is no ammonia in mixed juice but
some (1 to 20mg11) may be found in limed juice. The amount of
ammonia found in condensates depends on the removal of
incondensable gases in the first effect. If this is efficient, then there
will be less ammonia in the condensates. High pH levels (8 to 9) in
condensates will generally be due to high levels of ammonia.
Ammonia and oxygen attack copper; this probably causes the
presence of copper in condensates, from the copper and brass
calandrias and tubes.

A number of organic acids have been found in condensates; some

results are given below, for V2 condensate:-

Acetic 1 62

Butyric 23

Propionic 12

Formic l _. 2

At least two mechanisms can account for the formation of acids. The
first is a sequence of reactions,
starting with a-amino acids, which
degrade to aldehydes, carbon dioxide and ammonia:
H
I
R-C - COON -~P- R- CHO + COz + NH3
i
NHx I
oxidation

R - COOH

-53-
These reactions can take place under the conditions found in the
evaporators.

The second mechanism involves the hemicellulose fraction of

bagasse, which contains a small amount of acetate esters. These react
with lime, and hydrolyse to calcium acetate, which in turn produces
volatile acetic acid in the evaporators. Experimental work carried out
in a diffusion factory showed conclusively that the levels of acetic
acid in mixed juice and in V2 condensate were linked to liming in the
diffuser. Some measurements done in a South African factory, where
mixed juice, clear juice, feeds to the first and second effect
evaporators and the VI, V2, and V3 condensates were analysed, are
given below.

It was also found that:-

- an increase of 10°C in the diffuser produced an additional

200 to 300 mg acetic acid on brix

an increase of half a unit of pH increased the acetic acid

concentration by about 200mglkg brix.

The condensate pH will be affected by the concentrations of

ammonia, of carbon dioxide, and of organic acids. When high levels
of acetic acid are present, it has been shown that there is a good
relationship between condensate pH and the concentration of acetic
acid; the condensate pH will drop to below 7 when the acetic acid
concentration reaches about 20mg11, as shown in the graph.
 conaemate pry =d acethc aetd
concentration

75-

x
a
iu
r
a
28.5-
!ll

55-

20 40 80 80 100 120 140

ACETIC ACID IN CONDENSATE (ffvM

4.4.2 Non-volatile constituents

The major non-volatile constituent of condensates is sucrose, with

minor amounts of other juice constituents. These find their way into
condensate through entrainment or leaks. This section will Anaanb orcondeasate for sucrose
concentrate on the analysis of condensates for sucrose traces.

Analytical methods for sucrose, particularly at trace concentrations,

are sophisticated and costly. Generally, high pressure
chromatography, or HPLC, has been used, mostly in research
laboratories. At factories, colorimetric methods, which are simple
but not specific for sucrose, have been used for many years. Two
such methods are the phenol/sulphuric acid, and the
resorcinol/hydrochloric acid methods. The latter has been well Resorctmot I $c1 method
investigated in South Africa, one of its advantages being that it can
be automated, using an autoanalyser system. It is not specific far
sucrose; ethanol, acetic acid and ammonia, at concentrations up to
1 Uamgll have no effect on the response, but aldehydes, other organic
breakdown products of monosaccharides, and nitrates, for example
do affect the response. The following steps minimise the
interferences:-

the reagents, particularly the acid, must be of good quality

• enough ferric chloride is added to the reagent to overcome

-55-
the sensitivity of the method for iron

• the recommended wavelength is 480nm (not 520nm)

-basic lead acetate (10 drops per 20cm 3 of sample) preserves

the sample, and tends to remove some of the interfering species. It
also flocculates samples which contain suspended matter; the
autoanalyser cannot handle suspended solids.

Nevertheless, the resorcino11HC1 method can pick-up significant

quantities of non-sugars. Concentrations (mgn) of sucrose in
condensate samples analysed by three different methods, in South
Africa, are given below.

Comparbao of m saerese aped

MCthOd WLC) with two
colorhoetrie o ws
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

1 Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation. The fundamentals
b Evaporation. The practice

In preparation:-

Diffusion
Crystallisation
Pan boiling
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
EVAPORATION
THE PRACTICE
 STS'

Sugar Technology For Students

EVAPORATION
THE PRACTICE

Prepared by G R E Lionnel

Study Text 6

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 41351
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright ,J 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISSN 0-620-24197-7

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
251-laleric Rd, Durban North, 4051, KZN, RSA.
 INTRODUCTION

A general introduction to evaporation has been given in Study Text

5, Evaporation: The Fundamentals. That unit covers basic concepts
dealing with energy, heat, and multiple effect evaporation. Various
calculations are given in details. Finally, the chemistry involved with
evaporation is discussed.

For many years Roberts vessels and Kestners were the main types of
Eyodpmeut : Now dedgm
evaporators used in the sugar cane industry. There has, however,
been considerable developments recently, and a number of designs
new to the cane industry, have been tested with cane juices, and some
have been introduced on the industrial scale. A section on equipment
is found in this Study Text, titled Evaporation. The Practice.

Considerations particular to the cane sugar industry have always

formed an important part of this study programme. This approach Tne TeC

continues with evaporation, and the section titled The Technology is

an important part of this Study Text.

Finally, the bibliography, for both Study Texts, is given at the end of Mbaoffmpbr
this unit.
 2.TRE EQUIPMENT

2.1 Evaporators

2.1.1 Long tube climbing film

Keatnera
Long tube climbing film evaporators have been used mostly as first
effects in the cane sugar industry. They are often called Kestners,
after their inventor, Paul Kestner.

The main advantages of the Kestner are its short residence time, its
ability to contain much heating surface in a single vessel, its high
coefficient ofheat transfer and low levels of temperature differences.

It consists of long vertical tubes inside a cylindrical shefl. As many as

5000 tubes may be found within a single shell. The liquor to be
concentrated is fed to the bottom of the tubes, where it is heated by
steam condensing inside the shell. As vapour is formed in the tubes,
it carries the liquor up the tube as a thin film against the tube wall.
Heat transfer is favoured by the decreased distance between juice and
wall, and by the high juice velocities.

At the top ofthe tubes, the mixture of concentrated juice and vapour
exits and is separated in a separator, usually of the tangential type.

SUARAIUR

C?OT~NSAIB

OONCOMA'nm
1[B8
The tubes are fi to 10 metres long, 7 metres being common in South
Africa, and 27 to 51 mm in diameter, 50, 8mm being found generally
i n South Africa, with a wall thickness of 1,2mm. Stainless steel tubes
are preferred since they are not subject to steamside corrosion and
are longer lasting, particularly if mechanical cleaning is used.

The separator in the cane sugar industry is generally located outside

the evaporator itself. It consists oftwo sections, a lower one in which
juice collects and is withdrawn to feed the next vessel, and an upper
one through which vapour is withdrawn. This upper section often
contains an entrainment separator, usually a wire mesh pad. The
diameter of the separator depends on the entrainment device used,
and is usually similar to that of the evaporator vessel.

The liquid feed should be distributed evenly below the bottom tube
plate. Recent work in South Africa has shown that there are two
basic requirements for the feed to a Kestner. The first is to have
single phase feed in the feed ring, that is to have liquid only, with no
flashing; this ensures even distribution of the feed to all the tubes.
Secondly, enough juice must be available to ensure that the feed ring
is operating at design capacity. As far as feed temperature is
concerned, it is believed that it should be approximately 1°C below
that the boiling point of the juice at the vapour pressure of operation.

The lid is detachable, to facilitate access for cleaning. A safety device

is essential to prevent removal of the lid while there is still positive
pressure in the vessel.

Experimental work in a pilot plant has shown flow throughputs of25

to 140 kg/hr/tube to be possible, as first effect. In South Africa, 75
kg/hr/tube is the average in industrial first effects, while about 42
kg/hr/tube are found in second effects. Experimental work has shown
that, in first effects, the throughput should not fall below about 60
kg/hr/tube for good performance, in terms ofheat transfer coefficient.

Heat transfer coefficients (HTC) in industrial Kestners has been

measured at 2,3 kWWl°C in first effects, and 1,8 kWlm?l°C in
second effects_

Juice residence times in Kestners has also been measured. In fast

effects a time of 2,4 minutes is considered short, being about 15% of
that in Roberts vessels. Values of 4 to 5 minutes have also been
measured.
Finally mechanical cleaning is possible but becomes a strenuous
undertaking as the number and length ofthe tubes increase. Chemical
cleaning is also possible.

2.1.2 Roberts vessels

One of the main differences between Kestners and Roberts vessels is

Roberb
the tube length. In Roberts, tubes vary from about 1,9 m to 2,8 m,
with a diameter of 38 to 51 mm.

There is no juice/vapour separator associated with Roberts vessels. Mengaginp spxe

The vapour space of the vessel itself acts as a disengaging space and
a height of about 3 to 5 m between the juice surface and the dome is
common. A rule of thumb is that the height of the cylindrical part of
the vessel should be about twice the length of the tube.

VAPOUR

EVTRAN-WFNT SEPARATUk

CA4ANORTA

WCONDENSABI.E CMS

SYRUP
The diameter of the vessel has an effect on entrainment since vapour
velocity is affected by the cross sectional area.

Juice feed is normally through a feed ring, inside the vessel, with FKa ring
slots. Again there should be no flashing in the feed ring.

The calandria is where the heat transfer takes place. The distribution
of steam or vapour into the calandria should be as uniform as
possible, and bales may be used. The downtake returns the boiling
juice to the base of the vessel. Its diameter varies from 114 to ll8 of
the vessel diameter. Some vessels do not have downtakes; there is
then no provision to return the juice to below the calandria and it
must be assumed that the tubes which are boiling less efficiently than
average act as down comers. There are two basic types of
downtakes, the sealed downtake and the open downtake. Typical
arrangements are shown below.
An entrainment separator is essential. It can be located in the top of
the vessel or consist of mesh, or baffles, arresters in the body itself.

In most evaporators the tubes are arranged in a staggered

configuration, which permits the greatest number of tubes per unit
area of tube plate, for a given distance between the tubes. This
staggered arrangement is shown below.

10-0 a_

!K = distance between tubes

P - pitch or distance between

tube centres

AB' BC '° p (pkch)

Tube diameter - d
It is possible to calculate various ratios concerning tube arrangements
in tube plates. All the following calculations are based on the
diagrams on the previous page.

The four quarters of the tubes inside the parallelogram ABCD have
an area equal to nd214.

The corresponding area of tube plate is equal to the area ABCD. This
will now be calculated.

Using geometry
height
Sin 60 =
P

and

height = 2 x P

base =px Cos 60 = 0,5p

Then

ABCD =2x Px
2 2
p +(p-U,5p) x
2
VP

2 Arcs oiplade AHCD

P
2

Let K. be the ratio of area of holes to that of the total plate. Then

area of holes
total plate area
Again referring to ABCD, the area of the holes is nd x14, while the
-.r3-
total plate area is p'. Then
2

Zd 2 14

2P

It is now easy to show that

d Relationship between pitch

p = 0,952 and tube diameter
e

In industrial evaporators ICe is approximately equal to 0,5. Then

p = 1,4d

that is the pitch of the tubes is about 1,4 times their diameter.

We can also calculate X, the plate distance between tubes. Then

X --p-2r

=p-d

that is
Relationship between x and
X = 0,4d tube diameter
Typical values for the heat transfer coefficients in Roberts vessels,
and the juice and vapour temperatures, are shown in the following
table.

The residence time in Roberts vessels usually ranges from 5 to 10

minutes. This can vary considerably and tracer tests are needed when
precise values are required.

Operating juice levels in Roberts vessels should be kept about hall;'

way up the first sight glass, which normally corresponds to about 50
nun above the top tube plate.

Finally, cleaning can be done mechanically or chemically.

2.1.3 Falling-film, tubular, evaporators

Falling-film, tubular, evaporators are popular in the beet industry, but

applications in the cane industry have been slow. When used with
cane, the choice seems to have been based on energy considerations.

This type of evaporator consists of a cylindrical vessel with the feed

being spread, at the top, on a vertical bundle of tubes, by means of a
juice distributor. Juice then flows as a film down from the top to the
bottom, with the vapour also flowing from the top to the bottom.
Thus both juice and vapour travel in the same direction. The
concentrated juice and the vapour reach the base of the vessel and the
vapour exits through a separator.
 Srbematic diagram of a tubular
Uhmg-SLn evaporator

Tubes
The tubes are usually made of stainless steel, with a diameter of 38
to 51 mm, and are 7 to 10 m long. It is generally recommended that
a wetting rate of 12 to 15 kg of juice per hour, per cm of tube be
provided.

The juice distributor is an important part of the evaporator, and its Juice dhtrtbutor

design is vital to the operation. The distributor must not be blocked

by suspended matter, for example scale, and juice velocities are
important. Many designs are available and both steady and uniform
flow is essential. A nozzle may replace the distributor and this is
being evaluated in South Africa.
Separator
The separator can be incorporated inside the vessel or can be a
situated outside the evaporator itself. Centrifugal or gravity
separation may be used.

A pump may be used to ensure correct flow, through recirculation. FrrC

The heat transfer coefficient has been found to be about 2,4

kW/m'/°C, with cane juice, in a clean evaporator used as a first effect.
After about 3 weeks of operation the HTC decreased to about 1,4

-1 0-
kW/m2/°C.

The residence time is short, with work in India showing times of 0,5 pAiention tow
to 0,6 minutes, but other workers quote values around 2 minutes. In
South Africa little to no inversion has been found to occur. Cleaning
must be by chemical means.

One such vessel has been operating in South Africa and the
experience (Rousseau et al., 1995) shows promising results. A
second evaporator is being installed.

2.1.4 The plate evaporator

This is a different concept, not utilising tubes as such. The heat

exchange surface is in the form of plates or cassettes_ Both rising and
falling film configurations are available. The plates can be inside a
pressure vessel, or an external separator may be present.

Again this design is popular in the beet industry where significant

energy savings have been achieved through its application.

The plates are usually about 0,6 mm wide with plate gaps of 10mm. Tlales
They are made of stainless steel, and gaskets are fitted between
them. Plate area is about 2,6 m 2. The recommended wetting rate is 16
m3 per hour per 100m 2 of area.

HTC
The heat transfer coefficients in a second effect at 3,5 kWlmxl°C,
were about 40% higher than found in Roberts vessel. The general
consensus is that HTC values are high under optimal operating
conditions, but are sensitive to control, fouling and general
operations.

Retention times, found with beet juices, were short at claimed values Resl$ence thne
around 30 seconds. These times are stated to be about l/IOth those
found in Roberts vessels, for the beet industry.

Plate evaporators have a number of special requirements:

• The gaps between the plates are small. The feed juice must
therefore be free from suspended matter. In the cane
industry sieving or filtration may be needed.
 • It is critical to have uniform and steady feed distribution, at
the designed flowrate. Juice flow control must be good.

• Cleaning must be by chemical means, and must be efficient.

Opening the heater for physical cleaning may damage the
gaskets which are expensive.

2.2 Entrainment separators

Entrainment occurs in nearly all processes involving gaslliquid

contacting. It can be reduced by proper design and operation, but
cannot be totally eliminated. Recovery devices, called entrairiment
separators, are therefore installed in evaporators to recover the
entrained liquid.

There are four main types of separators:

• Centrifugal separators Mentyp"orsepantam

• Zigzag bales

• Impingement separators

• Wire mesh pads

2.2.1 The centrifugal separator

Centrifugal force is used to throw the entrained droplets against an

outer wall where they collect, drain, and are returned to the vessel.
Series ofvanes or circular flow channels are used to force the vapour
to flow in a circular path. These separators are usually situated in the
dome of the evaporator.

2.2.2 Zigzag baffles

These are a specific case of the impingement type of separator. They

consist of series of parallel plates with bends. They are located across
the cross-sectional area of the evaporator body. They are sensitive to

-1 2-
the vapour velocity. Metal or plastic may be used for construction.

Sehemadc dla=ram of a z4pn baffle

2.2.3 Impingement type

As with the zigzag bale, the impingement separator causes the

separation of the liquid droplets.

schematic dlagram of an
knpWSement separator
2.2.4 Mesh pads

Multiple layers of crimped, knitted mesh can act as an impingement

separator. They are typically 10 to 20 cm thick, and the mesh density
can be changed. They come in segments and, contrary to zigzag
baffles, can be made to fit a vessel of any shape. They can however
foul and plug; a strict washing programme is necessary.

schematic dia;ram of a mesh in a

Separator

2.2.5 Washing arrangements

In final effect evaporators entrainment can be high due to high vapour Cteaning mesh separators
velocities. If mesh separators are installed, washing is essential.
Experience in South Africa shows that the following conditions may
be used. Wash water temperature should be about 80°C, about 50 I
of water per m2 of mesh are required, and a 5 minute wash every hour
was adequate. This resulted in a mesh separator needing no removal
for more than three month of operation. Steam or vapour may also
be used for cleaning mesh separators. Two cleaning arrangements are
shown schematically below.

-1 4-
 Gleaning ofa umsb separator wdtb
hotrrater

p 4

a 0

Cleaning with vapour

2.3 Condensers

The condenser is a heat exchanger, between the vapour and the cold
water. This exchange will be more efficient as the contact between
RAW ft-Ay coaaemem
the vapour and water is more intimate. Counter current, rain tray type
condensers are well utilised in the South African industry. Some
design details are as follows. Vapour velocity is about 60 m/s;
injection water velocity is around 1,5 m/s, and the air velocity is 12
m/s. A perforated plate distributes the water; it usually has holes of
about 12 mm diameter, with an average sized condenser requiring
2000 to 3000 holes. A splash plate is used to even out the water
distribution. A schematic diagram is shown below,

7
WATM J 9I.AM PLATE
[ Y
Am

P®lFORATW
'4'_ 1 MAIM

Y l- .
------------

WATFY

VAPOVA
2.4 Condensate

There are two different conditions for the removal of condensates.

The calandria pressure can be above atmospheric pressure, in which calandda above amampberk

case gravity may be used, since the condensate will flow freely. The °ressum

pipe must not however be empty and thus allow steam or vapour to
be lost. A steam trap is necessary. This is a device containing a float, steam trap
which will open only when water reaches a given level. Then an
equilibrium is reached and the float opens to let only water escape.

The calandria pressure can be at sub-atmospheric levels. A number

of devices may be used

• Sealing legs, as shown schematically below.

seafts IM

The calandria of the 4'' effect will be at the same pressure as the
vapour ofthe 3' vessel, say 50 to 52 kPa absolute. This corresponds
to a head of water of about 5 m, which with a 25% safety margin
requires a leg of about 6 m; one needs a vertical distance of 6 m
between the bottom tube plate of the 0 calandria and the top of the
weir in the last compartment. This does not cater for accidental high

-17-
vacuum levels and the literature recommends about 10 to I 1 m. This
is often a practical problem in terms of space.

The three condensates are at different temperatures and thus should

discharge in three separate wells. This prevents accidental flashing if
the hotter condensate reaches the highest vacuum leg.

Siphon. Siphons pass condensates from one calandriato the

next and recover the flash. A U-tube or inverted siphon is used.
Length and height must again have a generous safety margin. This
can once more cause practical space problems.

• Flash pots. These are small vessels situated below the

Fhtsh pots
evaporators, in which flash takes place. They do not require the
vertical space of the two previous devices but need relatively complex
piping. They should have sight glasses to allow visual inspection of
what is happening inside them.

2.5 Incondensable gases

Incondensable gas vents in the calandria should be located as far as

possible from the steam or vapour entry point into the ralandria. The
pipe should start about 100 mm, at least, from the base of the tube
plate, to avoid contact with condensate.

For calandrias where the pressure is above atmospheric,

Incondensable gases are allowed to escape to atmosphere through a calaRaria above xtincepherk
P
regulating valve. Flow is set to allow a small wisp of steam to be seen
escaping continuously.

For calandrias under vacuum, the Incondensable gases are led to the
vapour space of the same vessel. The gas vents and pipes from
successive vessels must be made progressively larger because of the
accumulation of gas in this system. As a rule of thumb, one can use
the following

_l8_
 1' vessel 13 mm pipe
2' vessel 13 to 19 mm
3"° vessel 19 to 25 mm
4' vessel 25 to 32 mm.
 3. THE TECHNOLOGY

3.1 Energy

Many cane factories diversify their operations, depending on local

conditions. Thus, back-end refining, bagasse exports to by-products, r comiaersuom

the production of electricity for the grid or for irrigation, can be

major considerations. These increase the demand for the self-
generation of energy, while often reducing the bagasse available for
steam generation. As a consequence it is often necessary to increase
boiler capacity and to burn fossil fuel; at the same time the amount of
steam for sugar processing must be reduced as far as possible.

Reid and Rein (1983) give detailed energy balances for a modern
South African factory. High pressure steam °Io cane is about 48%, for
a mill providing fibre for by-products while burning a minimum of stmm to the ev.p
omwrs

supplementary fuel. The major user of exhaust steam (203 kPa;

121 °C) is the evaporator station, consisting of a quintuple; of the 306
tons of exhaust produced per hour, the evaporators consume 276
tons or about 90%. Thirty seven tons of V 1 (164 kPa; 114°C), and
215 tons of V2 (130 kPa; 107°C) are bled per hour.

The following three aspects of technology are relevant to energy

savings in the cane sugar industry -

- Pinch technology. This can be used to assess the thermal

efficiency of the evaporator station. Pinch technology has been
much tedwaou
quoted (Singh et aL, 1997) as being an efficient tool to do so. There
is no doubt that new evaporator concepts and designs are being
adopted in the cane sugar industry because of energy considerations.

- Vapour bleeding. Vapour bleeding is a well established

process for the efficient utilisation of stearn. Normally in the cane
sugar industry, only vapour 1 and 2 are bled. They feed juice heaters
and the pans. Vapours from 3r d and 0 effects are at relatively low
temperatures and would require large surface areas for heat transfer.

- Condensate management. Condensates are utilised in two

main ways, to recover energy. Routing condensates to the next
calandria recovers energy through flash. The complete recirculation
of condensates in this way, for a quadruple effect, would give about
5% more evaporation. The use of condensates as a source of hot

-20-
water in the factory is the second, indirect way, of saving energy. The
most important use is as boiler feed water; here the early, relatively
uncontaminated condensates are selected.
condensates From

First effect condensates may be sent to the boner water feed

tank, via steam traps, or they are sent via steam traps to the second i. effect

vessel flash pot, any excess is then sent to the boiler feed water tank.

Second effect condensates are sent via steam traps to the Y d 2" enkd
effect flash pot, with any excess to the boiler feed water tank or to
the factory hot water tank.

Third effect condensates are sent via steam traps to the flash 3' effect

pot and calandria of the 41h effect. Any excess is sent to the factory
hot water tank.

Fourth effect condensates are sent to the factory hot water 0 effect

tank.

All condensates sent to boiler feed water are tested in line for
Test for entralnnrent
conductivity, to be rejected as feed water ifthe conductivity indicates
a possibility of entrainment of sugar.

3.2 Kestners

The use of long tube, climbing film evaporators (Kestners), as first

and second effects is well established in South Africa. Their large
capacities, coupled with short residence times, allow high evaporation
rates and efficient vapour bleeding. Recently much work has been
done to optimise the operation of Kestners in South Africa. Two
main conclusions have been reached

• Feed flow rate is possibly the single, most important rate

operational parameter.

• Fouling of the tubes is the practical limit to good

Tube scaling
performance.

Both these concepts are illustrated in the following figure, based on

the pilot plant work done mostly by Walthew (1995, 1996).

-2 1-
 20 40 60 80 100 120
FEED RATE (kg/hr/tube)

For Kestners as first effects, a minimum feed rate of 60 kglhrltube is

Minimum Bow rate for I' efred
essential. Based on tube diameter, this corresponds to 3,8 kgthrlcm XeSftWr%
of perimeter, for a tube of 50,8 cm diameter. It is interesting to note
that the heat transfer coefficient (RTC) does not decrease as flow
rate increases.

In the South African industry, for 54,8 nun tubes, the range of flow
rates varies from about 30 kg/hr/tube or 1.9 kg/hr/cm o£ perimeter,
to 82 kgfhrltube (5,2 kg/hr/cm). The average for eleven V effects
Kestners was 63 kg/hr/tube (3,9 kg/hr/cm), which is just about the
minimum recommended.

For Kestners as 2`d effects, an average given in the literature is 42

kg/hr/tube (2,6 kgfhrlcm perimeter for a 56,8 mm diameter tube).

These findings have prompted at least three South African factories Feed recycling In Kestnen
to install juice recycling on their Kestners. A connecting pipe has
been installed with a non-return valve, between the juice outlet from
the I" effect separator, and the feed line to the I' effect evaporator.
The practical objective has been to obtain 72 kglhrltube.

It is essential for the feed flow rate to be steady. Recycling does not

-22-
i mprove the HTC directly but creates operational stability and
reduces fouling.

Good feed distribution has been found to be a prerequisite for

Peed distribution
efficient operation. Recent work by Walthew (I 996)and mathematical
modelling by Peacock (1997) have shown that the feed should not
flash in the feed ring. Feed temperature should be 1,5 to 2°C below
the expected boiling point of the juice; flashing seems to disrupt even Feed temoperaturt

distribution. It should be noted however that the feed temperature

must not be too low since boiling must start within a short distance
up the evaporator tube.

James el al. (1978) query whether Kestners should not be used as

later effects. They support this claim with calculations which seem to
favour Kestners over Roberts as later effects.

3.3 Roberts vessels

Roberts vessels tend to be taken for granted. In South Africa little

work has been done recently with these evaporators, particularly
when compared to Kestners.

It should be noted that the single phase feed recommended for

Feed temperature
Kestners does apply to Roberts also.

Investigations done in 1981 (Smith and Taylor) have shown that very
low pressures in the last effect are in fact detrimental, reducing HTC
values, due to viscosity effects. Evaporation can decrease by about Pressure bo lag effect
10%. The results of some of their calculations are shown in the
following figure, and it is evident that the optimum pressure is about
16 to 20 kPa absolute, corresponding to 55 - 60°C.
 190
10 15 20 25 30 35
Last effect pressure (kPa abs)

3.4 Falling film, tubular

The falling film, tubular evaporator has been introduced to the cane
sugar industry basically from an energy saving point of view. It is
claimed that it allows high temperatures but with short residence
times. The literature quotes the following residence times

Effect 2nd 3rd 4d' Retention time

Residence time (min) ® 1,4 1,7 2,2 4,1

It is also stated that, with cane juice, the flow rate should be at least
200 kg/hr/tube, or for tubes of 50,8 mm diameter, about 12 kg/hr/crn Feed flow rat"
of perimeter. These are high flow rates when compared to those
recommended for Kestners.

Two tubular falling film evaporators operate in South Africa, as l"

and 2' effects. Inversion across the vessels has been found to be low.
Juice recycling is vital to ensure the correct wetting rate. Operation
and control have been said to be trouble free.

3.5 Plate evaporators

Again the use of plate evaporators has been driven by energy

-24-
considerations. The results obtained in the recent, and first,
i nstallations in the Southern Afi ican industry have been less clear than
was the case with the falling film, tubular evaporators. A number of Appl#catlan with carte Juice
concerns were envisaged

The effect of fouling under local conditions was unknown.

• Cane juice is more turbid than beet juice and tends to

contain more particulate matter. Sporadic carry over ofclarifier muds
does occur.

• Operating conditions in terms of flow control is not always

as good as required. Possibilities of dry out periods are very real.

It was clearly evident from pilot plant work in a local factory that
uniform and steady juice distribution was vital. Generally the rates
required were around 15 tons per hour per IOOm 2 ofplate area. Good
heat transfer coefficients were obtained, with high juice throughputs.

The results obtained with three new industrial plants were mixed. In
one factory where the evaporator was installed recently, the results
were seen as promising although the evaporator has operated for a
short period of time only. In the other two factories serious problems
arose, through poor juice distribution, caramelisation, cleaning
difficulties, and design/capacity problems.

3.6 Heat transfer coefficient values

A summary of heat transfer coefficients (kWlm2/K) measured in

various evaporators operating in the Southern African industry is
given below.

-25-
3,7 Control of evaporators

Evaporator control may involve the following major variables

- Clear juice feed rate to l" vessel.

• Steam flow rate or pressure to 1' vessel.

• Liquid level in evaporators.

• Final syrup brix.

• Absolute pressure in last effect.

The control philosophy will also depend on the type of the

evaporator, for example Kestners, Roberts, etc, and for Roberts
vessels whether they have open or sealed downtakes.

Generally very steady conditions of juice flow, steam supply and

vacuum are prerequisites to successful evaporator control.

In Kestners, liquid level is not usually controlled. For a 1" effect

Kestner, the Roberts 2°d effect can be used to control the flow to the
Kestner. Unsteady flows, or large fluctuations in vapour being bled,
for example when a batch pan stops or starts, can cause oscillations.
These are made evident by pressure swings, with the vessel boiling
and not boiling in turn, and by large ejections of juice into the
separator. The practice of recycling the feed should help in
eliminating this problem.

Finally, the use of neural networks has recently been proposed for
evaporator control.
3.8 Evaporator scale

The formation of scale in evaporators, also called evaporator fouling,

is a major cause of poor heat transfer in the cane sugar industry. As Prardeat impact of evaparatar
xafg
a result of this fouling either

• the evaporator station is over designed to allow vessels to

be taken off-line for cleaning, or

• the factory must stop crushing at regular intervals, to allow

the vessels to be cleaned.

3.8.1 Mechanisms of scale formation

Scale formation in evaporator tubes is a complex process. The

following mechanisms can be involved.

• Concentration process. As water is evaporated, solubilities Concemmtton proem

are reduced until precipitation takes place. The most soluble species
and those present at the lowest concentrations will be found as scale,
i n the later vessels. Generally the higher the syrup brix, the more scale
is produced. It is accepted that pH will also affect the solubilities.

• Chemical reactions. High temperatures and retention times

will cause chemical reactions to take place. Sucrose can cararneiise,
and the monosaccharides can decompose to form organic acids; these
in turn react with calcium ions, resulting in the fonnation and
precipitation of organic calcium salts.

• Particle deposition. Cane juice contains much suspended and Parttcte depe&ion

colloidal matter. The effects of suspended matter is not clear; it may

act as nuclei for the crystallisation of various species, it may attach
itself to the tube wall and encourage deposition of scale. It is believed
that juice velocities in the tube, and pH are important. The state of
the tube surface, on the juice side, has been considered. Tests were
done in a pilot, two tube, evaporator, where one of the tubes was
highly polished, by a commercial firm specialising in this type of
work, while the other was used as is. Juice was concentrated from 20
to 60 brix in 100 hours, with recycling. No difference could be found,
either in terms of HTC (3,8 kWIm ZI°C, for either tube), or in terms
of fouling resistance (1,8 and 2,4 m"ClkW, for the polished and
unpolished tubes respectively).

_Z7_
 • Operational factors. This is possibly the most important
factor in cane sugar factories. Low and/or erratic juice flow rates
result in severe fouling. In the worst cases, dry-out occurs and tubes
or plates are blocked. It has been well demonstrated that steady
operations, with the correct juice flow rate, reduce fouling and allow
longer periods of operations before cleaning is required.

3.8.2 Chemical composition of scale

3.8.2.1 Sampling

Sampling evaporator scale is not easy, particularly with respect to

representativeness. When mechanical cleaning is used, some
dissolution may take place, while the sodium hydroxide used in
chemical cleaning could leach out some of the scale constituents.
Finally, in wet scales, fermentation can occur and the acids formed
could change the composition.

3.8.2.2 Analytical techniques

• Drying. The scale sample is dried at 1 la°C, crushed and

subdivided.

• Asking. A sub-sample is ashed at 1004°C; this gives a loss

on ignition; only the oxides remain and the losses based on this
procedure.

• XRF. X-ray fluorescence is used on another sub-sample, to

yield information on the inorganic elements, for example SiO, CaO,
Mgo.

• XRD. X-ray diffraction is used to identify the crystalline

phases, both organic and inorganic. Thus, calcium oxalate, for
example, will be differentiated as either the monohydrate or
dihydrate; calcium carbonate crystallises in three different forms,
which can be identified.

• HPLC. High pressure liquid chromatography is used for

organic acids.

• Conventional analyses. These are used as required, for

specific information.

_2g_
 A calculations is done to balance the calcium found by 3dtF and that
accounting far the calcium phosphates and oxalates. Excess calcium
is normally left over after the calculation, and this is reported as
"free" CaO. This extra calcium is thought to originate from clarifier
mud carry over.

3.8.2.3 The chemical composition of scale in Southern Africa

Over the past few years a large number of evaporator scale samples
has been analysed in South Africa, mostly through the work of
Walthew (1995;1996). Work has also been done in Australia by
Crees el al. (1992). These results may be summarised as follows.

• Impact of clarification. The process used for juice

Effect of clmi8cat(oa
clarification will have a fundamental influence on the composition of
the scale. Sulphitation, for example, will result in much calcium
sulphate in the scale; defecation on the other hand results in the
presence of calcium phosphates. Silica, and the total calcium content,
however, seem to stay more or less constant.

• Organic species. Sugar, sometimes caramelised, and other

orgnk Speck-
organic species, may be trapped within bulky calcium phosphates, in
earlier effects. Oxalates, usually as calcium oxalate, CaC 2 O,,.2Hr0 or
Ca C204.H20, are formed in later effects. Aconitic acid, a rare scale
component, as calcium-magnesium aconitate, has sometimes caused
major problems, due to difficulties in removing it.

• Inorganic species. The main inorganic species are calcium, rnurp ak rpecirs
magnesium and phosphates. Calcium phosphate species include
Ca3(PO4)2, an amorphous calcium phosphate, and Ca so(OH)2(PO4)6
a crystalline hydroxy apatite. Silica originates from the cane itself,
being attached to the fibre. It is extracted from the cane, during
milling or diffusion, with temperature and more particularly pH,
i ncreasing its extraction. Silica can also be introduced in the raw
house when refinery sweet waters, which have circulated through
diatomaceous earth filter aids, are returned.

Very generally the distribution of scale in an evaporator tail depends

on the position of the vessel, Many factors come into play,
particularly whether hydroxy apatite (Ca,o(OH) 2(PO4)6) is present or
not. There is much variation but general trends in South Africa are
shown below.

_ 29_
3.8-3 Methods to reduce fouling

As mentioned earlier, the impact of fouling on evaporator

performance can be severe. Procedures to reduce, or even eliminate,
fouling have therefore been investigated.

• Removal. Species such as calcium, which cause scale, can Remorat

be removed from the juice. Chemical precipitation, ion exchange,
filtration, etc., during, after, or to replace clarification, are being
considered. Calcium can be removed by the softening process, that
is by replacing it with Na' or K'. Pilot plant work in South Africa
(Thompson, 1994) has shown that nearly all the calcium and
magnesium may be removed from clear juice. The scale formed in the
pilot plant evaporator tubes had the composition shown below.

-30-
Unfortunately the silica content is not reduced by softening or by the
usual defecation process. With softening, silica could become the
major scale species, causing it to be difficult to remove, since SiO.
does not respond well to chemical or mechanical cleaning.

• Antiscalants. A number of products are available Andscalmunds

commercially. They act as crystal habit modifiers, as complexing

agents, or as dispersants. As yet, they have never produced
spectacular results, in South Africa. They have, however, caused
scale to be softer and thus easier to remove mechanically. Crystalline
species in the scale may have been reduced, but no effects on the heat
transfer coefficients has been seen.

Physical methods. These have not been successful generally. Pkysical n,etlsads
The techniques tested have included the use of spiral turbulence
promoters, inserted in the tubes; of ultrasonic devices, and o£
magnetic devices.

Changes in operation, On the short to medium term, these Good operation control
certainly offer the best possibilities to reduce evaporator fouling.
Most importantly, juice flow rate to the evaporator must be at the
required level and must be steady. There must never be fluctuations
which could cause tube dry out; mud carry over must be eliminated;
pH control must be good. These are basic requirements in any
modern cane sugar factory and WIII go a long way in reducing
fouling.

3.8.4 Fouling resistance

The concept of a fouling resistance can be used in more fundamental

studies of fouling.

A fouling resistance, R,, is defined by equation 3.8.4.1

AcHnidon or rculhg r sWance

1
rr -
Tr -R
UV r VU

where Ut and Ufl are the heat transfer coefficients (kW/m=/°C} after
an operating time of t (s) during which fouling occured, and with

-3 1-
clean tubes, respectively. As usual U = ~, where Q is the heat

transferred (kJls), A the heat transfer area (m'), and dT the

temperature difference (OC). Rf is then the fouling resistance in
m2°CIkW.

The concept is used in making broad comparisons between

evaporators. Say we have an evaporator which has been thoroughly Evanoc oat& cakuLiHon orthe
cleaned and we measure the heat transfer coefficient (HTC) as it fouUng factor
starts operating. We obtain an HTC value of 4,1 kW/m il°C. The
same vessel operates for two weeks after which time its HTC is now
3,5 kW/m2/°C. Then, using equation 3.8.4.1

I
II -Rf
3,5 4,1

and Rf is equal to 0,04 m z°CIkW. This quantifies the fouling of that

evaporator under the conditions of operation.

Walthew (1996) gives values of R.. for evaporators in Southern

Africa, as shown below. The type of evaporator, its position in the
tail, the geographical area from which the cane originates, and the
climatic conditions all influence the fouling factor.

values of fouling factors in

Southern af hm

-32-
3.9 Evaporator cleaning

A wide range of options is mentioned in the literature for the cleaning

of evaporators. Practically, only two approaches remain, namely Mechanical and ehemicai optkns
mechanical cleaning, with rotary scrappers, usually under wet
conditions, and chemical cleaning, almost always involving the use of
sodium hydroxide solutions.

Whatever the option, evaporator cleaning has the following

pracescaf requirements of
requirements evaporatar cleaning

• It must be completed within the time available through the

factory scheduled shut down. There is less urgency if vessels can be
taken off line individually. In some cases a factory may have two
extraction lines and two evaporator tails; then one line and one tail
may be off line, without the whole factory being shut down.

• The cleaning process must restore the heat transfer

coefficient to an accepted level.

• Costs must be considered.

3.9.1 Mechanical cleaning

Rotary scrapers, or brushes, on a long, flexible, electrically operated

wet scraping 1 Lrnaldng
drive are used. The cutters are loosely mounted and centrifugal force
provides the pressure on the tube surface. This approach copes with
variations in tube diameter. The use of water assists in softening the
scale and washes it away.

The advantages of this method are that its cost is generally lower than Advantages and dlsadrantages
that of other options; it can utilise unskilled labour, and many vessels
can be cleaned simultaneously, depending on the availability oflabour
and equipment. It is, however, an unpleasant operation in term of
human comfort, and it may not always restore the heat transfer
coefficient to its clean tube level. Tube damage is possible and the
method does not deal well with hard scales. Visual inspection of
whether the tubes are clean or not is difficult and needs long
experience for good judgement. In South Africa mechanical cleaning
is still cheaper than chemical cleaning.

-3 3-
3.9.2 Chemical cleaning

in most cases sodium hydroxide is used; it is sometimes followed by

a second chemical, usually an acid. Recently (Walthew et al., 1997; opaons

Peacock et al., 1999), two approaches have shown promise; the first
involves the use of a wetting agent to improve the efficiency of the
sodium hydroxide solution, thus allowing a reduction in its
concentration; the second has revived the interest in the use of
chelating agents such as ethyienediaminetetraacetic acid (EDTA), and
of equivalent, but cheaper, chemicals.

The following practical details apply to the use of sodium hydroxide The tae or Naox :-
solutions

• Strength. Practical considerations such as handling Cotumtration

difficulties, and the possibility of gelling, limit the concentration of
sodium hydroxide that can be used, to 30 - 40 °Io (mass NaOH to
mass solution).

• Temperature. Observations in South African factories show Temperature

that cleaning improves as temperature rises. Usually a temperature of
at least 90°C is needed-

- Agitation. The sodium hydroxide solution can be used to Agitation

flood the tubes or can be sprayed onto them. If flooding is used, then
boiling is necessary and this provides the agitation. If spraying is
used, which requires a smaller volume of solution, then nozzles are
needed and about 0,5 to 1,0 llminltube must be circulated by
pumping. This corresponds to about 0,5 to 1,5 Ilminlm' heating area.
Generally flooding, with boiling, results in better cleaning.
Time
- Time. A minimum of 3 hours contact time is needed.

The sodium hydroxide attacks the organic species and silica in the
scale. It is however not very efficient with respect to oxalates and
phosphates. Once the scale has been physically disrupted by the
sodium hydroxide, agitation can break it up and causes it to be
removed from the tube.

Sodium hydroxide is not corrosive to metals but its chloride content

needs to be watched because of its effect on stainless steel. It has
been noted that sodium hydroxide can cause metal embrittlement.

-34-
The disposal of spent sodium hydroxide solutions can be a severe Disposal orspent N&OH

problem in the cane industry. This is one of the points which needs
careful consideration before this chemical is chosen for chemical
cleaning. Chemical treatment of the spent NaOH is receiving
attention in South Africa, but no obvious solution is apparent; it
remains a subject of much research. A typical analysis of spent
sodium hydroxide solution shows about 27% NaOH, 4% Na 2C03,
2,4°/o SiO2, 4,5% PO4, 0,3% CaO, and 66% water and others, all
expressed as mass on mass solution.
The we of wetting agents
Recent work in South Africa (Walthew, 1997) shows that the
concentration of sodium hydroxide solutions can be reduced, without
loss of cleaning efficiency, if a wetting agent is added. Results
obtained in a pilot plant evaporator are shown below, where the
concentrations of the sodium hydroxide solutions (mass on mass
solution) is indicated. When a wetting agent was added at the
concentration recommended by the manufacturer, the strength ofthe
sodium hydroxide solution could be reduced to 6% (mass NaOH on
mass solution) but the cleaning efficiency was excellent. These results
need to be confirmed on the industrial scale.

The lmpaet of a wetting agent on

eieanint with NmOH

(pliot Plant aeple)

Acids can be used, being more effective against oxalates and Acids and inhihitors

phosphates. Both sulphuric and hydrochloric acids have been

mentioned in the literature, at concentrations varying from I to 4 9/6,
at 60 to 80°C, for I to 6 hours. Both these acids crust be inhibited.
Inhibition prevents the acid from affecting brass, iron, child steel, etc.
Usually organic compounds are added to the acid, as inhibitors. The
organic molecule must have a polar group which attaches itselfto the
metal surface; the rest of the organic molecule then forms a
monolayer coverage and protects the metal. The polar group does not
bind to the scale, which can then be attacked. Phosphoric acid has
been used in South Africa.
s *harie add
Sulphamic acid, which has the advantage of being available as a dry
powder, has been found to be efficient at attacking scale. It is
however quite expensive; it decomposes at temperatures above 70oC
and cannot therefore be used above that temperature.
EDTA
Chelating (Greek chele : claw) agents, such as EDTA can be used to
remove calcium and magnesium. EDTA has six donor atoms ( 2
nitrogen and 4 oxygen) and this allows it to wrap itself around a Ca"
ion to form a very stable complex. EDTA has been used at
concentrations of 4 to 5% (mass EDTA to mass solution). The
sodium salt of EDTA is also compatible with an alkaline
environment; this makes it suitable as a follow up after the use of
sodium hydroxide solutions. Cost can however be a problem. Sodium
glutamate is being investigated as a possible substitute for EDTA.

The following procedures, among others, have been used in Southern

Africa Procedures used In South Arrin

• For tubular evaporators. 10 to 15% sodium hydroxide, plus

0,2°Io wetting agent. Boiled for 3 hours. concentrations . mass to novas
sotatiun

• For plate evaporators. 10 to 15% sodium hydroxide, plus

0,2% wetting agent. Boiled for 6 hours. Then flush with water and
circulate 6°Io phosphoric acid solution at 80 10 for 2 hours.

The efficiency of the chemical cleaning procedures depends on many

factors, some of which cannot be controlled while others are
unknown. It is necessary to proceed cautiously when this type of
evaporator cleaning is introduced for the first time; the concentration
of the sodium hydroxide solutions, temperatures, agitation and

-36-
contact times should be set at the higher levels. Experience may then
be used to optimise the procedures, both in terms of cost and of
cleaning performance.
3.9.3 Stearnside cleaning

Fouling on the vapour/steam side of the calandria is usually caused by

the action of heat on organic materials such as traces of lubricants in CAUS"

the steam, or entrained sugar and other juice constituents.

In South Africa Lewis et al. (1978) describe a number of methods to

clean the vapour side of calandrias. Two commercially available Cleaning chemic-a h
products were mentioned. Organic acids such as acetic or formic, at
concentrations of 2% (mass 1 mass water) plus 0,5°/0 (mass 1 mass
water) of a non foaming detergent may also be used. Power paraffin
in water has been used. Finally, diluted molasses has been allowed to
ferment in the vapour space, over a long period, such as the off crop.

3.10 Entrainment

The entrainment of organic matter, mostly sucrose, into condensates

i mpacts in two main areas. Firstly, there is a loss of sucrose which
impacts on recovery directly; the entrained sugars will also cause
problems in terms ofeffluent treatment. , °condly, entrainment affects
the quality of the condensate with respect to its use as boiler feed
water. There is therefore a need to prevent entrainment as far as
possible, and to monitor the levels which will occur even with the
best prevention measures.

3.10.1 Entrainment monitoring

The monitoring of organic matter in raw house condensates used for

boiler feed water requires a well designed conductivity system, and Conducttrity and damping systems
a dumping facility, on all condensates lines that supply the boiler feed
water tank. Most of the entrained organic species, including sucrose,
other than salts, have negligible conductivities. Their presence is
inferred through the conductivity of the salts, both organic and
inorganic, which are also entrained with the organic contaminants. Calibration
The ratio of organic matter to inorganic species varies and
conductivity set points need frequent and individual calibrations.

In refineries, where the liquor purities are very high, conductivity

rtef£netics
cannot be used. Total organic carbon analysers are used, but these are
costly and need relatively long analysis times which requires large

-3 S-
condensates storage volumes; dumping can be wasteful_

Monitoring entrainment from a sucrose loss point of view, is usually

based on a programme of sampling and analysis. Two main
approaches may be used. Firstly, samples ofwater are taken at points Basic prneedum for entrabiment
where specific streams meet; ifthe mixed condensates or waters show monitoring

unduly high levels of sugar, the various individual streams are

sampled and analysed, to identify the source of the problem. The
other approach involves the use of quick, non quantitative analytical
methods, which can show only whether sugar is present at a known
minimum level or not. Again, should the result be positive, special
sampling and quantitative analytical procedures are started.

There are two main types of entrainment. The first is a sudden

upsurge of juice, with flashing, due to a sudden increase in vacuum.
Large quantities of sugar may be lost and, if the monitoring system Types of entrnh+ment
is not well run, the loss may be missed. The second process is the
continuous removal of smaller quantities of juice. Although less
dramatic, this type of entrainment can be neglected and can cause low
but continuous contamination of the boiler feed water.

3.10.2 Quantification of entrainment

Hunan in 1979 and Lionnet in 1984 have measured entrainment in

cane sugar factories. Both authors show the importance of vapour
velocities. Some results are shown below.

Vapour velocEHes in entrahiment

sepai%tars
In South Africa, investigations at factories have shown that
entrainment occurs through two main types of processes. Firstly, the Two typn or entralnmeW
prmewft
sucrose loss correlates well with vapour velocity, through
relationships of the form
b
mg sucrose lost per unit time = a.(vapour velocity)

There are however, high, sporadic, losses which do not correlate with
vapour velocity. This is illustrated in the following figure, for a
centrifugal separator in a 2"d effect, Roberts evaporator.

4 6 8 10
VAPOUR VELOCITY ( MIS)

Excluding the outliers, the relationship is

mg sucrose lost 1 s = 19,1 (vapour velocity) ,"'

for 20 pairs ofobservations with a correlation coefficient of 0,84. The

sucrose lost through this entrainment process would be only about
50kg per week.

It can be seen however that, sporadic and high levels of sugar

contaminations were found, as shown by the squares in the figure.

Very similar results were found with an angle iron separator in a 3` J

effect, and with a centrifugal separator in a 4 t` effect.

_4p_
Some concentrations of sugar in South African condensates are
shown below.
Concen#rwdons of sugar in
condensatn
5uir~~satfk7~r}1

1 0-25 -
10-30 steady operation
90-300 unsteady operation
200-300 unsteady operation

3,10.3 Some practical points

Blocked separator return lines are often the cause of poor separator
performance. In situ separator washing systems have been described
i n the literature {Taylor, 1987; Lionnet, 1984},

Sight glasses on external lines allow quick, visual assessments of

performance. If no flow is evident, then the separator needs
investigation.

Finally, a steady vacuum is a prerequisite for controlling entrainment.

 BIBLIOGRAPHY

Austemeyer KE, Morgenroth B and Mauch W (1995). Plate evaporators in the sugar industry. Proc
Int Soc Sug Cane Technol, 22' Conf 91-102_

Bhagat JJ (1995). Falling film evaporators in the cane sugar industry. An Indian experience. Proc Int
Sac Sug Cane Technol, 22" d Conf. 82-90-

Blake JD (1976). An investigation of condensate and their contribution to effluent disposal from
sugar mills. Int Sug J 78: 131-137.

Byrne HJ (1977). Effect cleaning using sodium hydroxide. Proc Queens Soc Sug Cane Technol
Assoc 44: 239-242.

Chom TA and Hugo A (1984). Hydrochloric acid/resorcinol versus phenollsulphuric acid for
monitoring trace sugars. Proc S Afr Sug Technol Assoc 58: 64-67.

Cox MGS, Mohabir K and Hoekstra RG (1993). The volatilisation and condensation of acetic
acid during cane juice evaporation. Proc S Afr Sug Technol Assoc 67. 148-154.

Crees OL, Cuff C, Doherty WOS and Senogles E (1992). Examination of evaporator scales from
the far northern regions of the sugar industry. Proc Aust Soc Sug Cane Technol Assoc , 238-245.

De Beer TH and Moult JM (1998). Experiences with plate evaporators at Ubombo Ranches in
Swaziland. Proc S Afr Sug Technol Assoc 72: 228-232.

FitzGerald JR, Seillier DH and Sithole J (1991). Preliminary experiences with a falling film
evaporator pilot plant. Proc S Afr Sug Technol Assoc 65: 145-149.

Getaz MA (1985)- Plant trials on chemical cleaning of evaporator heating surface at Umfolozi
mill. Proc S Afr Sug Technol Assoc 59: 96-98.

Humm DM (1979). Entrainment separators for vacuum pans and evaporators. Sug Ind Tech, 39'h
meeting: 190-215.

Ivin PC and McGrath GJ (1990). Acid cleaning of evaporator scale. Proc Aust Sac Sug Cane
Technol Assoc: 45-56.

Ivin PC (1982). Condensate quality and sugar mill boiler operations_ Proc Aust Soc Sug Cane
Technol Assoc: 57-62.

Win PC (1978). Chemical cleaning of evaporators. Proc Queens Soc Sug Cane Technol Assoc 45:
321-326.
James DR, Matthesius GA and Waldron PF (1978). Heat transfer, mass transfer and scaling
characteristics in a long tube, climbing film, pilot evaporator. Proc S Afr Sug Technol Assoc 52:
64-68.

Lewis JWV, Archibald R and Mack C (1978). Steamside cleaning of evaporator tubes. Proc S Afr
Sug Technol Assoc 52: 33-35.

Lionnet GRE (1984). Entrainment from pans and from intermediate evaporator vessels. Proc S
Afr Sug Technol Assoc 58: 90-92.

Nilsson 1(1994). Industrial plate evaporators. Proc S Afr Sug Technol Assoc 68: 125-127.

Peacock SD, Walthew DC, de Beer TH and Neel P (1999). The use of sequestering agents for
chemical cleaning at Ubombo Sugar. Proc S Afr Sug Technol Assoc 73: in press.

Peacock SD and Starxak M (1997). A simplified model of a climbing film evaporator and its
practical application. Proc S Afr Sug Technol Assoc 71: 217-225.

Purchase BS, Day-Lewis CMl and Schaffler KJ (1987). A comparative study of sucrose
degradation in different evaporators. Proc S Afr Sug Technol Assoc 61: 8-13.

Reid MJ and Rein PW (1983). Steam balances for the new Felixton 2 mill. Proc S Afr Sug
Technol Assoc 57: 85-91,

Rein PW and Love DJ (1995). Experiences with long tube climbing film evaporators. Proc Int
Soc Sug Cane Technol, 22' Conf 251-259.

Rousseau E, Sifunda L and FitzGerald JR (1995). Practical experiences operating a first effect
falling film evaporator unit at Pongola. Proc S Afr Sug Technol Assoc 69: 127-131.

Schafer KJ, Day-Lewis CMJ and Montocchio G (1988). An investigation into the causes of
vapour pipe corrosion at FX mill. Proc S Afr Sug Technol Assoc 62: 9-11.

ScMffler Kl, Muzzell DJ and Schom PM (198 5). An evaluation of sucrose inversion and
monosaccharide degradation across evaporation at the Darnall mill. Proc S Afr Sug Technol
Assoc 59: 73-78.

Schaffler KI (1987). Estimation of pH of sugar cane juices at high temperature. Proc S Afr Sug
Technol Assoc 61: 14-17.

Schafer KJ (1978). Sugar entrainment monitoring. Proc S Afr Sug Technol Assoc 52: 123-124.

Singh li, Riley R and Seilher D (1997). Using pinch technology to optimise evaporator and vapour
bleed configuration at the Malelane mill. Proc S Afr Sug Technol Assoc 71: 207-216.
Smith IA and Taylor LAW (1981). Some data on heat transfer in multiple effect evaporators.
Proc S Afr Sug Technol Assoc 55:51-55.

Taylor K (1987). The washing of demister screens at Illovo. Proc S Afr Sug Technol Assoc 61
62-64.

Thompson MC (1994). Softening of clear juice. Proc S Afr Sug Technol Assoc 68: 115-120.

Tobe P (1995). Falling film evaporators for the sugar industry. Proc Int Sac Sug Cane Technol,
22~d Conf 73-81.

Vukov K (1965). Kinetic aspects of sucrose inversion. Int. Sug 7 67:172-175.

Walford SN and Walthew DC (1996). Preliminary model for oxalate formation in evaporator
scale. Proc S Afr Sug Technol Assoc 70: 231-235.

Walthew DC (1996). Aspects of evaporator scale formation and control in the South African
sugar industry. Proc Sug Proc Res Inst, 1996.

Walthew DC, Khan F and Whitelaw R (1998). Some factors affecting the concentration of silica
in cane juice evaporators. Proc S Afr Sug Technol Assoc 72: 223-227.

Walthew DC, Whitelaw RW and Peacock SD (1995). Preliminary results from a long tube
climbing film pilot evaporator. Proc S Afr Sug Technol Assoc 69: 132-137.

Walthew DC, Morgenroth B, Diringer T, Hattwig N, Przybylak P and Friedrich C (1996). Pilot
plant investigations into a Balcke Diirr falling film plate evaporator at GH sugar factory. Proc S
Afr Sug Technol Assoc 70: 226-232.

Walthew DC and Whitelaw RW (1996). Factors affecting the performance of long tube climbing film
evaporators. Proc S Afr Sug Technol Assoc 70: 221-224.

Walthew DC, Whitelaw R and Mohabir R (1997). Chemical cleaning of evaporators. Proc S Afr Sug
Technol Assoc 71: 199-206.

Walthew DC, Wienese A, Squires R and Friedrich C (1996). Preliminary assessment of a rising film
plate evaporator. Proc S Afr Sug Technol Assoc 70: 225-230.

Walthew DC and Turner LM (1995). Analysis of scale from some South African sugar mills. Proc
S Afr Sug Technol Assoc 69: 138-143.

Watson L3 (1987). Heat transfer mechanisms in evaporators. Proc Aust Soc Sug Cane Technol
Assoc: 221-227.

Webb BL and Koster KC (1991). A review of energy management and improvements at Noodsberg
sugar mill over the past eight years. Proc S Afr Sug Technol Assoc 65: 202-204.

Wong Sak Hoi L and Tse Chi Shum S (1996). Estimation! of sucrose inversion in evaporators. Proc
S Afr Sug Technol Assoc 70: 236-240.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

1 Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation. The fundamentals
b Evaporation. The practice

In preparation:-

Diffusion
Crystallisation
Pan boiling
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
PAN BOILING I
Sugar Technology For Students

PAN BOILING I

Prepared by G R E Lionnet

Study Text 7

Published by G A E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright 0 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISSN 0-620-25000-3

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 1. MTRVDUCTION

Nearly all the sugar available commercially is produced through the

Pan bou"e
crystallisation process. This crystallisation, also called pan boiling in
the sugar industry, involves the removal ofwater by evaporation until
crystals appear and grow. The material does not behave as a liquid hirneculte
anymore and is called a massecuite.

Pan boiling is concerned with two main areas. Firstly it involves the
basic properties of sucrose as far as crystallisation is concerned; thus CYystallissfon properties
solubilities, nucleation, crystal growth and crystal properties will be
relevant. Secondly it includes a large amount oflanowledge particular
Sugar technology
to the sugar industry. This deals with the chemistry of sucrose and of
the impurities found in cane and beet juices, with the equipment
developed over the years to carry out the crystallisation process, and
with the various systems and procedures used to produce crystalline
sugar efficiently. All these aspects will be covered.

The states of matter, particularly the crystalline state, will be briefly Crystallisaden
presented. Properties and definitions concerning solutions and
solubilities are obviously relevant to crystallisation. They will be solutions
discussed in detail. Nucleation, as far as the crystallisation of sucrose
is concerned, will be discussed and the use of "slurry" will be Growth rates
described. The quantification of the growth o£ the sucrose crystal,
which involves the measurement of crystal size and mass, will be
studied.

As far as the sugar technology is concerned, the topics will include a

large section on the equipment used for pan boiling in the factories. Fyudpa.-t

Batch operations were used for many years, but in the early 1980's Batch and contfunons
continuous pans were introduced in the South Af can cane industry
and are now replacing the batch pans on all grades of raw
massecuites. A section will be devoted to the practical aspects of pan
boiling. Boiling systems will then be discussed and typical
E:haustlaa
calculations described. Finally the important concept of exhaustion
will be studied.

The subject is covered in two guides, numbered 7 and 8. As usual a

bibliography has been included and will be found at the end of guide
number 8.
 2. THE CONCEPTS

2.1 Crystals

2.1 _ 1 States of matter

There are three states of matter, gaseous, liquid and solid. They
represent different degrees of atomic or molecular mobilities.
Molecular motion in a gas or Liquid is free and random, the physical
properties of these fluids being the same no matter in which direction
they are measured. They are isotropic.

Solids may be crystalline or amorphous, the crystalline state differing cry"AahV& Amor
pbom

from the amorphous one in its regular arrangement ofthe constituent

molecules, atoms or ions, into some fixed and rigid pattern known as
t.'m"
a lattice.

True amorphous solids, because of the random arrangement of their

constituent molecules, are also isotropic. Most crystals, however, are
Aubotropk
anisotropic, their mechanical, electrical, magnetic and optical
properties can vary according to the direction in which they are
measured. Cubic crystals are an exception to this rule, due to their
highly symmetrical internal arrangement.

True solid crystals comprise a rigid lattice of molecules, atoms or

ions, the locations of which are characteristic of the substance. This
raurfacw =gin
regularity of the internal structure results in the crystal having a
characteristic shape. A unique property of crystals is that the angle
between any two given faces is constant, irrespective of the relative
size of these faces. Interfacial angles for a given substance do not
vary, they are a characteristic of the substance.

2.1.2 Crystal symmetry

Many of the geometric shapes seen in the crystalline state show clear
symmetry, this can be used as a means of crystal classification. A
cube, which is a highly symmetrical body, can be shown to have 23
elements of symmetry. This type of analysis can be applied to regular
solids, such as the tetrahedron and the octahedron, and to semi
regular solids such as the truncated cone.

This symmetry concept has been used to show that there are 32
combinations of the three main elements of symmetry. For
convenience these 32 classes have been grouped in 7 systems:-
Crystal systems
Regular
Tetragonal
Orthorhombic
Monoclinic (to which sucrose belongs)
Triclinic;
Tngonal
and Hexagonal.

2.1.3 isomorph and polymorph

Isomorphism
Two or more substances which crystallise in almost identical forms
are said to be isomorphous (Greek: of equal form). Examples are the
alums and some phosphates.

A substance capable of crystallising into different forms, but each

Poiymorphism
being chemically identical, is said to exhibit polymorphism. Examples
are carbon, crystallising as graphite or diamond; sulphur, the crystal
form depending on the crystallisation temperature.

2.1.4 Crystal habit

Although crystals can be classified according to the 7 systems

Crystal habit
mentioned above, the relative sizes of the faces of one particular
crystal can vary considerably. This variation is called habit. Nearly
all crystals are distorted to some degree. Habit is altered by the speed
of crystallisation, by the presence of impurities, by agitation and by
many other factors.

Sucrose crystals can show severe habit modifications.

 s

Habit modification . (A) Elongated (needle) crystal.

(B) fl-shaped crystal.
(C) Slightly deformed white sugar crystal.
2.1.5 Composite crystals

Many crystals produced industrially may exhibit some form of

aggregation. These aggregates, called conglomerates in the sugar
Conglumenues
indust!y, may spoil the appearance ofthe product, may interfere with
free flow or with drying, and may retain impurities, for example
mother-liquor. They are therefore highly undesirable.

A simple form of aggregate is a twin, often found in beet sugar.

These are two intergrown individual crystals, similar in form, joined Twins
symmetrically about an axis or plane. Twinning occurs frequently
with the monoclinic system, for example with sucrose. Certain
i mpurities in the crystallising medium can cause twinning, even with
vigorous agitation.

The formation of crystal clusters or aggregates called conglomerates

i n sugar, occurs more frequently than twinning. Poor agitation, Conglomerates in white su¢ar

certain impurities, high levels of supersaturation and fast

crystallisation rates favour the formation of conglomerates. In white
sugar where conglomerates can occur, they cause lower bulk
densities, they lower purities and they result in the formation of sugar
dust, because of easy breakage.

The formation of conglomerates is reduced by good pan -circulation,

by using low supersaturations particularly when the crystals are small,
and by avoiding excessive crystallisation rates.
2.2 Solutions and solubilities

2.2.1 Solutions
solution : definition
A solution, which can be gaseous, liquid or solid, is a homogeneous
mixture oftwo or more substances. For solids dissolved in liquids, for Sohent and sohate
example sucrose in water, it is conventional to use the term solvent
for the water and solute for the sucrose.

In crystallisation the ability of a solvent to dissolve a solute, and the

effect of temperature on this property, are two important factors. The
ability to dissolve a solute is called solubility, and the temperature
effect is the temperature coefficient. This coefficient deals with the
amount of solute deposited when a saturated solution is cooled.

2.2.2 Expression of compositions of solutions

Before defining important terms such as solubility, saturation and

supersaturation, it is necessary to deal with the various ways in which Composition of wtntiow
the composition of a solution can be expressed. Unfortunately there
are many ways to do so, and not all of them are correct. The
composition may be expressed as:-

mass solute per unit mass solvent

mass solute per unit mass solution
mass solute per unit volume solvent
mass solute per unit volume solution

with the temperature being specified.

Examples of potentially misleading, and therefore useless,

approaches are -.-

a 10 % aqueous solution of sucrose: is that 10 g of sucrose

i n 100 g of water? or 10 g of sucrose in 100 g of solution? or 10 g
of sucrose in 100 cm 3 of water? and at what temperature?

a concentration of 20 ppm of sucrose: ppm, or parts per

million, can be particularly misleading. It generally means mg per litre
of solution. Without clear units, ppm could mean mg per litre of
solution, mg per litre of solvent, and in the sugar industry where
concentrations are often calculated on brix, mg per kg brix. ppm
should be avoided and the concentration given using all the units.
It is clear from the above that it is meaningless not to specify the units
and the temperature when quoting solubilities.

2.2.3 The solubility of sucrose in water

Sucrose is very soluble in water and its solubility increases with

temperature. The sucrose molecule has eight hydroxyl (OH) groups,
five of which can form hydrogen bonds with water molecules; this
accounts for the high solubility of sucrose in water.

The solubility of sucrose in water must be determined experimentally,

and there is still no absolute certainty as to its exact value. Various sadaany
authors give slightly different values. Following a recommendation by
Peacock (1995), the data of Vavrinecz have been chosen, as shown
in the table below.

The solubility of sucrose in water.

Temperature Mass of sucrose (g) dissolved `

(°C) in 100 gams of solution (brix)
20 66,8
30 68,6
40 70,4
50 72,5
60 74,6
70 76,8
80 79,1
90 81,5

Solubility and saturation concepts are now defined.

Solubility
The correct way of specifying the solubility of sucrose in water is to
give all the units and state the temperature. Thus an acceptable saabey
definition would be to quote the mass o£ sucrose in grains that can be
dissolved in 100 g of solution, at 80 °C.
Saturation
A saturated solution is in thermodynamic equilibrium with the solid
SiUU Afoa
phase, at a specified temperature. In simpler, but less exact, terms it
contains the maximum amount of solute in solution, at that
temperature.

Supersaturation
It is often possible, for example by careful cooling, to prepare Saperaatoration

solutions which contain more solute than represented by the

equilibrium saturation. Such solutions are said to be supersaturated,
at a specified temperature. Again there is a number of ways in which
supersaturation can be expressed; considerable confusion arises ifthe
units are not clearly stated. The temperature must also be given. Two
common expressions are the concentration driving force, Ac, and the
supersaturation ratio, S. they are defined as follows:-

S = clc' s

where c is the concentration in the solution, and c` is the equilibrium

saturation at the given temperature. The units must obviously be
consistent. The following data are used as example. For sucrose at 20
°C, c` = 2040 g/kg of water; let c = 2430 g/kg water. Then

Solution ~® Ac S
glkg water 2450 2040 410 1,20

The state of supersaturation is essential for crystallisation to take

place. Early in 1900, the terms "labile" and "metastable" were
i ntroduced to classify crystallising systems. In the sugar industry the
relationships between the saturation/supersaturation of sucrose in
water and temperature are divided into four zones.

• The stable, undersaturated zone, in which no nucleation or SUeie

crystal growth can take place. Any added crystal will dissolve.

• The metastable, supersaturated zone, in which added Metaxtable

crystals will grow.
 • The intermediate zone, where new crystals will form, if
crystals already exist.

• The labile zone, where new crystals will form spontaneously.

These zones are shown schematically in the following diagram.

LYysalBsafion zones for pore

sucrose salons

500

e
3
em
n
d 340
of
w
w
w
300
U
h

G7

240

45 85
TEMPERATURE (°C)

With impure solutions the width of the bands in this type of diagram
are larger.

The properties of sucrose as far as its solubility in water is concerned, PropertJe of sucrose with
are quite special. It is highly soluble in water and can form highly repect to cry dlon

supersaturated solutions. Yet it is capable of crystallising, that is of

moving out of solution, to deposit itself in a controllable manner on
existing crystals. Furthermore, its solubility in water increases as
temperature rises. This provides yet another method for its
crystallisation: a hot, saturated solution is cooled and crystallisation
takes place. This approach has recently been investigated and tried by
Italian workers, mostly with beet juices. Fructose and glucose are
highly soluble in water but do not posses all the other properties
required for recovery by crystallisation. This is why it is difficult to
produce crystalline fructose or glucose.

2.2.4 Particle size and solubility

The solubility of many solutes, in water, increases as the particle size

of the solute decreases. This effect is evident with sucrose. It has
been estimated that particles of sucrose about 1 gm in size will have
a solubility about 0,4 °/u higher than large crystals; particles 0,1 gm
have a solubility about 4 % higher, while particles 0,01 gm will have
a solubility about 40 % higher. These calculated values need to be
seen with caution but it is a fact that small sucrose particles dissolve
faster.

This property has two effects: -

• the composition of a solution may exceed greatly the normal

equilibrium saturation if the excess solute particles are very small

• dissolution rates are faster with small particles; this can be

useful in specific commercial operations.

2.2.5 Calculation of solubilities

We look at sucrosetwater systems. This simplifies the calculations

FWV SUCMM
since solubility data for pure sucrose in water are available.

Say 150 g of sucrose are added to 100 g of water at 60 °C. The

sucrose will dissolve to give 250 g of solution containing 150 g of
sucrose. The concentration can be expressed as

150 g sucrose
x 140
150 + 100 g of solution

or 64 g of sucrose in 100 g of solution. The brix of the solution will

be 60.
Reference to solubility data for pure sucrose in water shows that at
60 °C, 100 g of water can dissolve 74,6 g of sucrose. The above Ilndensatmmd=
solution will therefore be undersaturated at 60 °C.

Say we now carefully evaporate 20 g of water from a solution

containing 293,7 g of sucrose in 100 g of water, at 60 'C. We then
have 293,7 g of sucrose in 80 g of water. The sucrose concentration
is now 293,7 g in 373,7 g of solution or 78,5 g of sucrose per 100 g
of solution, at 60 °C.

This is higher than the solubility data indicates, namely 74,6 g per 100 sapersatorstlan
g of solution, at 60 IC. Thus, the solution is supersaturated at 60 OC.

The following concentrations may be calculated, for that solution, at

60 'C:-

- 78,6 g sucrose per 100 g of solution

• 367,1 g sucrose per 100 g water

• 3671 g sucrose per kg water (c).

A saturated sucrose solution at 60 °C contains:-

- 74,6 g sucrose per 100 g water

• 293,7 g sucrose per 100 g water

• 2937 g sucrose per kg water (c').

We can now calculate the degree of supersaturation:-

caealanom or sapersatmnnm
Ac = ( c - c) = 3671 - 2937 = 734 g per kg water

S = ( clc') = 367112937 = 1,25

Note that Ac and S are calculated using solubilities in water and not
Use aolnblFttes in water NOT
using solubilities based on the mass of the solution. those based on the solxton

Let us now cool a saturated solution of sucrose in water. At 70 oC

a saturated solution contains 76,8 g of sucrose in 100 g of solution,
This is equivalent to

-10-
(76,8x100)123,2 or 331,0 g of sucrose per 100 g of water.

We cool this solution to 60 °C, where the saturation is 293,7 g of

sucrose per 100 g of water.

Then: -
Csleulaffm or mpenatoratfm
Ac. = 3310 - 2937 = 373 g sucrose per kg water

S = 331012937 = 1,13

using again the definitions for Ac and S as given on page 7.

It is also possible to calculate concentrations based on the volume of Conceaf%tlom to mass per
the solution or solvent. This is often useful in industry where the unit rohUVe
volumes of tanks may be known, while masses are not available.
Thus one needs to convert mass of sucrose per mass of solution for
water) to mass of sucrose per m3 solution (or water).

Say we have a sucrose concentration of 2450 g per kg water at 20

°C. This corresponds to

2450
(2450+ 1000) x 100

or 71,01 g of sucrose per 100 g of solution, that is a brix of 71,01.

Peacock (1995) gives the following correlation to calculate density

(p), using the brix and temperature of the solution: -

B(B + 200) 0,036(T - 20)_) corrdaflon to cakuute anuay

p = 100 1+ 1
54004 160- T

where B is the brix and T the temperature in °C. Then the density is
1356 kg per m3 of solution. Tbus 1 kg of solution, at 20 °C, will have
a volume of (lxl)11356 or 7,375x10 -° m' . But 1 kg of solution
contains 71,01x10 g of sucrose. Thus 1 m3 of solution contains
962847 g of sucrose or 962,8 kg of sucrose. The concentration in
mass of sucrose per volume of solution is thus 962,8 kg/m.
2.3 Nucleation

2.3.1 Basic principles

The condition of supersaturation is not sufficient to cause

crystallisation in a solution. Before crystals can develop there must
be, in the solution, a number of small, solid bodies, embryos, nuclei
or seeds. They will act as centres of crystallisation.

Nucleation may be spontaneous or it may be induced artificially.

Practically, it is usually difficult to decide whether a system has
nucleated by one or the other method.

There is confusion on nucleation nomenclature. A terminology that

may be used is: -

Primary: Nucleation in systems that do not contain

Primary and MCOMdar7
crystalline matter, aucleatlom

• Secondary: Nuclei are generated in the vicinity of crystals

already present in the supersaturated system.

*p,u•W l~cnNDAx
iniocW by ayfb

HOMOCfMUi18 MUS
Spaea- kW-,W by &alga puoda

Homogeneous nucleation is not well understood at all. A number of

theories have been proposed. True homogeneous nucleation is

- 1 2-
probably very rare.

Heterogeneous nucleation can be affected considerably by the

presence of mere traces of impurities. Dust itself may cause
nucleation.

A supersaturated solution nucleates much more readily, for example

at a lower supersaturation, when crystals of the solute are present or
deliberately added. The term secondary nucleation is then used.

2.3.2 The use of "slurry" in the sugar industry

in the sugar industry nucleation in supersaturated sugar liquors is

traditionally induced by the use of slurry. This is a suspension of
small, broken, sugar crystals, in a liquid in which sucrose is not
soluble, such as an alcohol.

There are many procedures for preparing slurry. A conunon one in

South Africa is as follows.

800 g of refined sugar are weighed

21 of methylated spirits are added
The mixture is ball milled using 2500 steel balls of 10 mm Pmparation

diameter in a pot 160 mm diameter and 200 nun long. The pot is
rotated at 75 rpm for 12 hours.
The balls are sieved out and the contents made to 6 1 with
methylated spirits.

Quantities used for nucleation vary, depending on local conditions.

As a guideline one can use about 500 cm 3 for 100 m 3 of 13-
massecuite, but about 5000 cm 3 for the same amount of C-
massecuite.

Grabka (1989) discusses a new type of slurry for the seeding o£

massecuites, claiming the following advantages.

Less flammable materials

90 % of the crystals being 10 to 15 pm
Little to no conglomerates
The use of vegetable oil impedes sedimentation.

His preparation involves the use of icing sugar, with n-butyl or iso-

-1 3-
amyl alcohol. He then grinds the mixture and removes the alcohol.
Vegetable oil is used to fluidise the slurry.

2.4 Crystal growth

As soon as stable nuclei have been formed in a supersaturated

solution, they begin to grow into visible crystals. The growth
mechanism of the sucrose crystal has been well investigated.

Sucrose crystals grow through the transfer of molecules from the Transfer and sarrace fncorporadon
solution to the crystal surface, where they are incorporated into the steps

crystal lattice. Generally the transfer is slower than the incorporation

at low (c50°C) temperatures and is thus rate limiting, while it is the
incorporation which is rate limiting at higher temperatures. At
temperature between 54 and 60 °C each step contributes more or less
equally to the rate constant.

This process may be approximated by the following equations.

md = kr A(ci - c ' ) . .....................(2)]

where (1) and (2) represent transfer or diffusion and incorporation,

respectively.

m is the mass (kg) of sucrose deposited in time t (s)

A is the surface area of the crystal (m)
c is the concentration of sucrose (g sucrose per kg water) in the
solution
c is the equilibrium concentration (g sucrose per kg water) in the
solution
G is the sucrose concentration (g per kg water) in the crystal-solution
interface
kd is the coefficient of mass transfer by diffusion
k7 is the coefficient of mass transfer for incorporation.

_1 4_
A simplified pictorial representation of this model is shown below.

CRYSTAL

ADSOHP11ON LAYER

The two equations are difficult to solve because they involve an

interfacial concentration which is difficult to measure. It is convenient
to eliminate c;, by considering an overall concentration driving force,
which is easily measured. Then

dm
__ g
orema equation

Kg A(c
dr WC

where K$ is an overall crystal growth rate and g is an exponent with

no fundamental significance.

If g is equal to 1 and equation 2 is first order, then c, may - be

eliminated from equations 1 and 2 :-
or

kd k r
8 . kd + kr

If k, » kd, then Kg is approximately equal to kd and the process is Impact of N Md k

diffusion controlled.

If kd » k,,, then K.g is approximately equal to kr and the process is

incorporation controlled.

It should be noted however that both processes will always contribute

to Kg.

In reality growth mechanisms are much more complicated, but the

approach shown above has been used successfully to model the
growth of sucrose crystals in a simple way.

Recently there has been interest in growth rates based on the

measurement of crystal dimensions (Bubnick and Kadlec, 1992; V cad G

Lionnet,1998), Two growth parameters have been proposed, a linear

velocity, V, in m/s and a mass growth rate, G, in kg/ml/s. Both need
some characteristic dimension of the sucrose crystal and require the
use of crystal shape factors.

It is generally accepted that increasing the temperature increases the The rued or temper ate
rate at which the sucrose crystal grows.

Impurities can have a pronounced effect on the growth rate of

crystals and on nucleation. They can
Effect ortmpuritlet
• suppress growth completely

• enhance growth

-lb-
 - have selective effects, for example act only on some faces of
the crystals and thus modify the habit.

Impurities may also change the properties of the solution, for

example viscosity, solubility, etc_

Thus the presence of impurities in the sucrose/water system orighu or the ImpuM"
complicates the situation. Furthermore, the concentrations and types
of the impurities present in the solutions depend on whether they
originate from beet or from cane, on the climate, the location and on
many other factors.

In general the effects of the impurities in beet and in cane have been
studied separately and are very different.

In beet it has been shown that potassium is the most meiassigenic Beet
cation, sodium is a little less so, and the least meiassigenic cation is
calcium. This was determined through laboratory crystallisation tests.
The monosaccharides glucose and fructose are not present in beet
liquors_

Sahadeo (1998) used laboratory exhaustion tests developed in South Cane

Africa (Bruijn, 1977; Bruijn et al., 1972; Rein et al., 1981) to

investigate the effects of selected cations on the exhaustion of cane
molasses. His results indicate the following:-

- the meiassigenic effect in cane follows the trend Effect of cadons

Na' >Mg=' , Ca" >K +

which is different to the result found with beet

- polysaccharides (gums, dextran) reduced the exhaustibility Effect of yobwcch LMes

of the molasses. With gums at a concentration above 15000 mg per
kg of dry solids, it was impossible to exhaust the molasses to the
purity obtained when the gums concentrations were low or normal
(= 10004 mg per kg dry solids). The effect was linear as the
concentration of gurus increased from 15000 to 40404 mg per kg dry
solids

- fructose and glucose are important impurities in cane Effect of monosacclwridrs

liquors. They decrease the solubility of sucrose in water and thus
favour exhaustion.

- 1 7-
It is well established that the presence of impurities reduces the
crystallisation rate in sugar factories. This is illustrated below for the
cane sugar industry.

The efrect of purity on the

crystalhsarion rate
2.5 Measurement of crystal size

2.5.1 Sieving

Traditionally crystal size has been measured by sieving. This has the DWavmtapsorzIeving
disadvantages that

• it gives one dimension only

• it can be done on crystalline sugar only, this may require

complicated sample preparation

• it requires large samples

it is affected by conglomerates.

It is however a well known technique which has been used for many
years. Crystal size distributions by sieving are also well accepted and
well documented sugar quality parameters.

2.5.2 Image analysis techniques

Recently there has been much interest in computerised image

analysis. Laboratory systems are being used in many sugar producing
countries to measure one or more of the crystals dimensions.

In South Africa massecuites or sugar crystals are dispersed in sucrose SovM ArHCm trmge xnAbsb system
saturated glycerol and the mixture spread thinly on a microscope
slide. Locally developed software is then used to select the correct
crystals (air bubbles are eliminated using aspect ratios, and crystals
touching each other are separated by contracting/dilating processes)
and to measure the b-axis and c-axis, on each crystal. Histograms and
various statistics are then produced. A micrometer is used to calibrate
the system_ This approach is used to measure the average size of
crystals in industrial C-massecuites on a regular basis. The technique
has also been used for crystallisation studies.

- 1 9-
2.6 Chemical changes during crystallisation

2.6.1 General

Chemical changes dMio;

The chemical changes that occur during crystallisation are caused by
three main processes: -
Inversion
• inversion, resulting in losses of sucrose
Decompoddon of G and F

• the decomposition of monosaccharides mainly through Conreatrarion of non-sh=am

Maillard type reactions

• concentration effects, mostly on non sugars.

Work in South Africa by Purchase et al. (1984) showed that 20 to 50

% of the undetermined loss of sucrose can take place in the boiling
house. It is generally accepted that some inversion in the boiling
house is inevitable.

Morel du Soil and Schifer (1978) have investigated the fate of

sucrose, glucose and fructose during sugar boiling in South Africa. Low of glucose

There was an increase in fructose, which could be due to sucrose Loss of aanino-nitrogen
hydrolysis, confirming that inversion can take place. The largest
change was found to be the glucose loss which could rise up to 35 %,
between syrup and final molasses. Almost one-third of the amino-
nitrogen in syrup was destroyed.

Maillard type reactions are known to occur in the boiling house. Maluard " rep
Uvonred by:-
Massecuites swell and overflow, temperatures rise and gas bubbles
are clearly visible when massecuite samples are examined under the Mgh temperature

microscope. Newell (1978) investigated the reaction in the High brix

laboratory. He found that they can occur in all factory products from low i
syrup to final molasses. Temperature was found to have the greatest
effect on the rate of gas evolution, followed by high concentrations
of dry solids or prix, and low purities. Some sucrose, some fructose
and large amounts of glucose were destroyed by the reactions.

2.6.3 Concentration effects

Crystallisation requires that concentrations be raised to produce the

level of sucrose supersaturation needed. There must be impurities aeonfate
that reach concentrations high enough for crystallisation. Aconitic

-20-
acid, as calcium-magnesium aconitate, is known to produce small
crystals in low grade massecuites. These are clearly visible under the
microscope and can be mistaken for false grain. They however do not
dissolve when water is added, contrary to false grain. Calcium
sulphate di-hydrate has also been identified.
 3. THE EQUIPMENT

3.1 Vacuum pans

Pan boiling is the process during which sugar crystals are formed and
Vacuum paw
grown. Basically water is evaporated from the massecuite while a
sucrose containing solution is fed to it. A vacuum pan is thus an
evaporative crystalliser, using evaporation in a single effect, designed
to handle highly viscous materials. Both batch and continuous pans
are available.

A batch vacuum pan is similar to a Roberts type evaporator, modifies!

to handle massecuites. The modifications include

• large diameter tubes, diameters of 85 to 128 mm are Tube ten=th and diameter

common. Tube lengths vary from 800 to 10017 mm

Doentalce
• a large diameter downtake to facilitate massecuite
circulation

Condenser and rir pQmp

• each pan has its own condenser and air pump
Cyclic uppratlon
• batch pans operates in cycles.

Pans are operated under vacuum to reduce the boiling point of the
material. This has two main advantages:-
vacuum
* It reduces the destruction of sugars.

• It improves the heat transfer by maintaining an adequate AT

between steam or vapour and the boiling material_

Too high a vacuum will however reduce the temperature to levels Tcmperatores
where the increase in viscosity is such that the massecuite cannot be
handled. Temperatures at strike for batch pans are approximately as
shown below:-

A-massecuite 65 °C
B-massecuite 65 °C
C-massecuite 67°C.

_22_
3.2 Batch pans

The basic features of a batch pan are illustrated below.

Sehemdie diagram of it hatch pan

The various parts of a batch pan will now be discussed.

• CALANDRIA • The tubes, shell and tube plates form part of the
calandria. The central downtake, through which the massecuite Caiandrla
circulates, has a diameter about 33 to 50 % that of the body. There
are many di$'erent types of calandrias, some of which are illustrated
below.

_23_
 Different types of calamdrW

QM?MAL D~A=
CROCAL MW rare

CEN7Ln.DOWkaA=
RATDPMTMKA7!
cuucALiavseaM
n.u'M

ACATM CA ANOM
Al44UARDOWNLAIm

The calandria provides the heating surface. The ratio of heating

surface to volume is a design characteristic. Pans handling high purity Heating surface to Volume ratlos
massecuites need high heating surface to volume ratios, values
around b m~lm3 being common, while low grade massecuites require
values of 4 to 5 m'lm3.

Calandrias are normally fed with vapour 1 (V 1),

-24-
• INCONDENSABLE GAS • Incondensable gases must be removed
from the calandria; if they are allowed to accumulate, heat transfer
will be reduced to the extent that boiling will finally stop.

Pipes situated around the central downtake, both at the top and at the
bottom, are needed to remove the heavy and light gases. The Draw off pines

collecting holes at the bottom of the pipes must be about 100 mm off
the bottom tube plate to avoid flooding by condensates.

CONDENSATE • Condensates should be removed through two

outlets, diametrically opposite to each other. Steam traps or U-legs
are then used.

PAN FEED RING - An even, unrestricted flow of feed material is

needed. A common arrangement consists of a feed ring under the
calandria, where the feed flashes and thus intensifies the natural
circulation. A common value for the liquid velocity in the ring is 1
rills.

When the circulation decreases, for example during brixing up at the

JiZier steam
end of the cycle, steam may be added to promote movement. This is
"jigger" steam. Hot water may be added, now called "movement Movement water

water". These practices obviously consume energy and are often

somewhat abused.

Feed liquors are routed into the pan by a feed manifold which is Fred manifuid
connected, through feed control valves, to different products, for
example hot water, syrup, A- or B-molasses.

CIRCULATION - Good massecuite circulation in the pan is

essential for effective pan boiling. It brings fresh mother liquor into
contact with the crystals and thus assists crystallisation. It is Effect of bolting and of bubbles on
promoted by the bubbles of vapour formed as the massecuite is circulation

heated and boils in the tubes. As the bubbles rise they grow in size;
they entrain and mix the massecuite. Circulation is thus due to the
boiling process; should this stop, circulation will cease.

The central downtake in the calandria can have a diameter equal to Effect ofmawecafe density on
circulation
half that of the pan. The circulation is assisted by the difference in
density between the hot massecuite rising in the tubes and the cooler
massecuite descending in the downtake. The descending massecuite
is cooler because it has lost some of its heat by evaporation at the
surface.

-25-
For a given massecuite, circulation is affected by the design of the
Effect ordesip on circalaution
pan, the shape, number and positions of the tubes and by the design
of the downtake.

A schematic diagram ofthe circulation ofmassecuite is shown below.

M9aseculte clrcnladon

• CUT OVER PIPE • The cut over line is a large diameter pipe (200
to 300 nun) connecting the pans, seed receivers and magma tanks. It
Later-connectlnZ the pan foor
allows the transfer of material between pans, tanks and receivers.
This makes the pan floor more versatile as pans can be used for more
than one duty.

Cut over pipes must be steamed and drained after use; this prevents
massecuite built up, and the mixing of different products which would clews
result in the mixing of different crystal sizes.

Precautions have to be taken against possible explosions due to the

thermal decomposition of massecuites left in cut over lines. Prevftdng explosive mraeeculte
decomposition
Preventive measures include the presence of drain valves in each line,
which must be open when steaming is being done. There must be no
leaks through the steam valves.

• SIGHT GLASSES • These allow the visual inspection of the pan

contents and give an idea of the massecuite volume in the pan.

_26_
• PROOF STICK • This allows the withdrawal of samples, without
breaking the vacuum in the pan. The proof stick should be washed
before taking a sample, to prevent contamination by remains from the
previous sample. Usually these remains contain broken crystals, due sample conten tion
to the grinding effect of moving the proof stick through its sheath.

• DISCHARGE DOOR - This is the opening through which the

massecuite is discharged, or struck, from the pan. It must be sized to
allow the discharging of tight massecuites in a reasonable time; the
discharging process must not limit the final massecuite brix. The door
must fit properly and there must be no air leaks.

- STEAMING OUT • After striking, batch pans must be cleaned to

remove all the crystals left in the pan. If these crystals are not Batch pan ateamin= out
removed, they will grow again in the next massecuite, and this will
produce a number of very large crystals in that massecuite thus
widening the crystal size distribution. This affects the sugar quality.

Steamings should not be disposed of by discharging on the

massecuite in crystallisers. They will obviously dilute the massecuite. rHeposdoistewln=,
Generally A-seamings should be routed to remelt; B-steamings can
go to the remelt or to A-molasses; C-steamings can go to B-
molasses.

Finally the practice of steaming out has the additional advantage that
it makes raising the vacuum in the pan easier; the hot vapour is
condensed easily in the condenser and vacuum rises quickly.

- GRAINING VOLUME - This should be less than 40 % of the strike

volume, to limit the number of cuttings needed to reach the desired
crystal size-

- CONDENSER - Most pans in South Africa are provided with

individual condensers. Both internal and external condensers are
common. A schematic diagram of an internal condenser is shown on
the next page.

- HEATING SURFACE TO STRIKE RATIO - This ratio should fit

the type of massecuite boiled. Some common values are given below.

Refined sugar massecuites 8,2 : 1 mxlm3

A- and B- massecuites 5,9: 1
C - massecuites 4,9: 1

-27-
 WA1ZR O TCISr

Z8
_
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation. The fundamentals
6 Evaporation. The practice
7 Pan boiling I
8 Pan boiling II

In preparation:-

Diffusion
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
PAN BOILING 11
Sugar Technology For Students

PAN BOILING II

Prepared by G R E Liomiet

Study Text 8

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright 0 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-25400-3

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA
3.3 Continuous vacuum pans

Pan boiling has been the last operation in cane sugar factories to be
changed from batch to continuous. The advantages ofcontinuous pan Advantages of continuous pan
boiling
boiling are:-

• better plant utilisation

higher operating efficiencies

• better process control

• more uniform crystallisation conditions

• improved thermal economy.

Continuous pan boiling for low grade massecuites was established in

South Africa by the early 1980's. In 1986 a new design of continuous
pan was introduced for A-massecuite.

Rein (1986) has reviewed the development of continuous pan Continuous pans for ail n ts
technology. This culminated with the introduction ofa new design of
continuous pan at a South African factory, for A-, B- and C-
massecuites. Some of the design parameters are tube lengths of 1,45
in for B- and C-massecuites, but 1,3 m for A-massecuite, and the
incorporation of an entrainment separator and condenser as integral
parts of the pan.

Some specific points concerning continuous pans will now be

discussed.

• SEED • It is still not possible to grain in a continuous pan. The need for seeds
Thus all continuous pans in South Africa need to be supplied with a
seed or footing, representing about 30 °Io of the final massecuite
volume. The following table gives volumes of massecuites and seeds
for a factory processing 30 tons of brix in mixed juice per hour. The
calculations use results relevant to batch pan boiling.
 Example of We and need vaunus

• HEATING SURFACE • Generally the heating surface to

volume ratio is about 10 m2/m3. The evaporation rates of continuous
pans depends on a number of factors, but the following values may
be taken as representative:-

A-massecuite 22 kg/hr/M 2 Evaporation rate In ronttanaw

pans.
S-massecuite 10 kglhr/rn2
ke vapour per hour, per square
C-massecuite 8 kglhrlm2 metre of heather surface

• SUGAR QUALITY • Experiences in South Africa, where

raw sugar must generally be of the very high pol (VHP) quality, has
shown that there is no difficulty to achieve this level of quality under
normal operating conditions.

Much attention has been focussed on crystal size and crystal size Cry " size distribution ccsny bm
continuous pane
distribution. Rein et al. (1985) show that :-

• the crystal size distribution of the massecuite is affected by

the variation of crystal size in the seed

• the crystal size distribution is affected by conditions in the

continuous pan.

-30-
 Assuming a good crystal size distribution in the seed, particularly a
l ow coefficient of variation (CV), then the continuous pan needs to
have a flow system equivalent to 12 or more tanks-in-series, to
produce a good circulation and uniform boiling conditions. Then the
CSD obtained in the massecuite will be as good or better than that
achieved in batch pans.

- ENCRUSTATION - Batch pans are steamed out regularly,

as the vessels are emptied. This is generally sufficient to prevent Effect of massecuite purity on
enc. don
encrustation or scaling up of surfaces. Continuous pans on the other
hand may operate for long periods of time without being emptied. It
has been found industrially that encrustation is a function of
massecuite purity; with C-massecuites (48 to 52 purity in South
Africa) the pans can operate for a full season (25 to 40 weeks)
without having to be stopped and cleaned. In the case of A-
massecuites (85 purity) it is usually necessary to stop, liquidate and
clean the pan approximately every two to four weeks. Two problems
can occur in high grade pans , - Effect, of encrustation :-

- Sugar tends to build up on surfaces in the pan. These Blockages

encrustations break off in pieces and can block tubes or outlets.

-Progressive scaling of heat transfer surfaces takes place.

This reduces heat transfer and the pressure of the steam or vapour Scamil LIP

feeding the calandria must be increased. When the limit of this

adjustment is reached, cleaning is required if production rates are to
be maintained.

Encrustation can take place above the boiling massecuite or below

the massecuite surface. Each is considered in turn.

Encrustations above the boiling massecuite may be reduced or

Above massecdte surface
controlled by the following.

- Sprays of water or of syrup feed. An alternative is not to

lag the top of the continuous pan; some vapour then condenses and Sprays

runs down the surface.

- Raising the massecuite boiling level_ Ifthis is possible, it has rzalsed ode levels
been shown that the action ofthe massecuite at the boiling level tends
to wipe the surface clean.

-3 1-
 Positioning of crossover ports. If crossover ports are Position or crossover port
situated below the massecuite level, they are subject to encrustation.
The area immediately above the boiling massecuite is not usually
susceptible to encrustation; thus positioning crossover ports
i mmediately above the calandfa ensures they are kept clean.

• Good operating control. This tends to eliminate splashing. Cool uperatians

High crystal content and low supersaturation levels in all
compartments will also reduce encrustations. It is thus advantageous
to control massecuite quality in all the compartments. Similarly good
circulation and the absence of dead zones are essential. Finally, the
pan should start up and establish good circulation quickly.

Encrustations below the massecuite surface are far less severe and do Encrustation below the mlc level
not usually cause serious problems. They tend to occur at sharp leas severe
edges, and at discontinuities such as probe tips and edges of
submerged baffles. The scaling up of conductivity probes or of
temperature measuring devices used for the measurement of boiling
point elevation, can be severe, particularly in high grade massecuites.
The probes may need daily cleaning in C-massecuite, but more
frequent (sometimes every four hours) cleaning with A-massecuite.

This type of encrustation is controlled by good massecuite

circulation, good pan design and outside insulation to prevent cooling
of the pan surface.

Encrustation is a function - of the crystal surface area per unit volume

of massecuite, and of the supersaturation of the mother liquor. The
massecuite viscosity also influences it since it impacts on the time
spent by the massecuite running down the surfaces.

The scaling up of heating surfaces can be a serious problem. Often it

Scaling up orheM transfer surfaces
can be the factor determining the period during which a continuous ran be HMI ft
A-pan can be operated before it needs to be stopped. Encrustations
may take three weeks to stop a pan, but the scaling up of the heat
transfer surfaces can do so in two weeks. Experience in South Africa
has shown that scaling up can be sporadic. It could be that it is
associated with cane quality, for example the presence of silica and
ofcalcium. It can certainly cause severe problems over a given period
but then disappear for long times.

-32-
 - CONTROL - The control of continuous pans is generally
simple but many loops needed
less complicated than that ofbatch pans but the continuous pan needs
more control loops per pan, since one control loop per compartment
is necessary.

Calandria pressure can be controlled at a steady value or it can be

Pressure
regulated to maintain a preset evaporation rate.

Simple conductivity is adequate for B- and C-massecuites, but not for eo„dnedvity
A-massecuite or for refinery boilings. Conductivity probes are
suitable in A-massecuite but scale up very rapidly. Radio frequency RF probes
(RF) probes have been developed to measure massecuite properties.
Automatic control of continuous pans on high grade massecuites is
seen as being essential.

Boiling point elevation (BPE) is well suited to continuous pans since

the hydrostatic head is constant. The temperature probes can BPE
however scale up quickly.

Finally, continuous pan control has been well investigated in South

Africa, for example by Love and Chdvers (1986).

- ENTRAINHENT - In batch pans entrainment has been

associated with filling up or cutting over. These operations are not Reduced entrrinment
present in continuous pans, and entrainment is expected to be
reduced. In addition the load to the condenser is steady and smaller
air pumps are needed.

- PAN FLOOR OPERATIONS - Shutting the pan floor down

Shutting dorm
is not complicated with continuous pans. The pans are left: full, but
the massecuite brix and the level may be reduced somewhat.

Pan floor flexibility is however reduced when continuous pans are

used. The duties o£ batch pans can often be changed, as the quantity Flemibluty
and quality of syrup change. This is not the case usually with
continuous pans.

Finally, marginal expansions, say 10 %, can be done with batch pans,

Marginal e:panalan
by adding one or more pans. This is not the case with continuous
pans.

-3 3-
 • STEAM ECONOMY • Steam demand with continuous
pans is steady; the considerable changes needed by batch pans are
eliminated. The low boiling head and attention to good circulation
allow lower grades of vapour to be used. Steamings are also
eliminated, but with high grade massecuites cleaning is required
frequently, which generates large volumes of low brix solutions.

• HEAT TRANSFER COEFFICIENTS • HTC values for

continuous pans are given by Rein (1986) as shown in the following
table.
3.4 Pan feed storage and conditioning

3.4.1 Syrup

Normally all the syrup produced should be utilised by the pan floor. Malt storage: 0,6m°ITCH
There is however a need to store syrup, for example because of the
periodic boil-offs, because of short pan stops, and for any emergency.
Usually the evaporator syrup is stored in a large main tank which
feeds the pan supply system. The capacity o£ the main tank in South
Pan supply tank
Africa is about 0,6 m 31TCH (tons cane per hour). That of the pan
supply tank depends on the local conditions. Large storage volumes
could increase the possibility of sucrose losses.

3.4.2 A and B molasses

Here storage is required to cope with the various operations, such as

Storage and condiflowng
graining, cutting over, discharging, etc, on the pan floor. There is
also the need to condition the molasses. A and B molasses from the
centrifugals are normally pumped to storage tanks, and then to "blow
up tanks" where they are conditioned before being fed to the pans.

Conditioning is necessary for the following reasons:

Molasses quality, circulation and
steady steam
to dissolve small crystals

• to reach a temperature which is steady and higher than that

in the pan, thus promoting circulation by flashing

• to be of a constant brix, which helps maintain steady

evaporation rates, and thus a steady steam demand.

Blow up tanks are stirred and use temperature and conductivity 70 °C and 70 bri:
probes to control steam and hot water additions. The usual final
conditions are 70 °C and 70 brix.

The main storage tank capacities are about 0,5 m 3ITCH for A and B
molasses, with batch pans. With continuous pans 0,4 m3 ITCH of Storage and blow up tank Wdes
capacity for A molasses is adequate, while the corresponding figure
for B molasses is about 0,3 m'ITCH. For blow up tanks a capacity
resulting in 5 to 10 minutes retention time is adequate.

-35-
 3.5 Seed and magma receivers

These are storage vessels for seeds, magma, or massecuites at

intermediate stages. They are interconnected by cut over lines, are
subjected to vacuum, and are stirred.

3.5.1 Seed receivers

Seed receivers :-
Some of the requirements of seed receivers are as follows:-

- Stirring is required (at about 1 rpm) to prevent crystals from

settling and to keep conditions uniform. Stirred

Under vacuum
• They must be able to withstand vacuum.

• They are lagged. steamed out

• Sight glasses are useful.

• Facilities for steaming out are required.

Sizing depends on the local conditions.

3.5.2 Magma receivers

In South Africa 13-magma is stored, and supplied to the A-pans. In

other cases, B- or C- magma may have to be stored. B-magma
storage capacity depends on whether the magma or the syrup is
drawn first into the pan. If B-magma is drawn in bulk before syrup is
added, the volume of magma must cover the upper tube plate. Then
about 40 °Io ofthe strike volume is needed, to which about 5% should
be added for safety.

If syrup is drawn in first, then the required amount of magma should

be fed in rapidly, and it is the rate at which it is transferred, rather
than the storage capacity, which is relevant.

Again the tank must be stirred, at about i rpm. The tank may be open
at the top, and steaming out facilities are needed.

-36-
3 . b Pan stirrers

The importance of massecuite circulation in vacuum pans has been

well established. It impacts on energy, on massecuite exhaustion and Importance of circulation
on sugar quality. As a result pan stirrers have been investigated, and
are often used to promote circulation,

Bachan et al. (1985) in South Africa and Bentley et al. (1988) in

Australia, among others, have evaluated the impact of stirrers in
Effect of pan design
batch, low grade pans. The effect of the stirrer will depend to a large
extent on the circulation characteristics of the pan in which it is
located. Results obtained in South Africa and in Australia can
however be summarised as follows:-
Improvements in -.-

- Boiling times reduced by 10 to 30 %.

Boning times

- Increased evaporation rates and heat transfer coefficients. Evaporation rate and HTC

Pan rapacity
- Generally, increases in pan capacities of 15 to 34 %.

It should be noted however, that if the stirrer is stopped, the blades

can restrict massecuite circulation.

The work done in Australia and in South Africa shows that pitched
blade turbine impellers have been used, at 30 to 55 rpm. The power
needed varied between 50 and 75 kW. The stirrer can be top or
stirrer drive : top or bottom
bottom driven. If top driven, a long shaft is required and it may
interfere with the entrasnment separator. If bottom driven, the shaft
is short but its construction may be difficult and it may interfere with
the discharge door, feed lines, pipes, etc

Stirrers have been used successfully in refinery pans; they have

reduced the formation ofconglomerates. Finally, mechanical agitation
is an optional feature in one make of continuous pan (Journet, 1998).

3.7 Jigger steam

Jigger steam is added to pans to promote massecuite circulation. The Promotes circulation
amounts added to both batch and continuous pans is not negligible,
particularly in pans boiling low grade massecuites.

Recently Vermeulen and Pillay (1999) modified existing, A and B

-3 7-
continuous pans to improve circulation and found that the jigger Efcative In both batch and
steam system needed attention. The piping, the steam distribution and Centbumus Pam

the access to the jigger system were modified. Positive results were
obtained.

The quantity of jigger steam added is not easy to measure. Reid and
Rein (1983) give a figure of 1,5 vapour % cane, using V2, for the
continuous low grade pans at one factory. Earlier work (Jullienne and
Munsamy, 1981) reports on actual measurements of jigger steam on
Quantities msed
continuous pans for C-massecuite. Between 0,9 and 1,4 tons of V1
per hour were needed for the C-massecuite only. This was equivalent
to between 10 and 15 % vapour on C-massecuite, or 0,4 % on cane.
It was stated massecuite circulation was very poor without the jigger
steam addition, the impact of jigger steam on pan circulation was
therefore of importance. As was the case with stirrers pan design has
a large effect.

Apart from the impact on energy, the jigger steam will be condensed
in the condenser. It therefore affects condenser design, performance
and the amount of cooling water needed.

3.8 Steam for pans

The major energy requirement on the pan floor is the steam or vapour
needed for pan calandrias. Smaller quantities are needed for blow-up
Steam or vapour conum ption is
tanks, centrifugals, the remelter, the calorifier and as jigger steam.
Pam

The following values have been given for the conventional 3 bailing
system used in South Africa, with the partial remelt of B and C
sugars, using continuous pans for A-, B- and C-massecuites :-

Pan requirements lb % vapour (V2) on cane

Jigger 1,5
Ancillaries 2

Steam requirements can be estimated from first principles by

calculating the evaporation per ton of cane, in A-, B- and C-
massecuites, using brix balances and massecuite quantities. This
approach shows that, without any remelting of B and C sugar, about
15 % steam on cane will be needed. Remelting all B and C sugar
increases the steam demand to i 8 % on cane.

-3 8-
Steam demand with continuous pans is steady; this improves boiler
and evaporator operations, which in themselves are more energy
efficient. The low boiling heads and good circulation in most Steam economy wtth continuaus
continuous pans allow a lower grade of vapour (for example V2) to Pam

be used. In addition steamings are eliminated, again reducing overall

evaporation loads. On the other hand continuous pans, particularly
those on high grade massecuites, have to be stopped and cleaned at
regular intervals, which generates large amounts of water.

3.9 Condensers

Condensers have been described in study guide number 5 (page 15)

and in study guide number 6 (page 16).

In batch pans the evaporation rate, and thus the vapour to be

condensed, show large variations, depending on the grade of the Lam variations in the amom:t of
vapour to be ciandensed
massecuite and of the particular stage of the boiling. The early stages
in an A-pan will produce a much higher evaporation rate than the
brixing up period.

Evaporation rates for pans are not readily available, particularly for
batch pans. The load to the condenser is also influenced by the Effect of JWer steam

amount of jigger steam, which complicates the issue.

Rein in South Africa gives data for continuous pans. He gives (1986)
the following averages for continuous pans in South Africa:-

A-massecuite 22 kg/m 2/hr

B-massecuite 1 0 kg/m'/hr

C-massecuite 7,5 kgWlhr

Generally the evaporation rate depends on the AT (calandria steam

temperature - massecuite exit temperature). Any jigger steam used
must be added.

Julfenne and Munsamy (1981) give values of 5 to 6 kg/m 2/hr for a

C-massecuite continuous pan, with jiggersteam constituting about 50
of the amount.

-39-
 As far as batch pans are concerned, Bachan (1985) in South Africa
and Bentley (1988) in Australia give the following values, in kglm'lhr
for C-massecuite:-

. S`h .,. Lvaporatfon rates In batch C Pam

I

is„~f;an 14 18 12
D
Pall
ee= 12 20 to 25 3 to 5

Again, jigger steam must be considered. Stirrers will also influence

the evaporation rate.

Generally, in batch pans, large variations are expected and condenser

design needs to cater for that. Conditions are much more steady in
continuous pans.

3.10 Entrainment separators

Again, this topic is covered in guides 5 and b. Experimental work in

South Africa was done in 1984 by Lionnet. Since entrainment is
affected by vapour velocity, it is expected that large variations will be
found in batch pans, because of the variations in evaporation rates.
Again conditions will be more steady in continuous pans.

Practical experience shows that entrainment tends to occur when

l arge changes in operation take place, for example at cut overs, when
the pan stops or starts, or when abrupt changes in vacuum take place.
Prartleaf pahds
In addition the return piping of the entrainment separators is easily
blocked by the massecuite, if it is entrained into the separator.
Frequent and thorough cleaning with hot water or steam is essential.
 4. PRACTICAL PAN BOILING

4.1 Terminology

There are a number ofterms which are particular to the crystallisation

process as used in the cane sugar industry. It is useful to know the
meaning ofthose terms.

-AFFINATION- Basically the attempt at removing the liquor

film which is around the sugar crystal. The sugar is magmaed and
then centrifuged, with or without washing.

-BOILING HOUSE- That part of the factory, from mixed

juice to sugar, in which the process o£ manufacturing takes place-

-CONGLOMERATE- Randomly intergrown cluster of

several crystals.

-CRYSTAL CONTENT- The percentage by mass ofcrystals

in a massecuite, magma, etc.

-FALSE GRAIN- Undesirable, spontaneous formation of

small, new sucrose crystals at any stage in the crystallisation process.

-FINAL MOLASSES- The molasses obtained from the last

massecuite in the boiling house. No further crystals can be removed
economically from it.

-FOOTING- The initial charge consisting of a mixture of

crystals and sugar liquor drawn into a pan for boiling into a
massecuite. Also called "pied de cuite".

-GRAINING- The introduction of slurry into a sugar liquor,

which is ready for nucleation in a pan.

-MAGMA- A mixture of crystals and of a liquid sugar stream,

stirred by mechanical means_

•MASSECUITE• A mixture of sugar crystals and mother-

liquor produced by a vacuum pan. Massecuites are classified
according to decreasing purity: first, second, etc, or A, B, C, etc. The
term is also used in refining.

-4 1-
 -MOLASSES- The mother-liquor separated from the crystals,
in a massecuite, by mechanical means, usually in a centrifugal. It twe=M to s
usually contains added wash water or steam, used in the centrifugal.
It is termed first, second, etc, or A, B or C, according to the
massecuite from which it was obtained. The term is not usually found
in refining, where greens, run-offs, jets or runnings are used.

-NUCLEATION- The generation and development of small

sucrose crystals which will act as nuclei and grow.

•NUTSCH- Or putsch molasses. A sample of mother-liquor

separated from a massecuite without dilution or change of
composition. Done usually by a putsch filter (cyclone in Australia)
which utilises air pressure.

-PAN BOILING- Or sugar boiling. The crystallisation process

in a raw cane sugar factory.

-REMELT* A solution of low grade sugar in either syrup,

clear juice, water or any of the usual sugar liquors.

-SEED- Small sugar crystals serving as nuclei in the

crystallisation process.

-SEEDING- The introduction of slurry into a sugar liquor

which is ready for nucleation, in a pan.

-SLURRY- Small (2 to 10 gm) sugar crystals held in a non-

solvent (usually alcohol) and used as the nucleating medium when
graining in a pan.
4.2 Pan boiling procedures

4.2.1 Nucleation

There are three basic methods to instigate nucleation in a raw cane Fostering the nuclei
sugar factory or in a refinery.

The waiting method. The sugar liquor is concentrated until

The waiting method
the labile zone (page 8) is reached. This concentration is maintained
until the operator considers that the required number of nuclei has
been formed. Feed or water is then added and the boiling proceeds.

• Shock seeding. The sugar liquor is concentrated to the sh«f[seedmt

intermediate zone (page 8). A small amount of sugar dust or of

powdered sugar is added and this induces the formation of many
nuclei. Again the operator starts feeding liquor or water when he
considers that the required number of nuclei has been formed. This
technique is often used in refinery boilings.

True seeding. The sugar liquor is concentrated to the True seeding

metastable zone (page 8), and the required number of seed crystals
or nuclei added, using a predetermined volume of slurry. The system
is maintained in the metastable zone so that the introduced nuclei
grow but no new nuclei are formed. The crystals are not visible
immediately after the introduction of slurry, and can take 5 to 10
minutes to be seen. During this period the pan is kept boiling steadily.
This is generally the preferred method in raw cane sugar factories in
South Africa.

4.2.2 Bringing the grain together

After nucleation the crystals are very small and are widely dispersed
Transition ftom nuclei to crystals
in the liquor. ff the evaporation rate increases too much, local
increases in supersaturation may occur and false gain will appear,
since sucrose molecules may have to diffuse long distances to reach
an existing nucleus. The supersaturation should therefore remain
constant by balancing feed and evaporation rates. The total volume
of the pan contents should stay constant, while the nuclei grow
quickly i nto true crystals. These in turn grow thus reducing the
distance between crystals.

-4 3-
4.2.3 Growing the grain

After the grain has been brought together, the crystal are now grown
by introducing the relevant feed, which contains sucrose in solution,
into the pan. The volume of the massecuite increases to the final
strike volume.

4.2.4 Final concentration or brixing up

As the massecuite reaches the strike volume, a brixing up stage is

usually done. Feeding is stopped and evaporation allowed to proceed
until the desired massecuite brix has been reached. This brixing up

period should not be too long; it is usually preferable to control the

boiling process so as to be as close as possible to the final brix when
the strike volume has been reached.

4.2.5 Striking the pan

When the strike volume has been reached and the massecuite has
been brixed to the desired value, the pan can be discharged or struck.

The steam feed into the pan is closed and the vacuum broken. The
massecuite is discharged by gravity to a strike receiver or crystalliser,
by opening the discharge door.

A batch pan may also cut over to another pan or seed tank.

4.2.6 Continuous pans

The procedures used for continuous pans are different. No nucleation

is done in continuous pans; they must therefore be fed a "seed"
massecuite. This seed is prepared in a batch pan and then pumped
rateably into the continuous pan, where the other steps, as discussed
above, are now carried out. The continuous pan discharges the final
massecuite continuously, using a weir and barometric leg.
4.3 Practical pan boiling

4.3.1 Vacuum

An essential requirement for proper pan boiling is that the vacuum

must remain steady at all times. Vacuum fluctuations cause Importance of zl"ay v.cumn
temperature to change and, since the solubility of sucrose is
temperature dependent, result in changes in the supersaturation of the
mother liquor. If the vacuum fluctuations are large enough, crystal
dissolution or the formation of false grain is inevitable.

Automatic vacuum control is highly desirable. A typical system is

shown schematically below.

srbeaar akgr= of vim

When the vacuum in the pan increases the water supply is reduced
and vice versa.

-45-
4.3.2 Brix of pan feed

The brix of the feed has a marked effect on the steam consumption
of pans. For the same final mass of brix in a massecuite, a feed brix AdvautwZea wW dhadv=W;es of

of 55 will require about twice as much steam or vapour than one of high pan feed brLus

70.

Very high feed brixes do however cause problems.

• With syrup, pan tube fouling may occur.

• Small or broken crystals in the feed may not be dissolved.

• Circulation may be affected as the rate of evaporation is

reduced.

A uniform molasses brix of 70, which allows steady operations, has

been found to be optimal.

4.3.3 False grain

False grain formation is one of the worst problems as far as pan

boiling is concerned. The term "false' is misleading since the crystals Problem caused by fahe pale

are real sucrose crystals which grow normally, This new nucleation
is however unwanted since its size will not be similar to that of the
existing crystals. This will cause centrifuging problems which can
range from the complete inability of the centrifugals to purge the
massecuite, because the wide crystal size distribution prevents
molasses drainage, to high sucrose losses into the molasses, as the
small crystals pass through the centrifugal screen openings.

The following conditions may cause false grain.

• Low crystal content. The crystals surface area is too small Operwdooa fkM sae mum rake
erWn
and the distance that the sucrose molecules has to difuse over is too
long.

• The evaporation rate is too fast. Then the supersaturation

becomes too high for the crystallisation rate of that particular liquor.

• The circulation is poor. Local high supersaturation levels

can exist.

-46-
 • Abrupt changes in temperature. Ingress of cold air, through
leaks, can affect temperatures at specific spots in the pan.

• Turbid feeds. The small particles introduced with the feed

may initiate nucleation.

Practical ways for reraovinz false

False grain must be removed quickly. It becomes harder to dissolve
grain
as its size increases. It is removed by reducing supersaturation to
levels just below saturation, either by feeding water to the pan or by
increasing the temperature through increasing the absolute pressure.
This is not easily done particularly if the false grain has gown or if
the pan is nearly full. In the first case the false grain will not dissolve
quickly, while in the second circulation is poor,

4.3.4 Aconitic acid

Aconitic acid is the most abundant organic acid in cane. Its

concentration can reach levels such that it may crystallise out , as
calcium aconitate, in C-massecuites. These crystals look like false Cold= aconitate is me ncWtes
grain and can be very abundant. They will however not dissolve when
water is added and this can be observed under a microscope.

The presence of aconitate in massecuites and molasses increases the

Problems associated with aconitate
viscosity. It has been found that the presence of aconitate can be
associated with severe fouling of the non-working side of C-
continuous centrifugal screens.

Young cane and/or the presence of immature tops can result in high
levels of aconitic acid. Not much can be done to reduce these
concentrations or remove the aconitate from the juice.

4.4 Pan control

Pan control in the cane sugar industry can be divided into two main
Batch and continuoos
categories. The first covers the work done with batch pans, involving
the use ofelectrical conductivity, boiling point elevation and mobility
measurements. Continuous pans were introduced in the South
African industry in the early 1980's. This development renewed
interest in the investigation of pan boiling control.

-47-
The basic principles behind pan control systems can be summarised
as follows.

4.4.1 Electrical conductivity

The use of electrical conductivity to control pan boiling, in the cane

industry, was proposed by Honig in the 1920's. Sucrose itself does
not conduct electricity but some of the impurities present in cane
liquors, such as the inorganic salts, do.

In cane sugar liquors, conductivity reaches a maximum at about 30

brix. Thereafter viscosity effects reduce the mobility of ions and
conductivity decreases. Increases in supersaturation correspond to
decreases in conductivity. Thus the conductivity between a pair of Conductance decrease w briz
electrodes mounted in the wall of a pan, measured in rnihiamps when mcressft
a constant potential is applied to them, can be used as an indirect
method to measure supersaturation. As the brix of the material
increases the electrical conductance decreases due to the restriction
in the mobility of the ions.

The system must be calibrated locally since it uses an indirect

measurement to estimate the concentration of sucrose. Several trials
boilings are done and a conductivity curve plotted, using the pan- The need for callbratlvn
boiler's experience and actual brix measurements. The conductivity
curve is then used to control the feed or water addition. Recalibration
will be necessary from time to time.

The advantages and disadvantages of conductivity are given in the

table.

Advantages Disadvantages .=

Useful in raw houses. Purities Does not work in refineries;

below 95. ion concentrations too low.

Cost is relatively low. Scale build up and metal

Advantages and dhadranWgn of
corrosion, due to electrolytic condncdrlty
effects.

Requires little maintenance. Needs frequent cleaning and

recalibration.

Simple system. Sensitive to temperature

variations.

-48-
Generally conductivity is adequate for batch and continuous B and C
pans. It is not adequate for A-massecuite and in refineries. In A
Snitabk for B and C massecdtes
massecuites continuous pans conductivity probes are susceptible to
encrustations which occur rapidly, often after a few hours of
operation.

4.4.2 Boiling point elevation

Boiling point elevation (BPE) is proportional to the concentration of

dissolved components and may thus be used as an indirect indtreet measure ofeoneentradon
measurement of sucrose concentration. An accurate measurement of
temperature is required.

BPE relates only to dissolved components and thus is not influenced

by the crystal content.

The actual determination is based on the temperature measurement BPE is given by

of the boiling sugar material and on the measurement or calculation mlc temp - boiling water temp
of the boiling point of water at the same absolute pressure. The
difference gives the BPE.

BPE is more suited to continuous pans since the hydrostatic head is

constant. The temperature probe may however be affected by
encrustations.

The advantages and disadvantages of BPE are as follows.

Advantages Disadvantages Advantages and diudvantaps of

BPE
Applies to all solutions. A constant pressure essential
for good measurement.

Particularly suitable for Changing level in batch pans

refineries. need compensation.

In impure solutions BPE

measures brix and not sucrose
content. Supersaturation is
thus not accurate.

-49-
4,4.3 Radio frequency (RF) probes

A new type of measurement, using radio frequencies, to measure the

electrical properties of massecuites was developed to avoid the
RF probes Zlve taformation on
encrustation problems found with conductivity probes in A- mother liquor and on crystal
massecuites and in refinery massecuites. The RF probe measures the Content

resistance and the capacitance ofthe massecuite at radio frequencies.

Information on concentration in the mother-liquor and on the crystal
content may be extracted from the measurement.

RF probes may not be totally free from encrustations and, in A-

massecuite may have to be removed daily or every second day for RF probes need cleaning
cleaning. This can be done quickly and does not disrupt production.

RF probes have been used now for many years in South Africa, in
continuous A pans.

4.4.4 Stirrer torque

If a stirrer is used in a pan, the power consumption of its motor may

be used for control. The torque on the stirrer increases as the Useful for end point of boiling
concentration of the material in the pan increases. The method is
useful mostly to determine the end point of a boiling.

Its advantages and disadvantages are as follows.

Advantages Disadvantages
Can be used for all Very dependent on crystal
massecuites. content, temperature and
viscosity.

Useful for final brix control. Not very sensitive when

crystal content low, for
example at seeding.

4.4.5 Image analysis

Instruments such as the crystaloscope are being developed to produce

an image ofthe crystal being grown in the pan. The image could then
be used for pan control.

- 5 0-
At present, massecuite samples are taken and images of crystals
obtained in the laboratory. The images are then used as records of
crystal size and quality. A second, more exciting possibility, is the
development of equipment and of software to grab the image and
automatically produce crystal size distributions, mean crystal sizes,
histograms, etc., on line. The technology exists to perform all these
tasks in the laboratory, using a conventional microscope, a television
camera, proprietary software and available knowledge concerning the
properties of sucrose crystals. The main problem is the development
of hardware to sample and prepare the massecuite, so that the
crystals can be measured on line, in the pan.

Should the above techniques be successful, it would be possible to

control pan boiling using signals based on crystal quality and quantity.
This, in conjunction with signals based on mother liquor quality,
would allow control based on direct crystallisation parameters.
 5. BOILING SYSTEMS

Sugar syrups or liquors cannot be exhausted in a single crystallisation Optinud cxhanstlon cannot be done
step. The process of sugar boiling must therefore consist of a series in one crystallIsadon step

of crystallisation steps, which result in progressively decreasing

product purities. The number of steps is controlled by financial
considerations; at some stage the cost of recovering the sucrose as
sugar is higher than the returns obtained by selling this sugar.

A number of boiling systems, in which the number of steps is one of

the variables, has been developed over the years. The selection of a
system depends on a number o£ factors:- Factors affecting the choke ors
boiling scheme

• The purity of the incoming syrup.

• The quality of the sugar to be produced.

• The level of exhaustion which is desired.

• The need for flexibility, if conditions are likely to change.

The cost of production, for example the cost of energy, in

the form of vapour or steam.

5.1 Typical boiling systems

The following boiling systems, which will be discussed individually,

are widely used to produce raw cane sugar:- Some typ" boiling systems

• Two boiling scheme.

• Three boiling scheme.

• VBP (very high pot) scheme.

• Double Einwurf scheme.

5.1.1 The two boiling system

This is a simple scheme which requires less equipment since there is

no B-massecuite. The total quantity ofmassecuite does however stay

-52-
the same when compared with a three boiling system. The A-
massecuite purity is low, and thus A sugar quality can be poor, for nfmav*af&Ees ofthe tfo hoUf
example the sugar can be of high colour. The recirculation of A- "hems
molasses is essential and this is a disadvantage.

A simplified mass balance and the basic operations for a two boiling
system are shown on the following page.

5.1.2 Three boiling system

The classical three boiling system is widespread. Here two sugars, A

and B, are available as final commercial products. The raw sugar TWO su=ara for sale

quality is however limited by the presence of the B sugar.

Since the B sugar forms part of the saleable sugar, its quality is
operation al the B station
i mportant. Thus relatively high B-massecuites purities are required.
The B molasses purity tends to be high which in turn causes C-
massecuite purities to be high. This is a disadvantage of the system.
If crystal breakage is a problem when the B-massecuite is cured in
continuous centrifugals, then batch machines may have to be used,
again to meet commercial sugar quality requirements.

Less energy is required since all the B sugar is removed; there is no

remelting. Pan capacity is also improved.

A mass balance and simple flow diagram are given on the next page.

5.1.3 The VHP system

In the raid sixties South Africa was exporting low poi (98,6) sugar.
A number of problems were identified (Alexander, 1971, 1981; van
Hengel, 1952). High starch contents affected the refining of these
South African sugars. The sugar quality tended to deteriorate on
Qty and bandlinE problems with
storage; colour for example was found to increase, and poi tended to low poi m=ar
decrease. Both these problems were found to occur mostly within the
molasses film around the sugar. On arrival in the importing country
low poi shipments sometimes caused problems at discharging from Caused by molasses time
the ships. These were due to the stickiness of the sugar, which again
was felt to be associated with the molasses film.

A partial remelt system was introduced in South African boiling

-53-
 A RAW SUGAR FACTORY BOELE% HD SE MASS BALANCE
Two - Boiling Svstern

Syrup

T. Brix =-1004 Purity = 87

A - Masseruite
A - Sugar
T. Brix = 822
T.Brix = 1356 Purity =81,5 Purity = 99,2

T. Brix = 235
Purity = 54,3

A - Molasses

T.Brix = 534 Purity = 54,3

C - Masseeuite
C - Sugar
T. Brix =140
Purity = 8819 T.Brix = 318 Purity = 55,4
A RAW SUGAR FACTORY BOILING HOUSE MASS BALANCE
Three - Boiling System

A - Molasses

T.Brix = 358 Purity = 68,8

houses in 1963. The aim was to produce a standard, high pol, large
A crystal, from an A-massecuite of purity as high as possible. All ProdactM of VHP

South African factories would now produce only one type of raw
sugar, of a standard, high quality; it was found that the factories
could produce raw sugar of 99,5 pol consistently, under normal
conditions. The only problem with the production of this very high
pol (VHP) sugar was the formation of sugar dust, both at the
factories and at storage silos. Increasing the safety factor (moisture
% sugar/( Ifl0-pol % sugar)) helped.

A low pol sugar was however still needed for specific export
The am of HTyl
requirements. This was achieved by coating the VHP sugar with a
specially made product called high test molasses or HTM. This is in
fact not a molasses but an inverted liquor, with a high concentration
of glucose and fructose. It has a relatively low colour, a low ash Advantages of coating V HP
content, and a low viscosity. The polarisation is low and relatively
small quantities are needed to reduce the poi of the coated sugar.
The preparation of the low poi export sugar could now be done at
one central point (the Terminal), thus providing constant quality.
Obviously new equipment was needed at the Terminal, but this was
a small cost against the numerous advantages of the new system.

The coating of VHP with HTM was found to have the following
advantages:- Advantages of asin.p HTllf

-Affination in refineries is easier because of the low viscosity

of the HTM.

- The ratio of crystal to total sugar is high.

• The HTM film around the crystal contains a high

concentration of glucose and fructose. The (F+G)lash ratio to be
expected in refinery molasses will thus be high, which is favourable
to exhaustion. The colour will also be low.

It was found that, when the raw sugar poi is about 99,4, affination
station in refineries are not required. This was certainly the case in Advantages of 'VHP for retfning

local refineries, and the load on recovery houses was considerably

lowered.

Finally general specifications for VHP are given below:-

-54-
 Specificatiom for NW

Fol Minimum 99,3 %

Sulphated ash Maximum 0,20 %
Colour at 420 nm Maximum 1200

Starch Maximum 150 mgfkg sugar

Fines Maximum 20 %

The mass balance and flow diagram for the VHF boiling system is
given on the next page.

5.1.4 Double Einwurf system.

This is similar to the three boiling, partial remelt system, except that
all the C sugar is used as seed for the B-massecuite, while all the B
sugar becomes seed for the A-massecuite. Details are given by
Rodriguez (1980).

5,1.5 Very low colour sugar, VLC

This was introduced in Hawaii, in 1988. It has been described by
Hare] (1988).

5.1.6 Boiling systems in refineries

asa"rs saw sum
The concept of boiling schemes is also relevant to refining. A typical
example of a simple three boiling system for a back end refinery has
been included for completeness.

-5 5-
 syrup

T. Brlx- 100 Purity - 85

-7-
7. Brioc=
A-Pan Feed

110 Purity = 85

A-Pans

R&ndt ± A-pasSeailta

T. Bt= 10 Purity = 84 T. Brix= 121 Purity II 85

I
A-Con T. Brix= n Pd 4w : 94.54
- Pu a 94.63 I

B-Magna A-Molassm

T. Brix= 11 Purity = 90 T. Brix= 44 Purity = fit

8-Pans

C-FOOtinp

T. Brix= 14 Purity

C-5uyar

T. Brix= 6 Purity = 81 44
 A BACK-END REFINERY - PAN FLOOR MASS BALANCE
Three boilina scheme

Filtered Liquor

T. Brix _ 100
Colour = 302

T
Fine Liquor to Pans

T. Brix = 100 Colour = 318

1st Massecuite

' T. Brix = 100 Colour = 333

Fist Run-off
1st Sugar i.
T. Brix = 48 Centrifugals-
. Colour . = 676 T. Brix = 52
_ _ _ .... _ ._._ ~ Colour = 18
2nd Masseculte

T. Brix 48 Colour = 709

2nd Run-Off

T. Brix _ 24 2nd Sugar

Colour = 1361 ; I icenmfugals; -
T. Brix = 24
Calour _ = 32,
3rd Masseculte
1

0-1
T. Brix = Colour = 1430
24

3rd Run-off

T. Brix = 13
Colour = 2706

To Raw-House -* Refined Sugar

i
T. Brix = 87 Colour = 25J
5.2 Calculations for boiling house material balances

Although computer programmes are generally readily available to

calculate material balances for the boiling house, it is instructive to
use first principles.

5.2.1 Masses and volumes

In the boiling house one wants to produce massecuites by blending

streams. It is thus necessary to calculate volumes and masses as
required.

Say we want to produce 42 m 3 of seed at 72 purity and 95 brix. We

want to use syrup and A molasses, both of which are at 70 brix, but Conrvermon mMalrohme

syrup has a purity of 86, while the molasses has a purity of 63.
Densities are calculated using Peacock's (1995) correlation, with a
brix of 70 and a temperature of 70 °C :-

~ B(B + 200) _ 0,o36(T - 20) Correlation for density

density = 100 1+ 1 160-
54000

where density is in kg/m, B is the brix, and T the temperature in °C.

Then the density of seed at 95 brix and 70 °C is found to be 1487
kglrrr3, while that of syrup and of A molasses at 70 brix and 70 °C is
1323 kg/0.

Let the volume of syrup be 5 m 3 and that of molasses M m 3. Then by

brix and poi balances:-

mass brix in seed mass brix in syrup + mass brix in A molasses Brix and poi balances

mass poi in seed = mass poi in syrup + mass poi in A molasses

and mass is given by the product density x volume.

The brix balance is

70 70
(1487 x 42) x 95 = (1323 x S) x 100 + (1323 x M) x
100 100

-56-
or

5933130 = 92610 S + 92610 M .......... ............. ..-.(1}

The pol balance is

6
(1487 x 42) x ~4 = 0 323 x 5} x ~~ + (1323 x M) x 144

or

4271854 = 79644,5 S + 58344 M .......................(2)

Equations 1 and 2 can be solved and it is found that S = 25 m 3, while

M is 39 m3. This mixture will yield the seed, after evaporation to 95
brix.

5.2.2 Cobenze's diagram

Cobenze's method
When the mixture involves two streams whose densities and brixes
only if biix valaft are close
are similar, the mass balance can be simplified. Cobenze's diagram
may there be used, as shown below.

syrup - Relative syrup volume = 72-63 = 9

86
m/C purity
_ 72

Molasses Relative mol volume = 86-72 = 14

63

The mass balance of 5.2.1 simplifies easily to give a total volume of

syrup plus molasses of 64 m3. Then one can calculate the individual
volumes.

The above approach only works when the brix values of the two
streams to be mixed are the same.

-5 7-
5.2.3 The SJM formula

This important formula has been described in detail in study guide 4, See study ode munber 4
on page 24. It is based on material balances and requires no
assumptions. It is thus fundamentally correct.

This formula is central to the calculation of material balances on the

pan floor. It allows the distribution of sucrose or pol between three
streams.

The SJM formula is given below:-

i OOS(j - M) SAX formula

AS - M)

where R is the recovery of pol or sucrose, expressed as a percentage;

S is the purity of the purest material; J is the purity of the middle
purity material, and M is the purity of the least pure material.

An example will make the use ofthe SJM formula clear. Say we have
Example of the use of the 5dii
a syrup at 86 purity and containing 850 tons of pol. This syrup will formula
feed a boiling house, which produces sugar at 99,5 purity and
molasses at 35 purity. How much of the pol in the syrup will be found
in the sugar, and how much will be lost in the molasses?

The SJM recovery of pol is given by

100 x 99,5 x (86- 35)

86 x (99,5 - 35)
or
507454
= 91,5 Thus 91,5 % of the pol will be
5547 recovered to the sugar

Thus 91,5 x 8501100 or 777,6 tons of pol will be found in the sugar,
while 72,4 tons will be lost to molasses.

It is important to realise that the SJM formula allocates all the pol or
sucrose only to the streams under consideration. Undetermined loss

-58-
for example is not considered.

5.2.4 Computer programmes

Most boiling house material balances are produced by using either

proprietary or in house computer programmes. A typical example of
the results obtained with such a programme is shown on the next
page.

G. EXHAUSTION

It is generally not possible to assess one's performance if some

realistic standard against which comparison can be made, is not
standards for e:haustion
available. The formulation of such standards, for molasses
exhaustion, has received considerable attention over the years, with
work done in Australia, Hawaii, India, Mauritius, Puerto Rico and
Taiwan.

Most investigators have attempted to correlate the final equilibrium

purity of molasses with its composition. This concept was introduced opt effects
in South Africa in 1949 by Douwes-Dekker. In common with most F and G versus ash
workers, Douwes-Dekker shows the opposing influences which the
monosaccharides, fructose and glucose, and the ash, have on the
solubility of sucrose in molasses. Fructose and glucose reduce the
solubility of sucrose while ash increases it,

The exhaustion formula proposed by Douwee-Dekker was improved

by the SMRI in 1977. During 1978 and 1979 a systematic study of
molasses exhaustion was undertaken, using the accurate gas-liquid
chromatographic analytical method forglucose, fructoseand sucrose. The South AM= Target Purity
The molasses was boiled down and equilibrated for 48 hours at 40 Formula
°C, at a viscosity greater than 400 Pa.s. The results, obtained from
133 samples (Rein and Smith, 1981), yielded the target purity
formula shown below.-

F+G
Target purity = 33,9 - 13,4 log , a
( )

-59-
 BOILING HOUSE MASS BALANCE
CIIree t3oillng Partial Remeh Scheme)

Product Masses and Volumes

ons 292.4
r. Bra 37.0
T. Pal 31.2
T.N.Pel 5.8Icaaatr
Clew Juice % on cane

la

A-Pans

Bcmclt
ons 7.7 Cub, m. 5.8 A-Massecuite
T. Brit 5.3 Brit 69.97 Tons 57,4 Cub. m. 38.9 Crystal Conicat 49.2
T. Pot 4.5 Pmiry 85.38 T. Brit 53.1 Brix 92.58 Farhaustion 62.2
T.N.Pd 0.8 Colas 37202 T. Pot 45.5 Purity 85.5
T.N.Pol 7.7 Colour 25622
Cub. mares! ton lox in M.J. 1.05

A-S
A-cen - TOM 28.7 Pot 99.30
to T. Brix 28.6 Moist 0.30
T. Pot 29.5 99.6
B- A•MoLuses T.N.PoI 0.1 COlatlr 1025
11.6 Cub. m. 7.9 TOM 30.6 Cut+_ m. 7,2.0
IT-
T. Brix 1 0.8 Brix 92.97 T. Brix 24.5 Brie 80.02 B1-IR 91.13
T. Pol 9.7 Purity 89.9 T. Pot 16.9 Purity 69.1
T.KPot 1.1 Colour 20517 T.NYoI 7.6 Colour 54368
B-tl n,6 on A-Mm=, 20.3

r B•h'fadsecuite
Tons 22."C ub. m. 15
T. Brit 20.9 Brit 94.66 Crystal Con1rnt 41.4
T. Pal 14.5 Purity 69.1 Exhaustion 63.3
TXPol 6.5 CAM 62524
to Orb. metres 1 ton lox in M.J. 0.40

B•S
TM 11.5 Moist 2.00 44 B~cn '
T. Brix 11.2 Purity 89.9
. Pot 10.1 Colour 20517
T.NToI 1.1 B-Mohasco C-Foo '
fans 11.7 Cub, m 8.3 Tom 4.4 Cub. m 3
T. Brie 9.7 Brre 83.07 T. Bra[ 3.6 Brit 10.02
T. Pol 4.4 Purity 45.1 ~T. Pot 2.5 Purity 69.13
T.N.PoI 5.3 Colour 111194 ~TXPot 1.1 Colaua 54368

C-Pans 14

C-Massecuite
Tons 13.5 Cub. m. 9 Crystal Content 28.1
T. Brie 13.3 Brix 98.00 r Exhaustim 55.69
T. Pot 6,91 Purity 51.6
T.N.Pol 6.4 Colour 124723 _ _Final Mohasco
C-5 Cub, metres l ton lox in ht.J. 0.23 Tons 9:5 Cub. m 7
Tons 5.1 'foist 4. io T. Brix 8.4 Brit 87.99
_ T. Brix 4.9 85.0 T. Pot 2.7 Purity 32.0
1 T. Pot 4.2 Ciina 38614 TXPoI 5.7 Colour 174947
T.NYGI 0.7 ---- C-Ccnuifus Tons 95° Brit % cane 3.94
This valuable formula has since been used extensively in Southern
Africa. It has been shown, by experimentation, to apply to molasses unf"e-a natwe orthe target raft
formula
from many Southern African cane producing regions, to molasses
from Reunion, Mauritius and from the United States.

In 1995, Smith used the original experimental data (Rein and Smith,
1981) to derive a new equation which fits the results better,
particularly at low (F+G)/A ratios, namely

-0,74( F+AG

Target purity = 43,1 - 1 7 l-e

In 1999 Sahadeo and Lionnet measured the difference between the

actual true purity (sucrose by chromatography/dry solids) of the
molasses and the target purity as calculated by the above formula,
called the target purity difference or TPD, for molasses from 15 cane TPD

producing countries. The TPD values ranged from +3 to +7, for 36

samples. This range is commonly found in South Africa. These results
therefore confirm the validity of the concept, and show that it is a
useful and universal measure of molasses exhaustion.

Sahadeo (1998) used an approach similar to that used by Rein and

Smith (1981) to investigate the effects of selected impurities on
molasses exhaustion. The results show that the relative melassigenic
effect of the cations studied is:-
]Effects of Impnritfes on exhaustion
Na' > Cap', Mgx+ > K-

This is contrary to the findings in the beet industry, and will need
confirmation. Fructose and glucose favoured exhaustion, as would be
expected, while dextran and gums had an adverse effect.
 BIBLIOGRAPHY

Alexander JB (1971). The evolution of anew look South African raw sugar. Proc Int Soc Sug Cane
Technol, 14' Con: 1619-1625.

Alexander JB (1981). VHP yaws- Some pertinent facts for producers and refiners. Sug Ind Technol,
vol 40: 134-143.

Bachan L and Webb BL (1985). Assessment of a stirrer installed in a low grade pan at Noodsberg.
Proc S Afr Sug Technol Assoc 59: 39-42.

Bentley GA, Miller KF and Palmer BC (1988). Pan stirrer evaluation at Condong mill. Proc Aust Soc
Sug Cane Technol Assoc: 193-202.

Bruijn J (1977). Exhaustion of molasses. Equipment to determine target purity. Proc S Afr Sug
Technol Assoc 51: 123-124.

Bruijn J, FitzGerald JR, Koenig S and Macgillivray AW (1972). Exhaustion of South African final
molasses. Proc S Afr Sug Technol Assoc 46: 103-109.

Bubaick Z and Kadlec P (1992). Sucrose crystal shape factors. Zuckerind. 117, 5: 345-350.

de Robillard JPM and van Hengel A (1984). Preliminary results ofa modified boiling system at lllovo
factory. Proc S Afr Sug Technol Assoc 58: 47-50.

Grabka J (1989). A new slurry for the seeding of massecuites. Zuckrerindustry, 114: 467-468.

Harel JP (1988). Very low colour sugar. A discussion of the process and its effects on boiling house
operation. Hawaiian Sug Technol 1988, 47: F6-F12.

Hoekstra RG (1986). Simulation of effect of different values of operating variables in a continuous

pan. Proc S Afr Sug Technol Assoc 60: 84-93,

Journet G (1998). The CCTW continuous vacuum pan. Preliminary operational results. Int Sug .1100:
386-394,

Jullienne LMSA and Munsamy S (1981). Assessment of the Gledhow and Tongaat Fives-Call
Babcock continuous pans. Proc S Afr Sug Technol Assoc 55: 79-82.

Kruger GPN (1983). Continuous A pan boiling at Maidstone. Proc S Afr Sug Technol Assoc 57: 46-
51.

Lionnet GRE (1984). Entrainment from pans and from intermediate evaporator vessels. Proc S Afr
Sug Technol Assoc 58: 90-92,
Lionnet GRE and Rein PW (1984). Pilot plant studies on the exhaustion of low grade massecuites.
Proc Int Soc Sug Cane Technol, 17` s Conf. 2328-2350.

Love DJ and Chilvers RAH (1986). Tuning of pan feed control. Proc S Afr Sug Technol Assoc
60:103-111.

Montocchio G (1988). Les cuites continues a Felixton. 3`' Congres ARTAS: 198-207.

Morel du Boil PG and Schafller KJ (1978). Application of gas chromatography in a preliminary

investigation into changes in some non-sucrose constituents during sugar boiling. Proc S Aft Sug
Technol Assoc 52: 96-105.

Newell GM (1979). A preliminary investigation into factors affecting gas formation in massecuites
and molasses. Proc S Afr Sug Technol Assoc 53:62-65.

Peacock S (1995). Selected physical properties of sucrose solutions. Int Sug J 97:571-577.

Purchase BS, Blunt RL and Chasteau de Balyon JC (1984). Investigations of undetermined loss at
Pongola. Proc S Afr Sug Technol Assoc 58: 78-85.

Ravn6 AB and Lionnet GRE (1982). Exhaustion performance yardsticks in the South African
industry. Proc S Afr Sug Technol Assoc 56: 46-50.

Reid MJ and Rein PW (1983). Steam balance for the new Felixton mill. Proc S Afr Sug Technol
Assoc 57: 85-91.

Rein PW (1986). A review of experiences with continuous pans in Tongaat-Hulett Sugar. Proc S Aft
Sug Technol Assoc 60: 76-83.

Rein PW (1990). Encrustation and scaling in continuous sugar vacuum pans. Proc S Afr Sug Technol
Assoc 64: 204-208.

Rein PW (1992). Recent developments in continuous pan boiling. Proc Int Sac Sug Cane Technol,
21' Conf. 2328-2350.

Rein PW and Smith IA (1981). Molasses exhaustibility studies based on sugars analysis by gas liquid
chromatography. Proc S Afr Sug Technol Assoc 55: 85-91.

Rein PW and Msimanga MP (1999). A review of continuous pan development in the Southern
African sugar industry. Proc Int Soc Sug Cane Technol,23` ° Conf in press.

Rein PW, Cox MGS and Love DJ (1985). Analysis of crystal residence time distribution and size
distribution in continuous boiling vacuum pans. Proc S Afr Sug Technol Assoc 59: 58-67.
Rodriguez BM (1980. The double magma system: A report of its performance and experience with
it at United States Sugar Corporation. Sug 7 198(1:16-21.

Rouiliard EEA (1987). Some ideas on the design of batch and continuous pans. Proc S Afr Sug
Technol Assoc 61: 76-82.

Sahadeo P (1998). The effects of some impurities on molasses exhaustion. Proc S Afr Sug Technol
Assoc 72: 285-289.

Sahadeo P and Lionnet GRE (1999). An analytical survey of final molasses from 15 cane producing
countries. Proc Int Sac Sug Cane Technol,23' Conf in press.

Smith IA (1995). Exhaustibility of molasses with low reducing sugar level. Proc S Afr Sug Technol
Assoc 69: 163-165,

van Hengel A (1983). Modified boiling system for better sugar quality. Proc S Afr Sug Technol
Assoc 57: 38-4(D.

van Hengel A (1962). Better sugar by remelting, S Afr Sug 146:587-595.

Vermulen PM and Pillay V (1999). Preliminary evaluations of modifications to the CCTR, FCB
continuous pan at Eston and Sezela. Proc S Afr Sug Technol Assoc 73: in press.

Webb BL and Koster KC (1991). A review of energy management and improvement at Noodsberg
sugar mill over the past eight years. Proc S Afr Sug Technol Assoc 65: 202-244.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation. The fundamentals
6 Evaporation. The practice
7 Pan boiling I
8 Pan boiling Il

In preparation:-

Diffusion
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
DIFFUSION
Sugar Technology For Students

DIFFUSION

Prepared by G R E Lionnel

Study Text 9

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 2004

Copyright 0 2400 G R E Lionnet

Printed in Durban by
G R E Lionnet

I SSN 4-620-25448-X

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 CANE

PREPARATION
POWER
-------------
`
KNEF'ING ............. pI........ ........... .
L _ _ _ _ _ _ _ _ _ _ _ __

MAfNTENANCE SHREDDING
MUD RECYCLE

DIFFUSION
TYPES
THEORY
OPERATION
ENERGY IUCROBIOLOGY
NEW DESIGNS

DEWATERING

vs. MILLING

PRESS WATER
TREATMENT
 x. INTRODUCTION

The cane sugar literature shows that milling has been used for
extracting juice since the earliest days of the cane industry. In fact,
the standard three roller mill is based on a 1871 patent by Rousselot.

In the mid forties, most ofthe sugar technology textbooks stated that
multiple mills were used exclusively in crushing cane and in
expressing its juice.

Reference to earlier literature, however, shows that experiments on Experimeuta IR Leas

the leaching of cane had been done as early as in 1886. Maxwell in L, text t wb by 1932
1932, devotes a full chapter in his book "Modern Milling of Sugar
Cane" to diffusion. He compares the process for beet, cane and
bagasse, noting that strictly speaking, it should be called fxiviation Lwvlaflon

when applied to cane or bagasse. He states, however, that since it has

long been known as bagasse diffusion or milling-diffusion, it is
proposed to adhere to this appellation. Maxwell notes that the
diffusion of cane "chips" had been tried out in the past, but presented
serious practical problems, particularly in connection with cane EGYPT.-
slicing. There was however a very small Egyptian factory, in 1928,
where cane slicing and diffusion were operational. Bagasse diffusion, Cam difhAontried In Luxe
introduced in Egypt in 1904, had since undergone considerable Bftwse diffis4on starW in L%a
development and in 1925 was operational at the Nag-Hamadi factory o"rAaoaw ,h 1 925
in Egypt. This diffusion system, supplemented by a forced juice
circulation invented by Naudet, is shown in the figure on page 2.

Many years were needed for the technique, as we know it now, to be

applied successfully. In South Africa Douwes-Dekker (1956)
reported on Egyptian applications. It required another 10 years for
the process to be widely considered in the cane industry. Payne
(1966,1968) in Hawaii, Foster (1966) in Australia, Freund (1968) in Derelopnments du d t1w add sa's
Germany, Buchanan (1967), Graham (1968) and Lamusse (1974) in
South Africa, all report on it. There was a symposium on diffusion
during the 13' ISSCT congress, held in Taiwan, in 1968.

Finally it was left to Rein (1971,1972,1980,1992,1995) to provide Tboury

solid theoretical and practical studies on cane diffusion. Lionnet
(1985a) reported on mechanisms for the extraction of some
impurities, and Walsh (1998) described a new cane diffuser design. Cuntlaued interest
Recent papers (Rein 1999; Richards 1999, Walsh 1998; Meadows
1998) show that the subject is far from being exhausted.
 LIP JUICE

I I n
, I I n
I I I

I . MEASURING TANKS.
. r

Q LIMING TANKS.
r l
. I
MILLS

I
I
I .
I I
I I
rl S TRAINER

r Pump. PUMP

rrr TUfCE
STRAINER.

PUMP FOR DRAIN WATER.

AIR MI
IT

COI, PENSATOR

NE,a7 CPS I C LO I FIER

Hi
fJ I f= USE

V PUMP 6 MILLS FOR

SUBSIIDER
PRESSING BAGASSE
v

PUMP.
RECEIVER
STRAINER FOR
..MILL WATER...
 2. CANE PREPARATION FOR CANE DIFFUSION

Although the equipment for cane preparation can be the same for
milling and for diffusion, there are important differences. These will
be highlighted in the next subsections.

2.1 Knifing
Reid (1994) provides a good review of the role of cane knifing with ae.Uw of adang

respect to diffusion.

Diffusion requires that more emphasis be placed on shredding than on

knifing, to achieve good percolation in the diffuser. The role of cane
knives must change. Experience has clearly shown that coarse knifing Comm ad" ma
and fine shredding are essential for proper percolation, and that the nne.nnaahv
converse causes flooding in the diffuser. Cane knives thus become
devices used to ensure even feed to the shredder and to eliminate
conditions leading to chocldng. Thus, cane knives are used as
levellers or prebreakers to facilitate shredding.

If the incoming cane has been well burnt and topped, and thus free of
trash and leaves, or if it is chopper harvested to yield clean billets,
then it has been suggested that a large shredder on its own would
suffice. This is not generally the case in South Africa, where there are
five types of knives -. -
Types ores

e Billeters to facilitate conveying of cane on belts.

* Levellers on main carriers, with a clearance of 500 to 1500

nun, to facilitate feeding to the main knives.

* Primary knives with a clearance of 60 to 600 mm, to

prepare the top layer of the cane; the tip speed is about 55 ms'.

* Main knives with a clearance of 10 to 40 mm, to complete

the knifing. The tip speed is about 80 ms'.

* Feeders mounted above the shredder, to break lumps and

accelerate the cane feed into the shredder.

No factory in South Africa has all five types installed. Some

arrangements found with cane diffusion in South Africa are given
below, based on installed capacities.
 KntHme systems as histrned in two
factories

The major maintenance of knives is the refurbishing of the cutting

edge because of wear. There is a direct relationship between wear
and the sand content of the delivered cane. In South Africa each knife manr4nar"
must be hard faced weekly or fortnightly. Palms need building up
with hard facing once or twice a season (30 to 35 weeks).

South African factories usually have a least one set of knives. Most
knives are arranged to give a Preparation Index (PI, see section 2.3 ) PI
of about 85. In many cases a second set of knives is used as a feeder
to the shredder.

2.2 Shredding
Fifty years ago shredding was not a critical aspect of cane
preparation. The usual practice was to use knifing and then a heavy
crusher, normally with two rollers, such as the Krajewski crusher.
Crushers extract juice while shredders do not. The first real shredders Early sy~-
were the Searby and Gruendler shredders; the hammers in these
shredders weighed 3 to 7 kg, and had a tip speed of 60 to 65 ms'.

Generally shredding has been studied much more extensively than

knifing. In 1968 Payne, in Hawaii, investigated the effect o£ cane
preparation for diffusion. Australian (Clarks et al., 1970) work
followed; tip speed increased to 90 and 110 ms"', and hammer mass Tongaat shredder
to 15 kg. Moor (1973,1974) used research findings and practical
experience from a South African factory to design a new shredder,
called the Tongaat Shredder, This shredder was easier to build,
required less maintenance and had a better performance. Some ofthe
design characteristics of this shredder are as follows.
 OThe rotor has alternating, staggered plates. This reduces
stress in the plates, hammer bars and hammers.

*The hammers provide full width coverage. Some design characteristics of the
ToagoatShredder

Ot has a rigid rotor construction.

*It has simple, rectangular hammers which simplifies

maintenance.

*Anvil bar and grid bars are identical.

A schematic diagram of a typical shredder is given below.

Schematic diagram of a shredder

STAOEXED SLDlF.DDED
PLATES ROTOR CANE

GRID PLATE (adpsta61e)

Some general details about shredders will now be given.

- Power
Installed power ranges from 40 to 60 kW per ton fibre per hour Power
{WrM. Absorbed power ranges from 30 to 50 kW/T'FH. The
rotation speed ranges from 1000 to 1200 rpm, the latter being more
common. Tip speed is more relevant and that varies from 65 to 115
Ins'.

- Hammers
Hammers
The coverage provided by the hammers should extend across the full
width of the shredder to avoid short circuiting by the cane. Hammers
should weigh at least 15 kg each, with most hammers in South Africa
weighing between 16 and 19 kg each. What may be more important
than the mass of each hammer or than the number of hammers in a
shredder, is the total mass of all the hammers in a shredder. This
ranges from about 170(1' to 4 100 (number o£ hammers x mass of one
hammer in kg), averaging about 2800 in South Africa.

The mass of fibre per hour, per unit hammer mass averages 12 ( kg
fibre per hr/kg hammer) in South Africa.

Hammers wear on the leading edge and on the tip. The usual
procedure is to first rotate half the number of hammers to present the
unworn face, and replace the other half on which both faces are worn.
The life of each face is about two weeks in South Africa. The
hammers are built up to the original shape and then about 10 rum of
hard facing is applied.

One South African factory has processed 2,5 million tons of cane
with one set of hammers, but the sand content of the cane has a vital
effect-

- Grid plate Grid plate

Grid plates cover a working are of 90 to 120 °, and have five to seven
grid bars. High speed photography in Australia (Cullen, 1974)
confirmed the effectiveness of this type of equipment; the cane
particles explode on impact.

Recently a new design of shredder has been proposed and tested. Whelestalk shredder
This "whoiestalk shredder" is claimed to produce long fibres and a
minimum of fine particles, as required for diffusion. The system
consists of a leveller (30 rpm, 75[3 mm clearance) with an installed
power of 90 kW; a feed drum, 504 mm above the carrier and
requiring 75 kW; the shredder itself, with 2,5 MW of installed power,
for about 300TCH. In1999 there were three such systems in
operation. Problems arose due to large load fluctuations, because of
the absence of knives, and due to limited rotor bearing life.

Finally, Boshoff (1994) gives notes on shredder drives, comparing

Shredder drives
steam turbines and electric motors. He concludes that the choice
depends on local conditions.

2.3 Power for cane preparation

Cane preparation for division requires about 25% ofthe total power
needs of a factory. Power for knifing and for shredding has been
measured by Renton (1974) in South Africa and by Nicklin (1967) in
Australia. The following table applies to typical South African cane
diffusion systems.

Installed power (kW) in South Africa

Power for cane preparation
TCH Knives Shredder Total kW/TCH
Knives Shredder Total

375 2235 2090 4325 6 6 12

225 1000 2000 3000 4 9 13

300 2120 3000 5120 7 10 17

385 2800 2135 4935 7 6 13

There is a method to determine the number of open cells in prepared

cane. The method is not perfect and depends very much on sampling
and on rigid adherence to the analytical procedures. It has however PI
been useful in providing comparative values for the degree of cane
preparation. The method gives a "preparation index" or PI. In South
Africa the PI of shredded cane is normally at least 90.

Renton (1974) shows that there is a relationship between power

absorbed and PI; he used South African data to derive the following
equation relating PI to power, W, in kW/TFH, as absorbed by the
knives and the shredder -
 PI = 67,3 x W""

Renton stresses that this relationship can only give a crude

approximation of reality.

Crossman (1994) describes a typical South African preparation line.

His data have been used to produce the following figure.

Typical SArrican prep liar

2.4 Cane variety

Cane variety, more particularly as it affects pith to fibre ratio, can
impact on diffuser performance. Recently a new variety in Southern Effect of cane variety
Africa has been found to be unsuitable for diffusion, under existing
conditions of cane preparation, at one factory. This variety caused
percolation problems and flooding. The problems appear not to have
been solved completely; this variety is now blended with others which
perform well with respect to the diffusion process at that factory.
 3. DIFFUSION

In South Africa diffusion was first used in 1964 and all operations
involved bagasse diffusion, that is one mill followed by the diffuser. Diffusion in Southern Arries

The main reasons for starting with bagasse diffusion were to retain
one mill as a safeguard against adopting a completely new process,
a concern about juice quality and recoveries, and to avoid
complications with cane payment which was based on the sampling
and analysis of first expressed juice.

The advantages of cane diffusion were however seen as overriding,

and the first true cane diffuser was installed at Amatikulu, in 1974.
Now, in 1999, about 80% of the Southern African cane tonnage (33
million tons annually) is processed by cane diffusion.

A number of specific subjects pertinent to cane diffusion and to cane Only cane diffusion will be dealt
with to tbis guide
diffusers will now be considered.

3.1 Types of diffusers

Both Lamusse (1979) and Rein (1995) give details of the types of
diffusers that have been used. They can be divided into the following
main categories.

*Horfzontal moving bed. This is the most common type of

diffuser in the Southern African industry, with commercial fines such Horizontal moving bed

as BMA, De Smet and Tongaat-Hulett providing equipment. The

diffusers have long conveyors with the cane moving as a thick mat.

These diffusers can have moving screens (De Smet), or fixed screens Moving sad tined screens
(BMA, Tongaat-Hulett) where chains transport the cane over the
screen, These two approaches are compared below.
 Moving vs. Fixed screens
Moving screens Fixed sc7reem

Needs double the screen area Cane is more compact; this

since half the screen, on the can impact on percolation
return stretch, is inoperative
Screen is fragile, tears can Can use a dewatering drum to
occur; difficult to seal along reduce bagasse moisture
walls

Less friction; power for the Simpler cane discharge

drive can be about 1/3rd that
for an equivalent fixed screen

0 The best known diffuser of this

Vertical annular diffusers.
type is the Saturn, two of which operated in the Southern African
region. None are operational now.

*Inclined bed. The F & S, or van Hengel diffuser was of that

type, and operated at Pongola in South Africa. Cane tumbles from
cell to cell, which is an advantage as it promotes mixing. The design
involved a number of relatively small units or cells, which could be
added on as needed. This type of diffifser suffered from mechanical
problems, and none is operational now.

Moving bed diffusers are counter current extraction devices, Moving bed diffusers. dimeasions

operating on a stagewise basis. Juice is poured on a bed of prepared

cane, about 50 to 65 m long, 4 to 12 m wide, with 10 to 18 stages.

Cane preparation, for high extractions, is even more critical with cane
diffusion, than it is with milling. As much of the sugar bearing cells Cane preparation
as possible must be broken, and long fibres must be present for the
cane bed to be stable and open to allow high percolation rates. Thus
the need for heavy duty shredding but a minimum of knifing.

3.2 Diffusion theory

Some terminology is now needed, as given below.

opercolation rate. The rate, u, at which liquid is applied to

Nomenclature
the surface of a cane bed is called the percolation rate. It is the
volume of liquid, per unit surface area of bed, per unit time. The units
are thus m'miri ' rri z.

_ 1 0_
 OPercolation velocity. The vertical downward velocity, V, of
the liquid as it moves between the cane particles, is called the
percolation velocity. It is expressed as distance per unit time, that is
V has units mmini'.

0 Flooding. Flooding occurs when too much liquid is applied

to the top of the bed surface, more than can actually percolate
downwards between the cane particles.

e Bypassing and recirculation. We now refer to the figure.

Schematic diagram 03 diffuser

stages

Consider tray N. The amount of liquid appearing here depends on the

rate at which the liquid percolates downwards, and on the velocity at
which the bed moves horizontally.

Ifthe bed moves too slowly. Part of the liquid which should
By-passing
go to N finds its way to tray N-1. This is called by-passing; that is
some liquid by-passes tray N and moves forward too quickly.
 If the bed moves too fast: Part of the liquid which should go
to N finds its way to tray N+1. Thus some liquid originating from
Recircalation
tray N+1 returns to tray N+1. This is recirculation. Now the liquid
from N+1 to N can be increased, which promotes high liquid
application rates but flooding may occur.

The degree of by-passing and of recirculation can be Spray advance

controlled by moving the point at which the liquid is applied to the
top of the cane bed, that is by changing the spray advance.

Rein (1971,1972) developed a mathematical model defining the

extraction of brix by a cane diffuser. The model proposes that the neit.'s model

cane diffusion occurs via two first order processes. The first process
is the diffusive transfer of brix from within the unbroken cells to
outside the cells, followed by a connective dispersal of this brix. The
diffusive transfer is much slower than the dispersal_ The second
process is the connective mechanical removal of brix adhering to
broken cane cells.

Rein's model can be represented in a simplistic way by the following

drawing.

Schematic representation of Rein's

diffusion model

DIRUPGO Comtixlw
Srix in cone b Brix an cane
Stow Fus

BRTX FN
-jo- SOLL?lON

Cpl wfim
Initial brim on cline
Fan

This model was found to fit experimental data very well and has been
the basis of the theoretical knowledge of cane diffusion.

Rein (1971,1972), Love and Rein (1980), Rein and Ingham (1992)
Lionnet (1985a,1985b) and others have shown that the degree of
cane preparation, the percolation, pH and temperature all affect the
extraction of brix and of impurities present in cane. The above

- 1 2_
 Tracer tests involving the use of lithium chloride have been used to
obtain approximate values for the residence time of juice in the Juiee retention times
diffuser. It must be assumed that brix and the added Li+ ions have the

same retention time; this is usually not quite the case, but
comparisons between various diffusers can be made. A lithium
chloride solution is poured onto the cane feed of the diffuser and
juice samples taken at known time intervals for analysis. The Li+
concentration versus time graph usually shows a sharp initial rise, a
sharp peak and a small tail. Juice retention times can be calculated
using age distribution functions; values of 15 to 25 minutes would be
expected. Lithium is used as a tracer because it is not naturally
present in cane, and because atomic absorption analytical techniques
are very sensitive and precise for Li.

The retention time of fibre can beestimated by using the chain speed.
Fibre retentios times
In South Africa this is usually 60 to 120 minutes, for bed heights of
1,1 to 1,6 m and chain speeds of 0,7 to 1 mmin `.
publications should be referred to for details.

Percolation is central to diffuser performance. It is the process by Yerco[atioo

which the juice moves through the cane bed. As shown earlier in this
section it is defined as a percolation rate (volume of juice per unit
area of bed per unit time), and as a velocity (distance moved by the
juice in unit time). It has been well established that the quality of the
cane, cane preparation, and liming in the diffuser impact on
percolation. Love and Rein (1980) have investigated percolation both
in pilot plants and on the industrial scale. They have related it
mathematically to the degree of cane preparation and to the bulk fibre
density. Low bulk densities and coarse preparation favour higher
percolation rates. In South Africa percolation rates of 0,1 to 0,2
m'nw2 miti' have been measured. Percolation velocities have been
found to range from 0,15 to 0,3 mmir '.

Perco lation velocity is an important variable since it determines where

the interstage sprays should be located for juice to appear in the
Tracer teats
correct tray. Tracer tests have been a useful technique to study full
scale diffusion. A typical test involves the addition of a sodium
chloride solution, as an impulse, to the juice. The conductivity is then
monitored in the three relevant trays (N-1, N and N+ 1), as shown in
the figure on page 11. Typical tracer tests results are shown below.

Cc Oductirvity traces

The results from the tracer test, the geometry of the diffuser, and the
bed velocity and height are used (Love and Rein, 1980; Rein and
Ingham, 1992) to calculate the percolation velocity, the percent of
recycle (normally about 30 °Io), and the percent of by-passing
(normally about 40%).

- 1 3-
 b
w

a
x
cq

3
w
U

U
H

rS
W
V
M

p
3.3Uiffuser operation

3.3.1 Temperature Temperatorc

Process steam is required to enable the diffuser to operate at
Range and minimum
temperatures between 75 and 90 °C. As will be seen later, there must
be no spot in the diffuser below a temperature of 75 'C. These high
temperatures are required for the following reasons.

*To eliminate microbiological activity and thus sucrose Prevents microbiological activity

losses.

*To increase the rate of extraction by promoting mass

transfer and making unbroken cane cells more permeable to sucrose
Accelerates extraction of all species
molecules. Heat accelerates the rate of extraction of many soluble
species; thus the extraction of sucrose but also that of impurities such
as colour bodies, will be increased. An increase of 10 ° C can cause
colour in the juice to increase by 10 to 25 %.

Temperature is achieved by circulating juice through scalding juice scalding j nice heaters
heaters, and by direct steam injection into the diffuser, as shown in
Direct steam injection
the figure on page 17. Raw juice leaves the diffuser at temperatures
of 60 to 65 °C.

3.3.2 Liming
Since cane juice is acidic, corrosion of mild steel components in the
diffuser is an important consideration. Special materials such as Corrosion
3CR12 are often used for particularly vulnerable areas such as the
sides, roof or screen of the diffuser. Another approach is to protect
the metal by painting or coating.

It is also possible to control corrosion by raising the pH to values

pH
between 5,5 and 6,0. Milk of lithe may be used. High pH values
and/or local overliming must however be avoided, for the following
reasons.

*pH values above 7 cause percolation problems by affecting

the nature of the fibre irreversibly. Percolation velocity is reduced Percolation

considerably.

*Hydrolysis of the acetyl group in the hemicellulose

fraction of the cane fibre can occur. This produces calcium acetate
which in turn produces acetic acid. The acid is volatilised in the Acetic acid

evaporators causing very severe corrosion in calandrias, vapour and

- 1 5-
condensate piping.

*Laboratory work has shown that the extraction of silica

from cane is increased as the pH rises. Silica has been associated with sul~.
scaling problems in evaporators. It is also found in relatively high
concentrations in tops and trash.

0 Laboratory work has also shown that high pH values favour

Calorr
the extraction of colour bodies, particularly from tops and trash.

Good pH control is thus essential, but this is not easy. Automatic

control for the milk of lime addition, at a number of points, is pH coatral
required. Individual pH controllers (say three) are ideal but efficient
operation seems to be difficult and maintenance is high. Usually only
one pH controller is installed; it is often found that the system is not
working well. A solution which has been proposed is to measure pH
at one point only and use this signal to control mills of lime addition
to a header tank; the milk of lime is then fed by gravity to a number
of points in the diffuser. This is shown in the figure on page 17. One
of the problems with this method is that the milk of lime piping is
often blocked by lime solidification.

Recently it has been suggested in South Africa ( Barker and Lionnet,

2000) that saccharate could be used rather than milk of lime.
Unweighed mixed juice would be used to prepare the calcium
saccharate which would not affect the sucrose mass balance used for
cane payment. The advantages of saccharate are that it contains no
grit and that its pH is somewhat lower (11 instead of 14) than that of
milk of lime.
 IIISTRIBh7TON BOX
MILK OR LIME

VAPOUR I

DRARF JUICE

3.3.3 Mixing screws

Solids in the press water from the dewatering mills can plug the cane
Problems caused by solids in press
bed, at the point where the press water is returned to the diffuser. nater
This obviously prevents percolation and causes flooding. Press water
clarification was therefore essential in early diffusion installations; this
operation was never very successful and alternatives were sought. In
Lifting screws replaced press water
1958 van der Reit and Renton, in South Africa, developed an auger clarification
type screw, top driven by individual electric motors and set in line,
about one metre apart, across the width of the diffuser. These lifting
screws, which extend to about 200 nun from the bottom of the
diffuser and are located at the point where press water is returned,
mix the solids into the cane bed and prevent the formation of an
impervious layer of fine fibre. This has been an elegant solution to a
serious problem and nearly all diffusers in Southern Afi-ica have lifting
screws; often two sets of screws are found in one diffuser.

- 1 7-
3.3.4 Juice screening
Generally juice screens are not necessary on diffusion juice. The suspended solids :-

natural separation caused by the cane bed removes much suspended DHluser Jake, unscreened: 0,1%
matter. In South Africa suspended matter in mixed juice is measured MM ,screened Jndee: 0,694
reliably and the results show much lower values in diffuser juice
(0,1 % mass by mass) when compared to screened juice from milling
tandems (0,5°/0).

3.3.5 Flooding
Flooding occurs when more liquid is sprayed onto the top surface of
Problem mama by ass
the cane bed than can percolate downwards through the bed. It
causes serious problems. Extraction drops; it can cause cane to be
washed out from the feed or discharge ends of the diffuser; it
destroys the concentration gradient in the diffuser. High liquid flow
rates through the cane bed are however desirable, as they promote
high mass transfer. The diffuser should therefore be operated at all
ti mes with liquid flow rates at a maximum level, but just below the
level at which flooding occurs.

3.3.5 Basic diffuser operations

0 Starting a diffuser. The procedures will obviously depend

on local conditions. Basically the approach is as follows.
Basle procedure. t o Ma" a dllruser

);-.- Close all drain valves.

;;-Fill diffuser with water to about half full.

Open valves at scalding juice and to mixed juice.

aOpen steam inlet valves; allow temperature ofwater

to rise.

ACirculate water to scalding juice heater. Open steam

(V 1) valve to heater.

Y.-Start screws.

Feed cane.

BAs cane progresses start juice pumps.

- 1 8-
 0 Stopping a diffuser.
Basic procedures to stop a diRWrer

AReduce the imbibition water.

After the last cane has been through the shredder

stop the imbibition water.

aShut V1. Stop the scalding juice pumps.

;;,-Stop the tray pump as the last cane passes the tray.

;.--When empty of cane add imbibition water and pump

to front until brix reaches a value of 2. Depending
on the cane payment system, a decision is taken
to send this juice to drain.

aOpen drain valves.

a Scalding juice heaters. These heaters can be usual plate and

tube heaters. They treat the juice to temperatures between 92 and 95 sealding juice
°C. The aim is to have juice which is sufficiently hot to raise the
temperature ofthe feed cane to 85 °C. Scalding juice quantities range
from 250 to 350 % cane.
One bed mmt be uniform
9 Bed configuration. The bed level across the width of the
diffuser must be uniform. There must be no gaps or empty regions in
the bed. Varying levels of cane or gaps, ifthey persist throughout the
diffuser, will cause empty pockets under the pressing drum; juice will
then flow through onto the bagasse.

* Imbibition water. The imbibition water temperature in

South Africa is about 75 °C. From a diffusion point of view, there is Imbibbiou watec temperature and
gvaaaiy
no maximum or minimum imbibition rate. Local conditions must be
used to establish a balance between the increase in extraction and the
costs of additional evaporator capacity and increased energy demand.
Experience in South Africa has shown that very high levels of
i mbibition, around 400 % on fibre, can be handled in diffi,lsers.

-1 9-
3.3.7 Diffuser control
In a milling tandem, the mill feed is regulated by the speed ofthe first
mill. Cane feeding to a diffuser is controlled by one of the following
Cane reed
methods.

0 By feed control to the shredder.

0 By weighing, for example using a belt weigher, the cane

feed to obtain a constant mass flow by adjusting the speed
of the belt.

0 By measuring the depth of the cane on the belt conveyor.

This information and the belt speed are then used to keep
the product belt speed x cane height constant.

Temperature

Temperature control loops are needed for the scalding juice heaters PH
and for the direct steam injection. pH control is required and, as
Bed level
discussed earlier, two loops would be needed. Many factories use one
only. Some measurement of bed level is required. Finally, stage juice
temperature is an advantage.

In 1992 Rein and Ingham reported on the benefits to be gained by

controlling the liquid flow rate in each stage. This eliminates flooding
and keeps percolation velocities optimised at all tunes. A bubbler
system was used to measure the juice level in the cane bed; a small
quantity of air is purged into the side of the diffuser and the back
pressure measured. This signal is used to regulate the flow rate so as
to maintain the liquid level in the bed at its optimum value.
 4. THE MICROBIOLOGY

Low brix raw juices provide an ideal environment for

microorganisms to be active. Sucrose is broken down, and impurities
produced, by many organisms at normal ambient temperatures. In
milling tandems for example, Leuconostoc and Lactobacillus species
are often present.
Thermophiies
The higher temperatures and somewhat higher pH levels found in
diffusers Limit the growth of the microbial flora to the thermophiles
(thermos: hot, and philos: Loving, in Greek). ALL these Lactic acid
microorganisms use sucrose as nutrient and produce lactic acid as a
metabolic byproduct. There are other thermophiles which can be
active during diffusion; they consume sucrose but do not produce
Lactic acid. It is generally accepted however, that the primary
organisms responsible for sucrose losses in the cane industry are the
Lactic acid bacteria.
1 mass gait of lactic acid =
McMaster and Ravno (1977) show that substantial amounts of lactic 2 mass amts of sucrose

acid can be formed during diffusion. They show that two parts of
sucrose are required to produce one part of Lactic acid, on a mass
basis. It is thus possible to estimate the quantity of sucrose lost by
measuring the amount of Lactic acid formed. Lactic acid in cane juices
is analysed by a gas chromatographic technique. Many factories in
South Africa analyse weekly mixed juice samples for Lactic acid; a
concentration of lactic acid of 300 mg per kg brix is considered
acceptable. Higher levels require special attention; if the incoming
cane itself has high levels of lactic acid then the problem could be
unacceptably Long cane delays. Otherwise factory sanitation needs
attention.
Temperature:-
Temperature remains the most practical way ofcontrolling microbial
Average 85 'C
activity in a diffuser. Below 70 ° C sucrose Losses can be high; it is a
good practice to operate a diffuser at an average temperature of 85 Nowhere below 75 'C
'C, making sure that there is no spot in the diffuser where it is below
75 ° C. Practically, sufficient juice heater capacity must be installed on
scalding juice, at the feed end, to achieve a bed temperature of at
Least 75 'C within one stage. Raw juice exiting the diffuser is usually
at 60 to 65 °C.

A typical temperature profile in a South African cane diffuser is

shown below.

-21-
 Temperature is a diffuser
Location Temperature (*C)'-.
juice 68
Stage 1 82

Stage 2 85
Stage 3 85
Stage 4 85
Stage 5 86
Stage 6 83
Stage 7 85
Stage 8 85

Stage 9 83
Stage 10 85
Stage 11 83
Stage 12 83
Press water 84

The use of biocides

Biocides have been used; Ravno and McMaster (1977) report that
full scale tests in South Africa have shown that shock dosing each cell Shot h dosing
of a diffuser once every four hours with formalin (a 40 °Io aqueous
formaldehyde solution), at 300 mg per kg cane, was effective in
controlling the activity of thermophilic microorganisms. Recently,
Richards (1999) has shown that the use of Biocides can be financially
justifiable. Many proprietary Biocides are commercially available; in
all cases it must be ascertained that their use (including that of
formalin) is safe, and is permitted under local health regulations.

Generally however, it is believed that the attainment of the right

temperatures in a diffuser is a simple, cheaper and more effective
means of microbiological control.

-22-
 5. DIFFUSER BAGASSE

5.1 Bagasse dewatering

Maisture levels in saturated cane
Bagasse at the last stage of diffusion is saturated with water, showing fibre
a humidity of about 82 a1o. The water content of saturated cane fibre
is reasonably consistent. Equilibrium moisture % cane, that is the
maximum amount of water that shredded cane can hold, after free
drainage, was studied by Lionnet (1985), in South Africa. He found
that for clean cane stalks, well prepared in a Jefffco cutter-grinder,
this equilibrium moisture ranged from 79 to 82 %. Lamusse (1979)
gives a value of about 85 %. It is thus necessary to reduce these high
water contents. This is usually done firstly through a light dewatering,
in the diffuser itself, and secondly by conventional milling.

*Light dewatering. Various light dewatering devices have light denaturing

been developed to remove part of the saturation moisture, called the
easy moisture, at the final stage of diffusion. They reduce the
moisture content of the diffuser bagasse to between 70 and 80 a1o.

The press roller or drum ( see the schematic drawing of a diffuser) is Press drum
a typical example of such a device. It floats on top of the cane bed,
and can be filled with water to increase its mass. It rotates freely, due
to the forward movement of the bed; it does not have an independent
drive. Press drums do not reduce moisture to a low level; a bagasse
moisture of 77 % has been measured. The bagasse must thus be
dewatered in heavy dewatering equipment, to be suitable as boiler
fuel. They do however compact the bagasse and they act as a weir,
preventing juice on top of the bed from flowing off at the discharge
end. The low dewatering efficiency may be due to the difficulty in
draining the liquid away.

Presses, such as screw presses which are well known in the beet
industry, have been tried. High maintenance costs due to erosion by
the sand and soil found in the cane, caused this approach to be
abandoned.

OMilling. By far the most common dewatering process for

diffuser bagasse is the use of the conventional three roller mill, as
found in the usual cane milling process. There are however a number
of problems which are particular to diffuser bagasse.

• Feeding the first dewatering mill with bagasse at 75 to 80 %

-23-
moisture may be difficult. Some form of feeding device is usually
required; Donnelly chutes and underfeed feeder rollers are used in
South Africa.

• Juice drainage can be a problem. Practices used in normal

cane milling, such as grooving and feed to discharge work ratios, may
be utilised to help the drainage.

Sanitation and general cleanliness are often difficult to

control.

Capacity for dewateriag

The milling capacity installed for dewatering diffuser bagasse in
South Africa ranges from about 0,2 to 0,8 m3 total roller volume per
ton fibre per hour (m 3/TFH). Generally a moisture o1o bagasse of
about 50 can be obtained with 0,3 m3/TFH if a single five-roller mill
is used, or 0,5 m3/TFH if two three-roller mills are used.

Finally, the required installed power is about 50 kW/TFH.

5.2 Press water treatment

The low brix juice extracted by the dewatering mills is called press
water. It is recycled to the diffuser where it can cause serious Blinding problems
percolation problems, through the blinding of the cane bed. These
problems are due to the impurities present in it, which include fine
particles offibre, sand, soil and any precipitate produced by the effect
of heat and of lime on the juice.

Earlier attempts to prevent blinding of the cane bed involved the ciariflcatfon or press water
clarif cation of the press water. A number of chemicals were tried and
much work was done at the Sugar Milling Research Institute, in the
early 1970's. This work showed that the effectiveness of press water
clarification was very dependent on the type and quality of the press
water. The chemicals and processes which worked at the beginning
of the season, or at a given factory, could be totally ineffective at
other times or elsewhere. Furthermore chemical costs were high.

Press water is also very susceptible to microbiological deterioration.

This additional difficulty caused sustained efforts to eliminate the Lifting screws
need for clarification. The mixing screws described in section 3.3.3
solved the problem. No factory in Southern Africa uses press water
clarification; all the diffusers have lifting screws and no problems are

-24-
evident.

The following information may be useful if press water clarification

An approaeb re r press water
clarification
has to be used.

0 The nature of the press water has by far the most impact on

clarification. Laboratory tests may be necessary.

Many chemical treatments, for example the use of

aluminium sulphate, of phosphoric acid, of sulphur dioxide, may be
very costly.

Work in South Africa showed that stable precipitates were

formed only at pH values above 10,5 or below 4,5.

0 A possible approach would be to lime to a pH of at least

8,5, heat to boiling, add a flocculant and settle. The clear supernatant
is sent to the diffuser while the muds arc added to the clarifier muds.
It should be noted that, in countries where the mass balance across
the extraction plant is used for cane payment, this approach will cause
an interference. Past experience has shown that the type of flocculant

to be used needs to be established by trial and error. Concentrations

of 10 to 15 mg of flocculant per kg press water have been used. Quality and qua ntity or press water

Details of the quality and quantity of press water, as measured in

Southern Africa, are as follows.

The brix of press water is generally quoted as being about 2 %. Catch

samples analysed recently in South Africa showed lower values,
ranging from 0,7 to 1,5. Apparent purity was about 50.

Material balances done in South Africa have given the following

quantities, arising from the clarification ofpress water, from 100 tons
of cane:

Mass of press water 37 tons

Mass of press water muds 3 tons
Mass of lune 0,4 tons
Mass of supernatant 34 tons

- 2 5-
 6. ENERGY

The impact of cane diffusion on the energy balance in a cane sugar

factory needs careful evaluation; it has been studied by van Hengel
(1989) and by Hoekstra (1995) among others.

Heating the prepared cane to an operating temperature of about 80

'C is normally done by vapour bled from the first or second effect of
Heat losses
the evaporator. Part ofthe heat supplied is recovered in the juice, but
a large proportion is lost in the bagasse. Another heat loss is due to
evaporation in the extraction plant. Using V 1 for heating, it has been
calculated that the overall steam requirements in a typical South
African installation would increase the steam to cane ratio by about
3 % on cane, say from 50 to 53 %. The steam (V 1 or V2) bled to the
diffuser is equivalent to about 11 % on cane.

Another point that needs to be noted is that the sand or soil in the
Impact of asb
incoming cane ends up in the bagasse when diffusion is practised.
This decreases the calorific value of the bagasse.

Hoekstra (1995) used computer simulations to compare the energy

needs of mills and diffusers. Looking only at energy and fuel
considerations he arrived at the following conclusions.

0 if no power is exported, V 1 only is used for process, and

bagasse is used for by-products, then milling with high pressure steam Some specific cases

production has the advantage.

* If no power is exported and bagasse is not required for by-

products, then diffusion and low pressure boilers are preferable.

Olf the maximisation of power export is required then the

diffuser is the obvious choice.

0 I f V 2 is used for diffuser heating and for the pans, then

milling and diffusion are equivalent.

Finally, a diffuser factory requires much less prime mover steam

Lower pressure boilers can be used. Typically, installed power values,
excluding cane preparation, are 90 to 100 kW/TFH for a milling
tandem, but 45 to 90 k W/TFH for a diffusion plant, or about half the
amount required with milling.

-26-
 7. RECYCLING OF CLARIFIER MUDS

Factories using cane diffusion have the possibility (Meadows, 1998)

of routing clarifier muds to the diffuser. From a sugar technology
point of view there are no serious reasons why muds should not be
returned to the diffuser. Since the introduction of cane diffusion it is
clear that filter cake tonnages, and thus the amount of mud, have
decreased to about half the levels found with milling. Thus, roughly
half the suspended solids in mixed juice has already been retained by
the cane bed. This did not cause any special problems.

The results obtained in South Africa show no adverse effects as far

as extraction and processing in general are concerned, when muds
were returned to the diffuser. In all cases financial gains were
i dentified, due mostly to the elimination of the operation, Advantages of routing muds to the
diffuser
maintenance and labour associated with the filter station, to the
elimination of costs associated with the handling, transport and
disposal of filter cake, and to small savings in energy due to the
elimination of filter wash water and to the availability of all the
bagacillo as fuel. A reduction of sucrose losses is expected and this
adds to the financial gains.

There are some negative aspects. Ash in bagasse increases by about

10 %, which affects boilers negatively. This can however be Disadvantages
corrected by reducing sand levels in the incoming cane. Many
factories operating wet scrubbers mix the smuts with the filter cake,
for disposal on cane lands. This is not possible when there is no filter
cake and a smuts disposal problem may arise. When, like in South
Africa, the mass balance around the extraction plant is used for cane
payment, the mud needs to be weighed, sampled and analysed.
Equipment and procedures may thus be required.

The mud should be returned to a set of lifting screws; as far as

Special precwifous
possible the screws should be located at a point where the brix of the
percolating juice is roughly the same as that of the juice in the muds.

Another precaution concerns the temperature of the muds; it must

not be allowed to decrease by letting the mud stand. Finally, mud
withdrawal must be regulated so that excessive quantities of clear
juice are not lost with the mud.

-27-
 8. COMPARISON WITH MILLING

While extraction by milling has always been the conventional method Milling „a moving bed ease
of processing cane, extraction by diffusion is now an alternative diffusion
option. Its adoption in Southern Africa has been steady, and more
than 25 years of experience have now been gained. It is therefore
possible to compare the two approaches; this will be done in terms
of cane preparation, operations, raw juice quality, energy and costs.
The comparison deals with moving bed, cane diffusers.

8.1 Cane preparation

This has been dealt with in detail, in section 2. It is even more
important with diffusion, than it is with milling, being the most Heavy sbrtdding

important variable affecting extraction in diffusers. As described in Light knifing

section 2, the way in which the cane is prepared is critical. It was
shown that heavy duty shredders with a minimum of knifing is the
best approach.

8.2 Operations
Because of the long cane residence time in a diffuser, start up and
liquidation are more prolonged. Similarly, if long stops, say six hours Stoppages
or more, are encountered, it is advisable to empty the diffuser to
avoid deterioration; this would not usually be a concern with mills.

Usually, all stages are filled with water before starting up. Thus an Water supply
adequate supply of water is needed.

After the first cane reaches the diffuser, it takes about one hour for Bagasse storage
bagasse to reach the boilers. Adequate bagasse storage and reclaim
is thus needed.

At shutting down liquidation takes much longer; large quantities of

low brix juice are produced.

On the positive side, diffusers can cope well with wide cane Throughput flexibility
throughput rates. Speed can be reduced as low as the drive allows.
Bed heights can also be changed.

I mbibition rates are limited by evaporation considerations. In a

milling tandem very high rates of imbibition may affect feeding i mbibition

negatively. In South Africa imbibition levels of up to 400 °Io on fibre

have been handled by diffusers. Finally, mills require more attention
due to the use of large forces and pressures.

-28-
8.3 Juice quality
-Suspended matter- The concentration of suspended matter Suspended matter
in mixed juice is considerably lower with diffusion. Extensive data
obtained in South Africa show that mixed juice from milling tandems
contains up to three times more suspended matter than mixed juice
from diffusion. Comparable results show suspended matter levels of
0,2 % (mass/mass) in diffuser juice against 0,6 °/v in milling juice.

-,Colour- Colour affects sugar quality, particularly if the

Colour
refining of raw sugar is considered. Raw sugar itself may have a
colour standard; in South Africa VHP (very high pol) sugar has a
colour limit. Work done in South Africa has shown that there is little
change in colour from mixed juice to syrup, with the classical
defecation process. It has also been shown that the colour of VHP
sugar is equal to about 6 % that of the syrup, under normal South
African operating conditions. Thus sugar colour can depend very
much on juice colour. It has been well established that diffusion
extracts more colour from the cane than milling does. Comparisons
in the South African industry show the following results.

Cane colour Misled juice Difference

colour {MI-CaneyCane 25 % more colour in diffusion juice
(~Io}

Milling 23680 23000 -3

Diffusion 22480 28090 +25

The above results show that there is no real difference between the
cane colour and that of the extracted juice when milling is used. In
the case of diffusion however the juice shows a higher colour. This
is due to the long retention times, the high temperature and pH
effects if lime is added.

It must also be noted that cane stalks, tops and trash have very
different colours. Results obtained in South Africa are given below.

-29-
 Colour .;- .
The eololar of clean sulks, tops and
trash
Clean stalks 13400

Tops 140000

Trash 640000

Reducing the amount of tops and trash in the cane has a marked Effect ofernaatous matter
impact on the total colour entering the factory. Thus, with diffusion
the presence of vegetable extraneous matter is very undesirable.

-Starch- The level of starch found in diffusion mixed juice is

Lower Levels of starch
much lower than would be found with milling, for the same content
in the cane. The high temperature used during diffusion causes the
gelatinisation of the cane starch granules; this renders the starch
available to natural enzymes in the cane which then degrade it.

-Lactic acid- The formation of lactic acid during diffusion is Lower keels of lactic acid
lower than that with milling. This is due to the reduced
microbiological activity at the higher temperatures used during
diffusion. Comparable values obtained in South Africa show about
270 mg lactic acid on brix in diffuser juice, compared to 560 mg in
juice from milling.

•AcetatelSilicae The concentrations ofthese two species can

Effect of Goat on acetate sod silica in
be higher in diffuser juice, when compared to milling. This is usually juice
due to liming, more particularly over liming.

Koster (1995) provides a thorough comparison between diffusion and

milling, based on data for five seasons. His results are given below.

Diffusion Milling . Comparison between milling and

diffusion
Extraction 97,8 97,5

Pol % bagasse 0,87 1,03

Imbibition % fibre 390 344

Boiling house ref. 87,5 87,8

Pol lost in filter cake 0,23 0,42

Lactic acid mg/kg bx 380 540

- 3 0-
8.4 Steam and energy
This has been covered in section 6. Here we will concentrate on the Ash la bagasse
ash content of bagasse.

In South Africa the sand and soil contents of cane and bagasse are
estimated by an ashing technique. A known mass of shredded cane or
of bagasse is ashed in a laboratory oven at 850 °C. The residue, that
is the ash, is weighed and expressed as a percentage by mass on the Analytical method

cane or bagasse. The high temperature quoted above does have

disadvantages; for example it causes severe corrosion ifstainless steel
crucibles are used as containers. The possibility of using a
temperature of 650 'C has therefore been investigated and generally
found to be acceptable.

The cane bed in a diffuser retains most of the sand or soil entering the
factory in the cane. In the case of milling, the sand or soil finds its Impact of sand
way into the juice. Measurements done in South Africa have given
the following results.

Ash % cane Ash % final bagasse

Diffusion Milling

0,8 1,9 1,3

1,6 3,2 2,0

2,4 4,4 3,3

Thus, for a given ash level in the cane entering the factory, the ash in
bagasse will be higher with a diffuser. This has a direct impact on the
boilers where tube erosion may be a costly problem. Sand in the
bagasse will also decrease its calorific value. Sand in the juice from
a milling tandem will cause ehokes and stoppages as gutters, tanks
and other vessels fill up. Erosion is also a problem but it will affect
less costly equipment.

Finally there can be instances when the sand content of the bagasse
is so high that the fires in the boiler furnaces are physically put out.
This tends to happen when ash % bagasse reaches levels of 5 °Io and
higher.

-3 1-
8.5 Costs
The extraction plant is generally a high cost item in the complete
sugar factory complex. Absolute costs are of little value because of
differences in costs in different countries and because ofinflation. The
relative costs between diffusion and milling are therefore used here.
Lamusse (1979) and Rein (1995,1999) give much detail. They show
that comparisons must be made between a diffuser plus its dewatering
mills and a milling tandem. In that case, comparison of capital cost is
a function of the extraction desired, as shown in the table.

96 1 loo 1 66

98 100 60

One of the noticeable advantages of diffusion is the significant

reduction in maintenance requirements. Lamusse and Rein show that
the maintenance casts of a diffusion plant are of the order of 50 to 60
% of those of a milling tandem, These figures take into consideration
the fact that the diffuser chain either has to be replaced or needs to
have its pins and bushes changed periodically.

A diffusion plant can be operated with less supervision. Fewer

operators may therefore be necessary, resulting in lower manpower
costs. Offarop maintenance labour requirements are also reduced
significantly.

Two other points may be made. The diffuser requires less heavy
foundations and can be located in the open.

Finally, the filter cake production from diffusion is about half that of
a milling tandem, mud routing to the diffuser has also been shown as
a cost saving possibility.

-32-
 9. NEW DESIGNS

After developments during the mid 1964'8 the diffusion process

quickly settled on either fixed bed, or horizontal moving bed designs.
In both cases 12 to 18 stages were needed to achieve the extractions
required by the industry. Many workers however, noted that the stage
efficiencies were low.

The concept of displacement, as opposed to mixing or separation,

Displacement
has been discussed and designs generated to use it. The basic
approach consists of the following.

0 Air is displaced from the cane bed by an upward flow ofthe

juice.

:This is followed by a downward displacement of the

enriched juice in true plug flow,

0A final displacement is then performed, by a mixture of

press water and imbibition water.

This approach is seen as requiring three stages only and a much

shorter contact time, while achieving very high (98 %) extractions.
Walsh (1998) gives details and describes an industrial prototype.
 BIBLIOGRAPHY

Barker B and Lionnet G R E (2400). The use of lime saccharate to replace milk of lime for liming in
diffusers. S Afr Sug Technol Assoc 74, in press.

Boshoff TL (1994). Shredder drives. S Afr Sug Technol Assoc 68, 169-171.

Buchanan EJ (1967). The appraisal of diffusion performance without confusion. S Afr Sug Technol
Assoc 41, 94-100.

Clarke CD and McCulloch JR (1970). The performance of a heavy duty shredder. Proc Queensland
Soc Sug Cane Technol, 37, 181-195.

Crossman MT (1994). A review of modified shredder systems. S Afr Sug Technol Assoc 68, 166-
168.

Cullen RN and McGinn JA (1974). Photographic analyses of the action of a cane shredder. Proc Int
Soc Sug Cane Technol Ass 15, 1583-1589.

Douwes Dekker K (1956). Milling-diffusion process as applied in Egypt. S A Sug J, 789-793.

Foster DH and Hill JW (1966). Pilot plant diffusion experiments. Proc Queensland Soc Sug Cane
Technol Assoc 33, 111-I 19.

Freund P (1968). A theoretical approach to cane diffusion. Proc Int Soc Sug Cane Technol Ass 13,
133-141.

Fruend P (1968). BMA cane diffusion, the Egyptian system. Sug J Nov 1968, 23-26.

Graham WS, Morris RM and Oosthuizen DM (1968). Preliminary physiochemical studies on

sugarcane diffusers. Proc Int Sac Sug Cane Technol Ass 13, 122-131.

Hoekstra RG (1995). Energy consequences of diffusion vs. milling. S Aft Sug Technol Assoc 69,
205-207.

Ivin PC, Clarke ML and Blake JD (1987). Comparison ofextractives from milling and diffusion. Proc
Aust Soc Sug Cane Tecnol Assoc, 191-199.

Koster KC (1995). Some downstream effects resulting from diffusion compared with milling as
published by the South African industry. S Afr Sug Technol Assoc 69, 201-204.

Lamusse JP {1974). Five years of diffusion in South Africa. South African Sugar Yearbook, 1970-
1971, 19-23.

Lamusse JP (1979). Practical aspects of cane diffusion. Sug Tech Rev 7, 197-253.
Lionnet GRE (1985a). Preliminary study on the extraction of some impurities from cane during
diffusion. S Afr Sug Technol Assoc 59, 92-95.

Lionnet GRE (1985b). A study of the extraction of non-sucrose components of sugar cane. M Sc
Thesis, University of Natal.

Lionnet GRE (1983). The specific cake resistance of South African muds. Int Sug J 86, 80-83.

Love DJ and Rein PW (1980). Percolation behaviour of cane diffusers. Proc Int Soc. Sug
Cane Technol Ass 17, 1900-1924.

Maxwell F (1932). Modem Milling of Sugarcane. Norman Rodger, editor, London.

McMaster L and Ravn6 AB (1975). Sucrose losses in diffusion with reference to thermophilic bacteria
and lactic acid. S Afr Sug Technol Assoc 49, 149-52.

McMaster L and Ravno AB (1977). The occurrence of lactic acid and associated microorganisms in
cane sugar processing. Proc Int Soc Sug Cane Technol Ass 16, 2679-2693.

Meadows DM, Schumann GT and Soji C (1998). Farewell to filters: the recycle of clarifier muds to
the diffuser. S Afr Sug Technol Assoc 72, 198-203.

Moor B St C (1973). The Tongaat shredder. S Afr Sug Technol Assoc 47, 100-105

Moor B St C (1974). An evaluation of very fine shredding. Proc Int Soc. Sug Cane Technol Ass 15,
1590-1601.

Moor B St C (1994). Review of cane shredding. S Afr Sug Technol Assoc 68, 162-165.

Nicklin JH (1967). Power and energy requirements far cane preparation. Proc Aust Soc Sug Cane
Technol, 171-181.

Payne JH (1968). Cane diffusion - the displacement process in principle and practice. Proc Int Sac
Sug Cane Technol Ass 13, 103-121.

Payne JH, Sloane GE and Silver BS (1966). 1966 investigations on the diffusion operation at Pioneer
Mill Co. Ltd. Hawaiian Sug Tech 28, 86-91.

Reid MJ (1994). A review of cane knifing. S Afr Sug Technol Assoc 68, 159-161.

Rein PW (1971 ). The mechanism of extraction in the cane sugar diffusion process. Proc Int Soc Sug
Cane Technol Ass 14, 1254-1266.

Rein PW (1972). A study of the cane diffusion process. Ph D Thesis. University of Natal.
Rein PW (1995). A comparison of cane diffusion and milling. S Afr Sug Technol Assoc 69, 196-200.

Rein PW (1999). A review of diffusion in South Africa. Int Sug J, vol 101, 192-234.

Rein PW and Ingham PJS (1992). Diffuser performance optimisation through control of liquid flow
patterns. Proc Int Soc Sug Cane Technol Ass 21,779-796.

Renton RH (1974). A preliminary survey of power requirements for cane preparation. Proc Int Soc
Sug Cane Technol Ass 15,1575-1581.

Richards W (1999). Biocides at UCL. S Afr Sug Technol Assoc 73, in press.

Rivalland .JFR (1984). Milling and diffusion in Mauritius. Rev Agr Sucr He Maurice 63, 22-30.

van der Reit CB and Renton RH (1971). The Ernpangeni diffuser installation 1967-1970, S Afr Sug
Technol Assoc 45, 49-55.

van Hengel A (1989). Diffusion as a steam saver. Proc Int Soc Sug Cane Technol Ass 20, 233-241.

Walsh GH (1998). The Riviere juice extractor: a new approach to the extraction of juice from cane.
S Afr Sug Technol Assoc 72, 173-184.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

1 Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation. The fundamentals
6 Evaporation. The practice
7 Pan boiling 1
8 Pan boiling II
9 Diffusion

In preparation;-

Milling
Boilers
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)
 REFINERY
CARBONATATION
 Sugar Technology For Students

REFINERY
CARE ONATAT I ON

Prepared by G R E Lionnet

Study Text 10

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 2000

Copyright 0 2000 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-26009-2

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
r____________-
AFF SYRUP ~.........................

F -------------------
, ....,.,.„„„,.............., AFFINATIDN --------------_i
_______.,_____
--------------- __ __a ; AFF SYRUP i
~_________-___:
 1. HISTORY

1.1 Relining

In terms of its commercial importance, sugar is usually classed as Raw and reflaed sugars
either "raw sugar" or "refined sugar", the main distinction being one
of quality, mostly colour. Thus raw sugar can have colours ranging
from one to several thousands colour units; the corresponding range
for refined sugar is very much lower and narrower, typically from
about 20 to 60 colour units.

The distinction can be confusing and there is overlapping. Thus, in Beet and tans
the beet industry, there is usually no "raw" sugar; beet factories
produce white or refined sugar directly. In the cane industry it has
been traditional to first produce a raw sugar, in most cases. This raw,
yellow coloured sugar, may then be refined. The refining can be done Refiaiag.-

in another country; it can be done in the same country but in After export
standalone, large refineries; or it can be done in what is called a Staadalone
Batftend
"backend" refinery, which is a refinery attached to a raw cane sugar
factory. In this last case services, energy, staff, etc, are shared.

The situation, in the cane industry, can be somewhat confused when

the concept of "plantation, or mill white" sugar is met. Typically this Pisntatioa or mill wfiitt sugar
will be a sugar of a quality (again mostly colour) better than that of
a raw sugar but not as good as that of a refined one. Criteria are now
less defined and local specifications usually apply.

Refining has been defined as the purification of sugar through

recrystallisation, and chemical, and physical methods.

1.2 Carbonatation

In 1967 Chapman noted that carbonatation had been used by refiners

for more than 85 years, which now makes it nearly 100 years old, as
a refining process.

Carbonatation was introduced in the beet industry, in 1812, by

Sarruel. The beet juice was limed to high alkalinities and the excess Carboaatatioa with beet
lime was eliminated by using carbon dioxide gas. This became
common practice in beet factories, and it is still used today.

In 1863 Jelineck and Frey added lime and carbon dioxide

simultaneously into the beet juice, and Jaquiers introduced the plate
and frame filter to the industry.

It was tried on cane juice, in Java, in 1876. By 1880 it was well In cane factories
established in the cane factories of Java, and carbonatation could
produce cane sugar which was equal in quality to white beet sugar.

Carbonatation was the subject of much investigation in the cane

industry over the period 1890 to 1905. By 1910 it was well
established; over the next 30 years a number of developments such as
the double carbonatation process, the De Haan process, and middle
juice carbonatation, were introduced.

Rault (1960) notes that carbonatation was introduced for treating Used at tbe NaLid Estates
factory in 192!1
cane juice, at the Natal Estates factory in South Africa, in 1920. A
white cane sugar was produced. In March 1959 flue gas
carbonatation was introduced at the Huletts refinery, in South Africa,
where it is still in operation now. It is also used in six backend
refineries in Southern Afica.
 2. THE CHEMISTRY

2.1 C0 2 and water

The chemistry of carbon dioxide is well described in chemistry

textbooks, but as is omen the case, the conditions which apply are Theoretical Limitations

ideal; thus the system consists ofpure water, pure calcium hydroxide,
dilute solutions, etc., at 25 ° C. This simplifies the discussions and
makes the results more exact but less practical. It is nevertheless still
useful to consider some of these basic properties.
Solrtions in water
C02 in aqueous solution exists only partly as H 2CO,, being largely
present as C0 2 (.,), the ratio of C0 21H 2CO3(4 being 600:1.

C02{aq} + H2O H2CO 3tav

H2C03 is a weak acid, ionising in two steps, and thus a solution of

C02 in water is slightly acidic with a pH of about 5,7:
Weak acid ionisation

H2CO3i&q3 + H20cn H30 +i 10 + HC03 -(aq)

HC03 + H2 0tn r H30 { (.q) + CO 2-1.q3

2.2 CO= and OH -

As a weak acid, a solution of carbon dioxide in water will react with Reactions with lime
bases. Of particular interest here is its reaction with lime or calcium
hydroxide

C02(g) + H20iu H2CO3(.l)

H2CO 3t4 + Ca(OH)2 " CaC03gsl + 2H20tn

The calcium carbonate precipitates and removes calcium from

solution, but with more carbon dioxide

CaCO3(,) + C02(s) + H20ti} Ca" (10 + 2HC03-(,o

and now the bicarbonate is soluble. This reintroduces calcium into the

_3_
solution.

As with most weak acids, reactions and equilibria are controlled by

pH. In this system it is established that : EfeaofPH

C02 - + H2 O H2C03 is slow and

H,CO3 + 0H - '7c~ HCO3 + H2O is fast at pH values < 8.

At pH values > 11 however

C0 2 + OR HC03 is slow and

HCO; + OH- - C03 + H 2O is fast.

In the pH range of 8 to 11 both sets of reactions occur.

Interpretations of acidlbase behaviour of this type of system are
therefore complicated since reaction rates vary and there are pH
dependencies.

The situation in impure sugar solutions of high brix and at high

temperatures when carbon dioxide reacts with milk of lime, can only Limitadons

be more complex. The solubilities and equilibria cannot be established

with any certainty. The measurement of pH under these conditions is
difficult. For these reasons laboratory or pilot plant investigations
dealing with carbonatation in the sugar industry are very system
specific.

2.3 Solubilities and dissociation equilibria

The efficiency and control ofthe carbonatationprocess depend on the Limiwiaas

solubilities of lime, carbon dioxide, calcium carbonate and other
calcium salts taking part in the reactions, since only dissolved species
can react. Thus the need to look at solubilities and at dissociations.
Again, the limitations mentioned in the previous sections will apply.

Acid-base equilibria in water:

Say we have an acid, HF, in water :-

HIF(aq) + H20(t) Y H30+i 4 + F (sq)

-4-
We can now propose an approximate equilibrium constant, Y, for Egailimamconstsat

the above reaction as

[ H3 a+] [F_]
K

For dilute solutions we can propose an acid ionisation constant, K„

as

Acid loalsstion constsat

H
Ka = [ 3 0+1 IF]
[HF]

In both equations the square brackets represent concentrations.

A generalised approach yields :-

HA H+ + A-

and

+ [A_
[H I ]
Ka
[HA]

strength of acids
Acid ionisation constants give an indication of the strengths of acids.
For a strong acid, Ke at 25 ° C is about 1x10 7 ; that is the product ofthe
concentrations [H+] and [A-] is high, while [HA] is low. There is a
high concentration of H' ions in the solution.

For a medium strength acid K,,, at 25 - C, is about 2x l O -S. A very weak

acid would have a K, value of about 5x10 -'°.

Some acids have two ionisation constants. Thus for carbonic acid :-

Diprotic acids
H2C03 H+ + HC03

HCO3 Y H+ + CO32-

and each step has its own ionisation constant, K,,, and K.2 :-
 -
__ [H+ J IHC0 3 l

'` [H2C031

and

2.
[H+l [CO3 1
K.2
[HCO 3- 1

The values of K8, and K. 2, at 25 ° C, are 4.5x10-' and 4.7x14""

respectively. Thus carbonic acid is a weak acid; its second ionisation
is weaker than the first, a usual property of diprotic acids.

The concept of more than one ionisation can be extended to Polyprode acids
polyprotic acids, that is acids with more than two ionisation
constants; a good example in the cane sugar industry is aconitic acid,
with three ionisation constants.

Sucrose can behave as an extremely weak acid, with a K,, value of

saccbarale
3 x l 0 -'3 and a K., value of 3x 10 -1°. Thus, calcium hydroxide will react
with sucrose in aqueous solution to form a saccharate or sucrate ion.
Aqueous sucrose solutions will thus cause more calcium hydroxide to
dissolve than will be the case with water, as shown in the following
table.

Solubilsty of Ca(OH) 2 (in gram Ca0 Per 100 ml solution) ...

at fi0'C to sucrose solutions

Sucrose conc. (g1100 cm3 sol') g CaO 11(10 cms solution

0 0.09

12 0.42

24 2.0

30 3.1
2.4 Solubility product

Lice ionisation constants, solubility product is a concept which allows

the quantification and comparison of a chemical property in a
meaningful way. Say we have a compound such as calcium carbonate, Solubility product of calcium
in contact with water. A small amount of the carbonate will dissolve carbonate

and, at equilibrium we can write the following equation:-

taco (,) ' ca2+t•v + ca,2-(w

We can again write an equilibrium expression based on
concentrations, as follows:-

_ [ Ca 2+(.,1) ] [C03 2- cagf 1

Ke
[ Caco 3(s) ]

This is usually simplified to

K sp =
[Ca 2+cap 11C03'+(14] Solubility product COWant

where K, p is called the solubility product constant of calcium

carbonate. The higher the solubility product constant, the more Some values for 1C,
soluble the material. K, p values are affected by the temperature. Thus
for calcium carbonate (calcite form), K sp is equal to 4.4x10-9 at 25 °C.

Calcium hydroxide has a K, p value of 5.5x10 at 25° C, while the K~p

ofcalcium sulphate is 2.4x10 -5 at the same temperature. The K, p value
for calcium carbonate in a pure sucrose solution, at 85°C, is 7.5x10 -'.

In impure sucrose solutions, the li p concept loses its full usefulness,

as Ksp values now depend on the type and concentration of the
impurities.

The solubility of carbon dioxide in water is low; at 20'C and Solubility orearbon dioylde
atmospheric pressure, 100 grams of water will dissolve about 0.2g of
carbon dioxide. This will decrease to 0.08g at 50"C.

Carbon dioxide will dissolve in alkaline solutions as long as alkalinity

Effect of pH
is available to form carbonate or bicarbonate ions. In solutions2-
containing lime, OH" is available and C02 will dissolve to form C03
and HC03. pH has a marked influence on the equilibria; the ratio of
carbonate to bicarbonate concentrations, at 85 °C, as a function of
solution pH is shown below.

11 12 8

10 1.2 46

9 0.1 89

8.5 0.04 96

8.4 0.03 97

8.3 0.02 98

8.0 0.01 99

7.0 0.001 99.8

Calcium bicarbonate is soluble in water and will thus retain Ca" in i mpact arblearbonate

solution, which will affect the carbonatation process negatively.

2.5 Destruction of monosaccharides

It is well known that sucrose is chemically stable under alkaline

conditions, whereas this is not the case with glucose and fructose.
The two monosaccharides will degrade under alkaline conditions, the
kinetics being influenced by temperature and pH.

In beet juice the concentrations of fructose and glucose are very low,
Fructose and glucou in beet
and carbonatation is used to cause the complete elimination of these
two monosaccharides. Much work has therefore been done, in the
beet industry, to study the chemistry of these monosaccharides under
alkaline conditions. Some of the main results are as follows.
Chemistry of F and G ln alkaline
0 When treated with alkali the monosaccharides isomerise solaHons
extensively. This can be followed by the carbon chain breaking.

!Although the reactions are extremely complex, the following

scheme has been shown to be relevant to the destruction of F and G
under alkaline conditions.
 F and G (CH,,O,)
simplifled reaction scheme for the
I (isomerisation) degradation of F and G

ENEDIOLS straetarn (6 C atoms)

TWO TRSOSES (3 C arotms) DICAR$ONYL eontpouads

ACIDS sad SACCHARINIC acids

ALDEHYDES f6 C atoms. important
(3 C atoms) degradation products)

LACTIC acid
(3 C atoms Main degradatioa product) ACIDS and ALCOFOLS
(6 C atoms)

These investigations have shown that about two moles of acids (all
Lactic acid
acids formed) are produced from the degradation of one mole of
monosaccharide. Many of the acids formed are relatively stable and
would leave the process in the molasses. Lactic acid is the single most
important degradation end product; it constitutes between 30 to 50%
( by mass) of the products. This has a practical importance in the cane
industry, where there are relatively high concentrations of F and G.
Calcium lactate is soluble and will thus keep the Ca' ion in solution.
This problem will be discussed later.

The simplified scheme shown above does not highlight the formation Culoar
of colour, which normally accompanies the degradation of F and G in
practice.

The effect of calcium ions needs to be considered since these ions are The effect of Ca"
always present during carbonatation. Ca" tends to form complexes
with F and G, and these reactions yield 3-carbon atoms compounds.
Again lactic acid turns out to be the most important end product.

Workers in the beet industry have investigated the kinetics of the

Kiaetica:-
alkaline destruction of F and G. The results can be surr,_n1?rise d as
follows:-

*At 78 °C, 80 °Io of the monosaccharides was destroyed, at

high pH values, in 15 to 24 minutes.
 Temperature
*The activation energy was found to be about 1070lmol,
over a temperature range of 70 to 110 °C, and pH levels of 9.5 to 13.
This is a high activation energy and it is evident that the destruction
will be accelerated greatly by temperature.

*At 7$'C high concentrations of the calcium ion increased Presence of Ca='

the rate of degradation by 50%.

In practice beet juice is treated at high pH levels (11 to 12.5), at

about 95'C, with a lime content of about 1% CaO on juice (by mass).
Obviously fructose and glucose will be destroyed under these
conditions. Typical results obtained in the beet industry are shown in
the following figure.

%2,5 llesrroction rates of F and G io

beetjoice
u 2
u
0 1.5
1
U
Ut
90-5
z
0
0
a 5 to 15 20
REACTION TIME (min)

It is evident that the concentrations of the monosaccharide can be

expressed by a formula of the form

Ct = C a exp,

where C, and Co are the concentrations at time t and initially, Effect or original cooeentratioa
respectively. a is a rate constant and t is the reaction time. The rate of
degradation is clearly dependent on the original concentration of the
monosaccharide. This again has practical implications in the cane
industry.

Cox et al. (1990) give an excellent description of the problems that

monosaccharide degradation can cause in a cane sugar refinery using Reedcment

carbonatation. It is well established that the yield of refined sugar can

be estimated from the rendement formula, namely

R = Pal % - (4.5xAsb% } 1xReducing sugars °Ia)

where R is the rendernent or yield in o/o; Pol %, A°%% and Reducing

sugars°Ia are the percentages on raw sugar feed. This formula worked

-10-
well in the refinery under study, using very high pol (VHP) sugar as
feed. Ash balances in the refinery showed a severe (50%) increase of F and G degradation and lactic
acid formation in a cane refinery,
ash over carbonatation, and this increase could be attributed nearly wick carbanatation
entirely to a build up of calcium ions. At the same time lactic acid was
found to increase across the carbonatation station, and it was clear
that this could not be due to microbiological activity.

Cox et al. performed laboratory tests and demonstrated clearly that

the alkaline degradation of monosaccharides was taking place, with
the formation of lactic acid as the main end product. They showed 100 lactic acid= Z2 ca" in solution
that 100 parts of lactic acid caused about 20 parts of Cat ' to be
retained in solution, which is close to the stoichiometric value given
by the equation

CaCO3 + 2C3H60 3 =* Ca(C 3H503) + H2CO3

The formation of lactic acid, and thus the degradation of F and G, Effect or lime dosage
increased as the lime dosage to the melt increased. At 80 ° C a sharp
increase (about double) was seen between 1.4 and 0.7% CaO on brix.

At 0.7% CaO on brix, the formation of lactic acid was very Effect of temperature
temperature dependent. This is shown in the following table.

Temperature (°C) Lactic acid (mgtkg brix)

60 150

70 180

80 300

90 450

Finally, the amount of lactic acid formed depended on the

concentration of monosaccharides.

These results are thus very much in line with the findings obtained in
the beet industry.

Cox et al. conclude by showing that the soluble ash increase was
reduced to normal levels by decreasing the liming temperature to Practical solutions

about 75 ° C, by reducing the lime dosage to 0.5 to 0.6°IoCaO on brix,

and by keeping the retention time in the melt liming tank as short as
possible.
 3. THE PROCESS

3.1 General

As stated earlier carbonatation has now been used for nearly 100 Gent
-
12 ral advantages and
years for the refining of cane liquors. It is a robust process using disadvantages of carboaabttioa
cheap reagents, but the plant is heavy and bulky. The gas scrubbers
can be cumbersome and lime plants are usually dirty and expensive to
maintain. The disposal of the filter cake can be a problem; filtration
requires large plants, the process is messy, needs much labour and
produces large volumes of sweetwater; filter cloths can be costly and
need special cleaning. Nevertheless, the process is well utilised in
many cane sugar refineries.

Carbonatation has two main objectives :-

plain objectives
0 To produce a voluminous precipitate of calcium carbonate
with a surface area as large as possible on which the impurities can be
adsorbed. Less solubles salts such as sulphates, colour bodies, starch,
and many other impurities are entrapped by the calcium carbonate.

0 To condition the precipitate for efficient separation by

filtration.

These two objectives are usually conflicting. For good impurity

Filtratlon vL impurity removal
removal a large surface area for the calcium carbonate crystals is
needed, which can be achieved by very intimate contact between the
carbon dioxide and the limed liquor. This will tend to result in many
small crystals being formed, thus increasing the surface area for the
same mass of crystals. A small crystal size is however not the
optimum from a filtration point of view. In full scale plants the usual
practice is to improve the filtration performance even if this reduces
the efficiency of impurity removal.

saturators
Full scale carbonatation cannot be performed in one step only, that is
by using one saturator only, mainly because of the large gas flows
that are required. For good filtration and good impurity removal,
experience has shown that a final liquor pH of 8.0 to 8.5 is needed,
and that the liquor temperature should be about 85°C. This requires
a large volume of gas and may result in high heat losses. A good
compromise is to use two saturators, in which case about 75% of the
gas is added in the first. Three saturators can also be used, with 75 to

-
90% of the gas being fed to saturators one and two; this has the
advantage that one of the saturators can be taken off line for cleaning,
without having to stop the whole process.

Batch carbonatation can be done, but has the major disadvantage of

having an uncertain impact on the filtration process. As a result of Batch carbonatadon

this, it has been abandoned industrially. The continuous process is

used universally and provides steady operation with good pH and
temperature control.

According to Chapman (1967) temperature is not critical in the first

two saturators of a set of three. A range of 60 to 80°C is found in
industry, with the lower value being thermally advantageous. The Temperatures

liquor then leaves saturator two at a pH value of about 9.6 and needs
heating to 85°C and gassing down to a pH range of 8.2 to 8.5 in
saturator three. Here, the higher the temperature the less the
formation of the soluble calcium bicarbonate.

3.2 Carbonatation flow sheet

The carbonatation refining process consists of four essential Melting, liming. carbonatation and
filtration
processes, namely melting, liming, carbonatation and filtration.
Depending on local conditions, an affnation stage may be needed. All Anluation

these processes will be considered individually later; except for

affnation, they are represented schematically in the following flow
sheet. This will provide an overall view of carbonatation.
 Lie god liquor ~"
MELT

MiR of 11me

WATER STEAM

MYLTFR
1-r
1-146
AFFLYATEP
SUGAR VENT

Saturator 1 Saturator 2 Saturator S

STEAM STEAM

. .. : : - I oxq l I] ~

WATER CARBONATED LI UOR

SLUDGE
FILTERS
WATER

FTLTERED LIQUOR
TO PROCESS PLA'T'E AND FRAMES

SWEET WATER
TO MELTER I I CAKE TO
ALSPOSAL

- 1 4-
3.2.1 Affination

This, when required, is the first process in refining. If the purity ofthe Isereases the purity of the feed to
raw sugar feed is low, then it is necessary to increase the purity of the the refinery

feed into the refinery by removing the relatively impure molasses film
found around the sugar crystal. This leaves behind the much purer
crystal itself, which is then dissolved.

Low purity raw sugars are mixed with an affination syrup to form a
magma. This is stirred in a magma mixer; the stirring movement Aluated sugar
causes the molasses film around the crystal to soften and predisposes
its removal by a centrifugation process. The resulting sugar is now
called affinated sugar or afned sugar. A material balance around an
affination station is given on page 19.

Affination requires high capital and equipment costs (centrifugals,

costs
tanks, mixers, etc.) and high operating costs. The latter include the
costs of handling the affination syrup, a material which is particularly
difficult to exhaust.

In South Africa it has been found (Alexander, 1971,1981; van

Hengel, 1952) that it is financially and technically justifiable to
produce a raw sugar which is pure enough to allow the elimination of VHP
the affination station in local refineries_ The sugar factories thus
produce a very high pol (VHP) sugar, with a pol of at least 99.3%
and, as a result, a colour which is relatively low; there is no need to
affinate VHP to produce refined sugars of the required quality. The
production of VU? in raw factories does impact on their
performance. It is accepted that there is a cost, both in terms of
throughput and of recovery, attached to the production of higher
purities raw sugars.

3.2.2 Melting

Traditionally in the sugar industry melting means dissolving a sugar Melting, meiter and melt

in a stirred vessel called a melter. The resulting melt is then

processed.

In refineries hot condensates and hot, impure sweetwater are used to

melt the raw sugar, producing a melt at about 70 ° C and 65 Brix. Proem details
Steam (exhaust or vapour 1) is used for heating, and rotating paddles
agitate the contents. Melters are sized to give a retention of about 20

- 1 5-
to 30 minutes. A sieve or screen is usually found at the exit of the
melter.

Under industrial conditions the colour of the melt is usually higher

Colotir
than that of the raw sugar used. This is caused by the use of impure,
often highly coloured sweetwater, and by the practice of returning a
number of reject refinery streams to the melter. This latter practice
should be strictly controlled, if not eliminated altogether. Colour
surveys in South Africa have shown that it is possible to limit the
colour increase across melters to 5%; increases above this level
should be investigated and eliminated, particularly in backend
refineries.

3.2.3 Liming

Liming is obviously a critical step in the carbonatation process. Milk

of lime, usually at 15 Beaume, is added to the melt, to reach the pH vs. volume of milk of lime
desired level of alkalinity. The amount of lime required for efficient
carbonatation is relatively high; pH cannot be used to control the line
addition because of the lack of sensitivity in the relation between pH U me and liquor wheel
and volume of milk of lime at those high pH values. A lime and
liquor wheel is used in many carbonatation refineries to control the
milk of time dosing. This is a mechanical device which can be set to
deliver the required volume of milk of lime. The quality ofthe milk of
lime must be constant.

Traditionally the quantification of the amount of lime needed for 0.6%C&0 on Brit
carbonatation is quoted in terms of CaO on melt Brix. Thus a value
o f say 0.6%CaO on melt Brix may be given; this means that 0.5kg of
CaO have been added per 100 kilogram of Brix in the melt. The CaO
has obviously been added in the form of lime, that is Ca(OH)2 .
Stoichiometry shows that 5fig of CaO are equivalent to 74g of
Ca(OH)2; thus a factor of 1.321 converts the mass of CaO to that of
Ca(OH)2. This way of quantifying the amount of calcium hydroxide
is not very clear but it is unfortunately common in carbonatation
literature.

The general operating conditions at liming should be a temperature operating conditions

of 75 to 80'C, a final pH of 10.5 to 11, and a retention time of about
5 minutes.
3.2.4 Saturators

The addition of carbon dioxide to the limed melt is done in large

reactors called saturators. The capacity of the saturators should be Capacity

such that a total retention time of about one hour is provided. Liquid
levels in the saturators should allow adequate contact time between
the gas and the liquor. In South Africa first and second saturators
have an installed capacity of about 1 m' per ton of refined sugar per
hour (RSO); third vessels have a capacity of about 0.4m' per RSO.

Since large volumes of gas are fed to saturators, the temperature will
Temperature
decrease and heating is required to keep temperature at the set (80 to
85° C) levels. Many saturators, particularly second and third vessels,
have calandrias to which vapour I can be fed.

Large quantities of precipitate are produced in saturators; the design

should therefore be as simple as possible, to prevent blockages by the
precipitate.

A vent is present at the top ofthe vessel to allow the unreacted gases £atrainment
to escape. The system must be designed to allow gas to escape
without the entrainment of liquor. This can be checked visually; there
should be no evidence of liquid and/or deposits on the external
surfaces of the vent pipe. Entrainment can also cause a fine spray
downwind of the vent. Entrainment will obviously cause severe
sucrose losses. In some countries health regulations do not allow the
discharge ofthe unreacted gases directly to atmosphere and scrubbers
are needed. This is not the case in Southern Africa.

An important section of the saturator is the gas distribution system. Gas distributor
Uniform and intimate contact is required, but the distribution system
must not get blocked by the precipitate. These two objectives are
usually in conflict, and compromises are needed. This will be
discussed later in more detail.

Finally, the saturators may need to be cleaned. Having three Cleaning

saturators now becomes advantageous in terms of throughput.

Chapman (1967) notes that it may be necessary to clean distributors
with acid, a few times a year. In South Africa saturators are cleaned
with high pressure, hot water hoses, a few times a year, but acid
cleans are not done.

- 1 7-
3.2.5 Filtration

Filtration is very much part of carbonatation and may have an

overriding impact on the overall process, both in terms of costs and
of performance. Refined sugar quality is affected by the filtration
process, large quantities of low Brix materials are generated during
filtration, the process is labour intensive, and the calcium carbonate
cake needs to be disposed of.
liquor
Two filtration stages are required. The first produces a clear filtered
liquor, often called brown liquor in carbonatation refineries, and a
sludge which must be desweetened. This desweetening is done by the
second filtration stage, which now produces a calcium carbonate cake
and sweetwater.

In South Africa filter aid is not used during the first or second Filter elolb
filtration stages, but filter cloth is used.

Filtration will be covered in detail later.

3.3 Material balances

Apart from showing the process itself, material balances are valuable Value of material balances
in many respects. They give good indications of throughputs, brix
loadings, decolourisations and other performances, and the
assumptions that are required are themselves instructive, often
highlighting areas for research. Two cases are considered here, the
first dealing with an affination station, while the second represents the
carbonatation process, with VHP as input.

3.3.1 Affination station material balance

Low purity, high colour raw sugars must be afnated if the refinery
is to produce refined sugar of the required quality. The basic reason
behind this observation is the fact that the relationship between the
amount of chemical used in most refining processes and the
purification obtained is not linear. Decolourisation during
carbonatation is a typical example; as more lime is used and more
carbon dioxide is added to reach the desired final pH, less and less
colour is removed, as shown in the following figure.
 Removal of colooras a runction or
chemical added

It is clearly evident that it is impossible to remove all the colour by

adding more lime and carbon dioxide. Even if this could be the case,
financial considerations would come into play, and it would probably
be beneficial to affinate.

The affnation material balance is shown below.

Material balance in an afoation

station

All to nnages are on a per hour

basis

To Ran")-

From RCReu}

_ 1 9-
The process must be started with water as magmaing medium, until Operation
sufficient tonnages ofmaterials have been made to produce jet 4, and
thus the affnation syrup. A quantity of the affnnation syrup is then
bled to the recovery house, depending usually on colour levels.

For a refinery handling about 47 tons per hour of input affinated raw
Dissdraotagrs
sugar, we note that about 88 tons of magma need to be cured per
hour. This is not a negligible centrifuging task. Furthermore, about 12
tons per hour of affination syrup need to be handled in the recovery
house; this is probably the most disadvantageous aspect ofaffination.

3.3.2 Carbonatation station

A material balance for a carbonatation station using VHP as raw

sugar feed is given. The values used are based on typical South
African conditions.

R {w SUG ATc Carbonatation material ba3mnec

TONS 54.0
POL 7i Sv 3
COL 1300

tINSTEIN.:=
MF,7_7PR TONS 14 2
TONS POI
BRLC x sr All too nagea are on a per hour
bwu
n(Lr

Tnws 613
COL 1365

LA1E nnUx C.o ss mill 1.1i,is l

I.IMT71'A7F7.T

TONS $71

sArTrRwTOFs
TONS 0.42

TONS 85.3
TONS 3.7 $m% 62!
COL e8.

SLIm[a
BLit t$ To

Yo

-20-
The following points apply to the carbonatation material balance :- Notes on the materiel balance flow
sheet

0 A 5% colour increase over the melter.

0Lime is added as mills of lime (15 Beaume), at the rate of Lime

1 kg CaO per 100 kg Brix in melt.

0 Flue gas, that is gas from the boiler stack, is used as a

source of carbon dioxide. In South Africa, with bagasse boilers, the
content of carbon dioxide ranges from 8 to 12% (vlv). Gases from Co,

boilers using fossil fuels need to be scrubbed; lime kilns are also a
source of carbon dioxide. The production and utilisation of carbon
dioxide will be discussed later.

0 The cloudy filtrate from the first filtration stage is sent back
Cloudy filtrate
to the limed melt. This is a common practice in carbonatation, and is
considered to improve the nucleation of the CaCG 3 precipitate. This
practice can obviously result in an increase in the capacity required
for the saturators.

0 The change in colour from the raw sugar to the filtered Iletolourisation
carbonated liquor is from 1300 to 682, a 48% reduction. From melt
to the same liquor it is 5001o, a typical value.
3.4 Lime

The quality of the lime used for the carbonatation process has an Lime quality impacts on filtration
i mpact on the filtration of the calcium carbonate. Bennett (1998)
reviewed the available results and showed that different types of
limes, under identical experimental conditions, yielded precipitates
which filtered very differently. Calcium hydroxide made in situ from
the reaction of CaC1 z and KOH, produced precipitates of calcium
carbonate which filtered significantly better than the precipitates from
any of the other types of lime. Bennett noted that although the
reactions between lime and sucrose, and between lime and carbon
dioxide, have been known for many years, there are many aspects
of practical importance which are still unknown.

Based on experiments with the types of lime available in the United

Kingdom, lime activity was enhanced when slaking was done at the Ageing of milk of lime
highest possible temperature. Ageing the milk of line was also
required.

Experience in South Africa has shown that the decolourisation

Operation of kiln
obtained across carbonatation can be reduced considerably when the
lime quality deteriorates. Qverbuming in a lime kilns was clearly
linked to the above problem.

Finally, the possibility of using calcium saccharate, instead of mills of

li me, has been mentioned.

3.5 Carbon dioxide

Before the advent of flue gas carbonatation, the carbon dioxide

required for melt carbonatation was produced by burning limestone The use of Due gas

in kilns. This process is still used in some cane sugar refineries, but in
South Africa most carbonatation stations use flue gas. Lamusse
(1988) gives a thorough review of the use of flue gas for
carbonatation, and interested readers are referred to this publication
for more details.

The main advantages of using flue gas, compared to burning

li mestone in a kiln are the lower capital and running costs. On the
other hand additional scrubbing with a sodium carbonate solution is
needed if sulphur containing fuels are burnt, and the gas contains less
carbon dioxide (12% compared to 30%, v/v).

The composition of the gas and thus the degree of scrubbing Scrubbi.g
necessary, depend on the fuel burnt. Fossil fuels containing sulphur
will result in sulphur dioxide being present in the flue gas. This will
require scrubbing with water and then with a solution of sodium
carbonate, usually at a concentration of about 5% (mlv). The
concentration of sulphur dioxide in the gas will depend on the
particular fuel; in South Africa a refinery burning coal reported 400
to 500 mg of SO, per litre of flue gas; this was reduced to 0.5mg per
litre after scrubbing with water, and to less than 0.1 mg per litre after
the second scrubbing with sodium carbonate. At these levels of
sulphur dioxide, the consumption of sodium. carbonate was found to
be between 13 and 15g per ton of raw sugar melted. Elsewhere, the
amount of sodium carbonate needed was higher at about 50 to 75g
per ton of raw sugar melted, indicating higher levels of sulphur.

Flue gas from bagasse burning boilers, in South Africa, requires

With bagssse as fuel
scrubbing with water only. The quantity of water needed is roughly
1 m3 for each ton of raw sugar melted, which is roughly equivalent to
a gas : water ratio of about 100 to 150 : 1.

Obviously the flue gas is drawn off after any scrubber with which the
boiler may be equipped.

Lamusse recommends that water or sodium carbonate scrubbers not

be oversized. It is preferable to have two units in parallel rather than
a single large one. This allows efficient gas scrubbing at lower
throughputs.

The scrubber cleans the gas and also cools it, with a temperature of
Temperature
50 to 50 °C being generally recommended. Temperature impacts on
gas density; the lower the temperature, the higher the C0 2 supply at
a given flow rate. The cooling effect of the gas in the saturators must
however be compensated by heating, as described earlier.

Flue gas needs to be compressed, and compressors are generally Compresmrs

installed between the scrubbers and the saturators. They keep the
scrubbers under a slight vacuum. If the flue gas contains sulphur, the
sealing water of liquid ring compressors should be treated with
sodium carbonate and the pH kept at a value of S.

The quantity of gas needed for the carbonatation process depends on

-23-
three factors :- Amount of gas needed:-

0 the amount of lime added to the melt

0 the percentage of CO2 in the gas, and

e the absorption efficiency in the saturators.

Let us consider the following case :-

0 The refinery uses 1 % CaO on melt Brix (i.e. 1 kg CaO per operating conditions

100 kg Brix in melt)

• Flue gases contain 12% CO2 (vlv)

• The gas contains 8% water vapour (vlv)

• The efficiency of CO 2 absorption is 30%

• The temperature of the gas after the scrubbers is 50'C.

By stoichiometry calculation

Cao + C02 --1' CaCO3

56 44 100

For 100 tons of Brix in melt per hour, we need 1 ton of CaO per
hour. This corresponds to a mass of CO2 of

l a 44156 x 1000 = 786kg per hour

or

786 x 1000/44 = 17864 moles C0 2 per hour

At STP 1 mole of gas occupies 22.4 litres. Thus the volume of CO 2

at STP is 400m 3 per hour.

The flue gas required must now be calculated, considering its carbon
dioxide content, its water vapour content, its temperature, and the
carbon dioxide absorption efficiency. Then

-24-
 400 1 100 273 + 501
Vol of gas = 0.12 g (.
g 0.92 g 30 273

14289m3 per hour

or
Typical requirement of 143m' or
flue gas per hour per ton Brix i n
143m3 of flue gas, per hour, per ton of Brix in melt. melt

The efficiency with which the carbon dioxide is absorbed has been Efficiency of CO2 absorption
investigated. A number of factors impact on it:-

pH. As expected high pH values will cause the efficiency

0
to increase. The following figure shows relative trends.

Effect of pH on absorption
efficiency
 Gas flow rate. The slower the gas flow the better the
absorption, since there is more time for the reaction to take place.
Effect of gas flow rate
The following table gives industrial data.

Saturator m' gas per pH Gassing

minute efficiency (/o)

1 80 9.5 28

2 25 8.7 14

3 5 8.5 25

The high efficiency in saturator number three is due to the very low
gas flow rate. At high gas flows, more power is needed, foaming can
take place and liquid entrainment becomes a possibility. At low gas
flows however, liquor residence times increase; throughput and
equipment size are now affected.

0Temperature. Gassing efficiency at 80'C is much higher Effect of temperature

than at fi5 ° C. Although carbon dioxide is less soluble at higher
temperatures, the increase in absorption is due to the higher reaction
rates and to the lower viscosities; these two effects override the
solubility one. Industrially, saturator one operates at 75 to 80°C
while the final saturator operates at 83 to 85T. It should be noted
however, that high temperatures can affect the ash levels and the
destruction of the monosaccharides.

0 Concentration of C0 2 in the gas. Both laboratory and full Effect of the concentration of Col
scale tests show only slight improvements in gassing efficiencies as
the content of carbon dioxide increases in the gas. The advantages of
having high concentrations of carbon dioxide are the reduced energy
requirements, the smaller equipment sizes, and the reduced heat
losses.

0 Design of equipment. Equipment to distribute the gas into Gas distributors

the liquor will have an effect on gas absorption. The finer the gas is
dispersed into the liquor, the higher the absorption but the greater the
risk of clogging by the calcium carbonate precipitate. Various devices
including perforated plates, in-line mixers, gas distribution rings,
perforated pipes, etc, are used. In the beet industry a gas distributor

- 2 6-
called the Richter Tube has been reviewed recently (Waegeneers,
1997), although the design is about 100 years old. A rotating shaft is
Richter tubes
arranged inside the tube, driven from the outside, and it carries
scrapers located in the slots through which the gas escapes. The
scrapers clean the slots and keep them free of precipitate. The shaft
rotates to and fro continuously. The Richter tube has been claimed to
i mprove the absorption, to reduce maintenance and to result in
energy savings.
 UMPURITY REMOVAL

4.1 Introduction

As stated in section 3.1 one of the main objectives of carbonatation

in refining is to remove the impurities present in the liquor. Two
types of impurities, namely colour and turbidity, stand out as the most
i mportant, but the others cannot be neglected.

Colour bodies are the main species which must be removed during
Colour
refining; the removal of other impurities will often follow the trends
obtained with colour; the analytical methods for the determination of
colour are well established and are relatively rapid and easy; finally
experienced plant operators can gauge colour visually, which allows
them to take action rapidly, when required.

Turbidity is more difficult to measure by analysis, but can also be Turbidity

gauged visually by the operators. In refineries where the filtered

carbonated liquor is to be treated further by processes involving its
flow through materials such as ion exchange resins or activated
carbon, it should be free of turbidity since suspended matter will
accumulate in the interstitial spaces and block the flow of liquor. This
will slow down or even stop the process, and require backwashing
procedures. Turbidity, even at levels lower than those which would
cause the above mentioned problems, can affect refined sugar quality
seriously, as will be shown later.

The other impurities which need to be considered include ash, starch,

other impurities
gums, silica, salts of organic acids, sulphates, phosphates, proteins,
etc.

4.2 Laboratory work

Bennett {1974) has done much pioneering work; using a final liquor
pH of g, a temperature of 75 - C, a retention of 1 hour and a liquor at
65 Brix, he investigated the effect of varying lime dosages on the
removal of many impurities. His results have been used to produce
the following figure, which confirms the trend mentioned on page 19.

-28-
 0 0.5 1 1.5 2
CaO °Io Brix in melt

Most of the purification is achieved at a CaO % Brix in melt value of Removal of impurities as cKOHt~
a are added to melt
about 0.61/o. Turbidity removal is nearly complete, proteins are a CO2
removed in excess of 80% while colour and gums show a 65%
removal. The levels of removal reached under industrial conditions
would be somewhat lower than those obtained in this laboratory
work. Bennett also showed that fructose and glucose were destroyed,
between 75 and 80% being lost, due to the effect of high pH,
temperature and retention time.

The effect of carbonatation on the ash (that is the inorganic species)

Ash
content of the filtered carbonate liquor is complex. The application
of solubility and equilibrium data to the formation of the calcium
carbonate precipitate and to the residual calcium content ofthe liquor
is difficult, due to the high concentration of sucrose, to the presence
of many impurities, both inorganic and organic, and to the high
temperatures. Rather than look at the theoretical aspects, most
workers have preferred experimental work; this limits the
generalisation ofthe results. In South Africa melt from a refinery was
carbonated in the laboratory; samples were removed during the
process, centrifuged to remove the solid material, and the supernatant
analysed for pH (24"C) and conductivity ash. The results are shown
in the next figure, ft is evident that, for that particular sample,

-29-
conductivity ash could be reduced to about 0.2%, compared to a
value of 0.17% in the untreated melt.

7 7.5 a 8.5 9 9.5 10 10.5 11

Reaction pH

Murray and Runggas (1975) found similar trends; according to these

authors the addition of carbon dioxide should be stopped when a pH
of 8.7 has been reached, and the use of a second saturator should
allow the conductivity ash to reach a minimum value around 0.10%.

0.45
.. 0.4
s 0.35
m 0.3
0.25
U7 0.2
0.15
0
C 0.1
0.05
7 7.5 8 8.5 9 9.5 10
Reaction pH

-30-
Cox et al. {1990}have investigated ash gains over carbonatation and
their findings have been described earlier (pages 10 and 11); to
Ash gain due to lactic acid
reduce ash gains due to the formation of lactic acid the liming
temperature should be about 75 ° C and the retention time prior to the
addition of carbon dioxide should be as short as possible.

4.3 Organic acids

The impact of lactic acid during carbonatation has already been

discussed. There are a number of other organic acids that have an
impact during carbonatation; the relevance ofthese acids is that their Solubility of calcium salts of organic
calcium salts have varying solubilities in water and thus could keep acids

calcium in solution. As mentioned before, the solubilities under the

carbonatation conditions are the relevant ones but these are not well
known. The solubilities of some calcium salts of organic acids in
water are given below.

Calcium salt Solubility

(g/100g hot water)

oxalate 0.0414

citrate 0.1

acetate 30

lactate 8

Work done in South Africa has shown that oxalic, citric, aconitic and
Removal of organic acids
acetic acids are present in melt from VHP sugar. The traditional
carbonatation process removed between 60 and 90% of the oxalic,
citric and aconitic acids, but had a negligible effect on the acetic acid;
these removals could well be influenced by solubilities. We have seen
that lactic acid can be formed, and this complicates the situation.
There is obviously much work to be done here.

4.4 Impurity removal in full scale plants

Colour is the only impurity for which data are available from many
refineries, from different countries. Results published from refineries
in South Africa, Mauritius and the United Kingdom show that most

-3 1-
carbonatation stations achieve at least a 40% colour removal; a 50°/0
removal represents as good a result as can be expected.

4.5 Mechanism of impurity removal

Bennett in 1972 compared the "physicar' removal of selected Physical vs. chemical removal
impurities to that obtained by the usual carbonatation process. He
added inert calcium carbonate to a liquor, and filtered it, for the
physical process; the same liquor was carbonated traditionally, for the
"chemical" test. His results are given below.

Original Physical Chemical

Colour 2480 1270 630

Turbidity 312 3.7 1

Gums (mg/100g) 280 155 46

Starch (mg/100g) 78 51 12

Proteins (mg/100g) 18 11 3

SiO2 (mg/100g) 15 11 6

Ca2'+Mg2- (mg/1 00g) 12 11 9

5042' (Mg/100g) 8 8 2

Bennett noted that the chemical, that is conventional formation ofthe

calcium carbonate crystal in situ, produced a much higher removal of
all the impurities investigated. Yet, the inert calcium carbonate added
had about ten times the crystal surface area than the chemically
precipitated calcium carbonate.

Already in 1972 Bennett used two analytical methods, namely X-ray

XRD and XRF
diffraction (XRD), and X-ray fluorescence (XRF), to study the
composition and nature ofthe carbonatation precipitates. The results
showed that the crystalline pattern of the precipitated calcium
carbonate was distorted by the incorporation of the impurities. Thus Chemical incorporation of impurity
Inside the crystal
the impurities are chemically included/incorporated inside the
growing calcium carbonate crystal, and this results in an efficient
removal. Murray (1972), working with starch, gives results which
support Bennett's findings.

-32-
 5. FILTRATION

5.1 Introduction
Second main objective
The second main objective of carbonatation is to separate the calcium
carbonate precipitate, which contains the entrapped impurities, from
the Sugar liquor.

There are a number of secondary, but important objectives.

0 The filtered liquor must be free of suspended matter. Any

re maining suspended matter may cause blockages in downstream Suspended matter causes blockages
and affects sugar quality
processes such as decolourisation by ion exchange resins or by
activated carbon. Suspended matter, particularly colloids, may well
affect sugar quality.

0 Sucrose losses must be reduced as far as possible. The

quantity of low Brix sweetwater must be as low as possible, and Sucrose losses
temperatures must be kept high to avoid microbiological activity.
Losses of sucrose in the filter cake, physical losses for example
spillages and leaks, must be controlled through good operation,
housekeeping and maintenance.

0 The filtration process must be as efficient as possible in

Filtration rate
terms ofcycle time, to avoid being throughput limiting. The filtration
rates of the carbonated liquor are therefore important. Temperature,
which impacts on viscosity, the quality of the precipitated calcium
carbonate, filter operation, etc. are all relevant.

Carbonated liquor has traditionally been filtered in large mechanical

filters. Some common types of filters will now be discussed.

5.2 Types of filters

In the early 1900's bag filters and plate and frame filters were
common in refineries. The first mechanical filter used in the industry
was the Sweetland, in about 1915; it was later modified so that each
leafhad an individual outlet. The Vallez filter was introduced in 1946, Horizontal tank/ Vertlcal leaf

followed by the Auto-Filter. All the above filters, and the Rota and
Gaudfrin filters are of the horizontal tank, vertical leaf type.

-3 3-
In the late 1940's vertical tank vertical leaf types appeared. The Vertical tank/ Vertical tear
Pronto and the Industrial filters fall in this category. Finally there are
Vertical tank/ Horizontal plate
also vertical tank horizontal plates filters, such as the Sparkler and
the Fas-Flo.

Sketches representing horizontal tank 1 vertical leafand vertical tank

1 vertical leaf filters are given below.

LEAF FILTRATE SIGHT GLASS

y
 LEAF

The Candle filter may also be used in carbonatation refineries. It has Candle filter
some advantageous structural features, such as a deep conical bottom
section where the precipitate can settle.

MTaT
-a

rnn

V DRAM

-35-
Filters, such as the Vallez, Suchar and Auto filters, are rotary filters. Rotary filters
The circular, vertical leaves are mounted on a rotating hollow shaft
to which the filtrate is delivered. The leaves and shaft rotate slowly
as the liquor, which is under pressure, is filtered through. Rotation
causes the cake to build up more evenly, and sluicing is more
positive. But, should the cake bridge between leaves, the leaves may
warp or even break.

The following design and operational points are important :-

Practical design and operational
points
* The ratio ofvolumetric capacity and filtering area needs to
be within a set range. This impacts on operational efficiency.

0 A vent on the top ofthe filter allows air to leave. There can
be much air trapped in the carbonated liquor.

Carbonated liquor forms voluminous cakes. Thus, the

spacing between the leaves must be large enough to accommodate
this.

0 Leaves may be made of metallic wire screen; cloth, dacron,

monofilament polypropylene (high temperature limit: 88'C),
polyester, nylon and cotton may be used.

0 Vertical filters should be fed from the side, not the bottom,
to prevent non uniform distribution of the calcium carbonate and
even its settling on the bottom of the filter. Horizontal filters and
filters with rotating leaves are less affected by this problem.

0 The filter must be filled completely before filtration begins,

and it must be kept full of liquor at all times during the filtration
process.

0 Between each filtration cycle the cake on both sides of the

leaf must be dislodged and discharged from the filter. Sluicing with
hot water, under pressure, is used. The minimum amount of water
should be used; the leave must be free of precipitate and there must
be no calcium carbonate left in the filter. These requirements are not
easy to achieve.

- 36-
In most carbonatation refineries it is necessary to desweeten the cake PLATE and frame filters

obtained from the filtration ofthe carbonated liquor. In South Africa

this is done mainly with plate and frame filters. The first plate and
frame filter was patented in 1828 and this type of filter was used in
European refineries in 1834; it was introduced in beet sugar factories
in 1862. Schematic diagrams are given below.

CLOTH

FEED

-3 7-
The early designs of plate and frame filters were not automated or disadvantages
mechanised. Their main disadvantages include a high labour demand,
low capacities per unit filtering area, and the discontinuous mature of
their operation. Cloth is used as filtration medium. When the filtration
is completed, the press is opened manually and the plates and frames
moved apart one by one. The cake falls off and is conveyed away.

Finally, Nicholas and Smith (199 1) compare the financial aspects of

various types of filters for carbonated liquor. Design, costs and
operational details are given.

5.3 Operation

A typical carbonatation refinery, processing melt of about 65Brix, Installed capacity-.-

using mechanical filters for the carbonated liquor and plates and
Carb. Liquor: 12m' per tan of melt
frames for desweetning the sludge, would have an installed capacity per hour
of about 12m2 of rotary leaf filtering area for the first duty, and
sludge: S to 5m= per too of melt
between 5 and 6m2 of filtering area on the plate and frame, both areas per hour
being expressed per ton of melt per hour.

In South Africa the carbonated liquor is mot reheated after the last
Temperature
saturator. This vessel usually contains a calandria to raise the
temperature of the liquor to about $5'C. As mentioned earlier,
viscosity is reduced as the temperature rises, and this facilitates the
filtration process.

A typical filtration cycle would proceed as follows.

0 The carbonated liquor is fed to the filter. The filtered liquor Filtration cycle
is then monitored, all cloudy filtrate being Sent usually to the first
saturator. When the filtered liquor is clear, it is sent forward to
process.

After the normal filter operation period, say six hours, the
filter is stopped. Hot water is pumped through and the water/liquor
mix sent to the saturator. When the desweetning is judged to be dome,
the liquid and cake mix is mow sent to a holding tank.

0 The calve and water in the holding tank are sent to the plate
and frame filter. Filtration is carried out. Water is then pumped
Sweetwater
through and Brix monitored. When the Brix reaches a value ofabout
10, the process is stopped. The cake is discharged and disposed of.

-38-
All liquids from the plate and frame filters are sent to the sweetwater
tank.

The sweetening off process takes place when the filtration cycle is sweetening off

complete, that is when the maximum pressure has been reached or the
maximum volume of liquor treated. Then, the cake must be
sweetened off. Basically the sugar bearing liquid is displaced by hot
water.

The sluicing process is the removal of the cake from the carbonated Sluicing
liquor filter by washing down with hot water and steam. The sluicing Sludge
process produces the sludge which is fed to the plate and frame
filters. It is important to sluice the filters very carefully.

Sweetwater is the liquid produced by the plate and frame filters. It is

Sweetwater
of a relatively low brix (about 10), it usually contains high
concentrations of impurities, for example colour and ash. About 20
to 30 tons of Sweetwater are produced per 100 tons of refined sugar
per hour.

Finally, losses of sucrose through microbiological activity is a real

Microbiology
possibility during filtration, particularly where low Brix liquids are
handled. Keeping all streams at high temperatures is the obvious
solution. A process which may be forgotten is the washing of filter
cloths; again care must be taken to prevent microbiological
problems, mostly by using high temperatures.
 6. FILTRATION PERFORMANCE

6.1 Importance of the filtration performance

The calcium precipitate formed by the carbonatation process contains

all the removed impurities. It must obviously be separated from the
sugar liquor, and this has always been done by filtration, as discussed
in the previous section.

Large quantities of carbonated liquor are handled in refineries; for a

Large quantities to be handled
production of say 45 tons of refined sugar per hour, the mass of
carbonated liquor, at 64 Brix, is about 85 tons per hour, which
represents about 65rn3 of liquor per hour. In addition the filters
require about 10 tons of water per hour; about 10 tons of calcium
carbonate sludge are produced by the main filters, which feed the
plates and frame. In turn these produce about 1.5 tons of cake per
hour. Finally, the filtered liquor quality must be good; ifthis is not so,
then the liquor must be recycled.

The filtration performance can therefore impact on throughput. If it

is poor, the filter cycles are shortened and the filter downtime lmpact on throughput

increases, while the quantity of sweetwater increases. This can reach

a point where the refinery throughput needs to be reduced. Finally,
the filtration of carbonated liquors is usually difficult and prone to
problems. It tends to be labour intensive and costly.

It is therefore evident that a measure of filtration performance would

be useful, not only to drive the plant but also to assess problems and
help solve them.

6.2 Filtration performance indices

Filtration is a well known process unit operation and we will start

Classical approach :-
with a classical approach. A calcium carbonate layer is formed in the
filter, and this is the filtering medium, more calcium carbonate being
deposited and adding to the thickness of the cake, while the clear
liquor passes through. The flow of the liquor may be represented by Poiseuille's equation
Poiseuille's equation, in the form

dV P
...................(i~
AdO fu[cr( W l A)+rj

-4 0-
where V is the volume of filtrate in m3
A is the area of the filtering surface in m 2
9 is the time in s
P is the total pressure drop across the filter medium and cake
in Pa
}I, is the filtrate viscosity in Pas
W is the mass of dry cake solids corresponding to V in kg
a is the specific cake resistance in mkg'
r is the specific resistance of the filter medium in rtf'
and
W = [t)V, where w is the mass of dry cake solids per unit
volume of filtrate in kgm'.

This last material balance assumes that the cake is incompressible or

Assumption
is compacted uniformly throughout its thickness. Experience has
shown that under practical conditions, any deviation from this
assumption usually has a negligibly small impact.
Assumption
For constant pressure filtration, equation (1) can be integrated to give

0 1tacv ~ V pr
V/A 2P A P

or

9 1taro 0 V + pr ................(2) Linear form

V 2PA 2 AP

,rare
Slope
and a plot of ON versus V gives a straight line whose slope is equal 2PA2
to (}caw1VA2), with units sm -6

Thus, if the assumptions are valid and we get a straight line, we can
obtain the slope through linear regression techniques, and since V, 6) Specific cake resistance, a

and P are known, we can calculate cc, the specific cake resistance.
This is a fundamental measure of filtration performance which allows The lower a, the better the tlltration

comparisons to be made. We note that the lower the value of a; the

better the filtration performance.

-4 1-
We now look at an example of the determination of a, based on the Filtration data from Moodley (2000)
data of Moodley (2000). Filtration times and corresponding filtrate
volumes are given on the right, for the filtration of a South African Time [e] . ' Volume [11.'0
carbonated liquor. The required plot is shown below. 0 0

22 . 00004

54 . OOo06

86 . 00008

128 . 0001

1 79 00012

236 00014

303 00016

0 SE-GS 0.000+ 0.00015 0.0002 0.00025 380 .00018

Volume tm3f
458 . 0002

545 .00022

644 .00024
A correlation coefficient of 0.997, for 1 i pairs of observations, and
visual inspectionofthe plot show clearly that the required linear trend
is present.

Linear regression yields a value of 1.03x10 10 sm-6 for the slope. For
this test Moodley gives A=0.0035m 2, P=300000Pa, [i=0.005Pas and
[il=10.3kgrrf a.

It is easy now to calculate the specific cake resistance which is found a = 1.5210" micg-'

to be 1.5x1012 Mk-1.

This particular calcium carbonate precipitate thus has a specific cake

resistance of 1.5xl 0 1 2 mkg"', and it can be compared with precipitates
from other stations or with precipitates produced under different
operating conditions, etc. Since a is a fundamental property, we can
compare the values obtained with different precipitates, as long as the 1.6X1 0' < a < 1.5110 11
assumptions are valid. The literature shows that a usually ranges
from about 1.6x10 4 , for materials such as kieselghur which have low
resistances, to 1.5xl0' 4mkg""', for thixotropic gums which filter very
poorly. Lionnet (1984) found values of6xl0" to 4x10"mkg' for raw
and treated clarifier muds, from South African cane sugar factories.
As expected all these values are within the extremes given in the
literature.

- 4 2-
Although a is a fundamental concept, it has a number of practical
disadvantages. The experimental procedures to measure it are fairly Disadvantages of [L

complex; it requires the value of W, the concentration of solids per

unit volume of filtrate, which is not readily available; it is a large,
cumbersome number with strange units.
Ben nett's approach :-
Bennett (1967,1968) has proposed an approach in an attempt to
eliminate these disadvantages. He proceeds as follows.

He defines a quantity, F as

F= 1 .................(3) Definition of F
ate

Let us now look again at equation (2)

yaw , . + p r
V ................ (2)
V ^ 2PA x AP

it can be assumed that Rr1AP is negligible in term of magnitude, Assumption

because r, the specific resistance of the filter medium, is much smaller
than a. Then

- paco . V
V 2PA :1

and

where V is the volume of filtrate passing through an area A, in time

6.

-43-
Let Q be the mass (kg) of Brix in a given time, R the Brix % filtrate,
and p the filtrate density (kgri3 ). Then

Definition of Q

Let the mass (kg) of CaO corresponding to the total carbonated Definition of L
liquor for the same time be L. Then

_ 100L
• ... ... ......... (6)
56V

since ca is the mass of CaCO, per unit volume of filtrate and the
molar masses of CaO and CaCO3 are 56 and 100 respectively.

Going back to equation (4):

= B2PA 2
a .. .. -.......... (4)
V 2 0)

_ 02pA256V
from (6)
V 2 p100L

_ 02pA 2 56p,9
a
100Qp100L from

But
F = ................. (3)
a a)

_44_
and thus

_ 100Q#100L _ 1
F
r 0 2PA z 56pp w

and, using equations S and b it can be shown that

a
Q ft Z x constant F related to Q
0P(PflA)

and IF is directly proportional to Q, the mass of Brix handled by a

filter station in a given time. From equation 3, it is seen that F has m x fF Tie nnett's filterability index
as units, and thus IF has m as units.

VF is Bennett's filterability index. We note that the higher >~F the f

The higher F the better the
filtration performance
better the filtration performance.

We now need to find out how IF is determined experimentally. We Practical determination of PF

go back to equation (3):

F _ 1 ................. (3)
atv

From equation (2) we know that the slope of a plot of ON versus V

is

partj
slope = 2PA2

that is
2PA slope
a

-45-
By substituting in (3) it is easy to show that
Equation showing how IF is
obtained
F
iPA 2 slope .......

where IF is Bennett's filterability index (m)

ii is the filtrate viscosity (Pas)
P is the pressure drop (Pa)
A is the filtering area (rn x)
Slope is the slope of the plot of 61V versus V (sm-6).

Using Moodley's example again, where A = 0.0035in2, P = Using actual data to tale ulaie IF
300000Pa, [L = 0.005Pas, and the slope = 1.03x101° se, we
calculate the value of VrF

4-F =,r( 0.0051(2x300000x.0035 =x1.03x10 t°))

2.6x10-7m

Bennett's filterability index ranges from about 2x10 7 to 8x10 -7m.

Range far IF
Below about 2x10"'m, filtration difficulties and throughput problems
can occur in carbonatation stations. Murray (1972) reports values of
about 4x10- 'm for South African carbonated liquors.

Bennett has thus produced a filtration performance index which is

directly proportional to the Brix throughput of a carbonatation
refinery. It has the advantage of not requiring the concentration of
Advantages and disadvantages
solids in the liquor, and it has a simple unit. It does however still
involve the experimental determination of the slope required by
Poiseuille's equation.

Having done most of the experimental work, it seems worthwhile to

do one more analysis to determine the solids in the liquor, so as to
also obtain a.

-46-
6.3 Some trends with ix and IF
If the calcium carbonate cake produced by carbonatation consisted
of pure CaC03 and the crystalline form was independent of the Effect of impurities, in «e taco, an
a and on 4F
operating conditions, such as lime content, temperature, nucleation,
etc, and of the impurities present in the liquor then :-

0 a, the specific cake resistance, would be constant

r IF, Bennett's filterability index, would decrease as co, the
concentration of solids in the liquor, increases.

But the cake is not pure CaC0 3 ; it contains many impurities, bound
to it both chemically and mechanically. Experience also shows that Trends between a, IF and lime
added
the type, the size and the size distribution of the precipitated CaC0 3
are affected by the operating conditions and by the impurities. Many
workers have investigated these effects; Bennett (1967) shows the
trends between the specific calve resistance, his filterability index 4-F,
and the amount of lime added.

n Vs CRO in Melt

0.2 0.4 0.6 0.8 1 1.2 1.4 1.8

CIO %Brix in melt

IF Vs. CIO in melt

-4 7-
It is evident that the amount of lime added has a large impact on a Effect of quantity of lime and of
and on IF. Absolute values depend on the melt itself, the two type or Sugar

samples used by Bennett originated from raw sugars produced by

different countries, but the trends are similar. At low lime dosage the
impurity / CaCO3 ratio is high, the impact of the impurities is thus
large, and a is high. At high lime dosages a becomes independent of
the amount of lime added and the properties of CaCO3 dominate. A
useful result of these types of test is the determination of the amount Lower value of a or peak value of
IF versus amount of lime
of lime needed to reduce a to the lower levels where the CaCC3
dominates, or where the peak value of IF has been reached. These
two quantities are therefore meaningful.

Unfortunately many workers have not adopted one or the other ofthe
above methods. In an attempt to simplify the determination of Simplified experime ntI based on
filtration performance, they have compared the volume of filtrate, volume 1 time relationships

from the sample, obtained after a given filtration time, with the
volume obtained under the same conditions but using a "standard"
liquor. They then calculate a filterability index, expressed as a
percentage, from

volume filtrate from sample

Filterability {°/o) = x100 rt%a -volume from sample I
volume filtrate from standard volume from standard

This technique is based on work published by Nicholson and Horsley

in 1956.

It has however been well established in the previous section that

filtration performance is not linear in terms of the volume o£ filtrate
produced in a given time. Going back to equation (4) we note that a
is proportional to 1N'. Thus

a = K,N" .........................(7)

where K I is a constant. From Nicholson and Horsley, the filterability

Relationship between the N&H
FNH, is proportional to V. Thus 81 term biIity and cake specific
resistance, a

F K „= K 2V ...........................(8)

where Ki is a constant. From equations (7) and (8)

a = K~(Fr n)2

-4 8-
A similar argument holds if the time for a given volume of filtrate is
used. It is thus clear that the value chosen for the volume (or for the
time) will impact on the result obtained for F NH

It is unfortunate that many countries use the Nicholson and Horsley

approach; Mauritius, South Africa, the Philippines, Australia have all Serions limitations of the N&H
filterability index
used this basic approach but with some experimental variations
(different filtration times or volumes; different standard liquors, etc),
to calculate a °Io filterability index. The results may be comparable
locally, although this is doubtful in view ofthe above arguments, but
they are certainly not comparable internationally.

Donovan (1994) appears to be one of the few workers who

compared an N&H filterability index with the IF concept. He Comparison or F„a and Tf F on the
obtained a good linear relationship between his filterability index, same sugars

using affinated raw sugars, and IF measured on corresponding

refinery carbonated liquors. It should be noted that the two
determinations were done on basically the same sugars. His results
are shown-below.

8o

ae70-
m
r

e
LL 4Q

30 -
4 & 7 8 9
Square root of F (x10"7m)
6.4 Effects of the impurities on filtration performance

The specific cake resistance concept (a), Bennett's filtration

performance index (IF), and the various filterability indices based on impact of impurities on filtration

the Nicholson and Horsley method (F~ffl ) have all been used to
measure the effects of impurities on the performance at the filters.
This illustrates the importance of filtration, and the impact of
impurities, often even at low concentrations, on that operation.

Suspended solids have long been associated with poor filter suspended solids
performance. A filtration index (N&H) was measured on a number of
sugars affinated in the laboratory. The filtrates were then tested again
by the same procedure. The results in the table below show that there
was a large increase in the value of the index when the filtrates were
tested; the first filtration must have removed materials which impede
the filtration process. Nevertheless, the index with the filtrates did not
reach 140%, showing that other impurities also have an effect.

Effect or removing suspended solids

Filtration index ( % )
Affinated raw sugar Filtrate from first
test

56 82

68 91

64 87
The removal of suspended matter
49 91 i mproves the filtration index

50 79

54 90

37 76

36 74

40 81
39 77

In an attempt to investigate the problem further, an affinated sugar

-5 0-
solution was tested as is, and after treatments to remove suspended
matter. The untreated solution showed a filtration index of45%. The
subsamples were treated to remove suspended matter of size larger
than 40Vm, 20[Ln1, l 0[Lrn and 5jLm. These subsamples all showed Suspended matter of size > Slim do
not affect the filtration performance
filterability indices of 46%. It is therefore clear that suspended matter
of size larger than about 5pm are not the ones causing filtration
problems.

Murray (1972) selectively removed suspended matter according to

size. He measured IF on the resulting solutions. His results are in the
table, and show that the value of IF increased only when particles
smaller than about 5[Lm were removed, confirming the previous
findings.

Particles removed IF (x107m) 4'F Increased when particles < SWm

were removed
40Vm 3.9

a 20 ~L rn 4.0

3Vm 4.5

0.8[Lm 4.7

0.45 ~trn 5.4

0.2}tm 5.8

Finally, Lee and Donovan (1995) show clear trends between

increasing levels of suspended solids and reductions in the filterability
index, as shown in the figure.

00 --
Effect of suspended solids to sugar
Bo --- on the filterability of the
carbonated liquor
So

sa

200 400 600 Boo 1000 1200

Susp. sat. (mg per kg original sugar)

-5 1-
A second critical impurity as far as the filtration performance of starch
carbonated liquor is concerned, is starch. Starch presents special
problems in that there are many different types of starches; obviously
in cane sugar, one finds cane starch, but this particular type is not Different starcbes

available for tests. One must use potato starch, corn starch or soluble
starch. All these have different properties. Secondly, starch consists
Amylose and aaylopecrin
of two distinct components, amylose a straight chain compound, and
amylopectin, a more compact branched chain one. The properties and
effects of these two compounds will be different.

The carbonatation process removes up to 50% of the starch present

in the melt. The presence of starch in the calcium carbonate
precipitate does affect the filtration performance. Murray in 1972
Effect of starch on IF
investigated the carbonatation of South African liquors in the
laboratory, and added potato starch which had an amylose
amylopectin ratio similar to that of his raw sugar. It was clear that
IF decreased as the concentration of starch increased, as shown
below.

4.5E-07

... 4E-07

U- 3.5E-07
0

°0 3E-07

2.5E-07
a
S 2E-07

1.5E-07
0 100 200 300 400 5oo
Potato starch (mgfkg original sugar)

Different starches, and the different components of starch were Different starcbes

investigated by Whayman and Willersdorf (1976), Hidi and Different components of starch
McCowage(l 984), and by Ramsay and Watts (1974). The results are
given in the table and figure that follow.

-52-
 Type of starch :; Filter
` billty (• ] Effect of different types or slarch on
100mg Brlx) Filterability index

Control 53

Cane starch 47

wheat starch 49

Corn starch 47

Soluble starch 61

5E-07

4.5E-07
E
F 4E-07
starch ~~ antylopectin
3.5E-07

3E-n7 J
q

0 2.5E-07
(
amylose
2E-07 -4
0 100 200 300 400
mg per kg original sugar

There is no doubt that the different starches have different impacts,

and that amylose decreases the filtration performance more than Amylose hasthelargest Me t
on
amylopectin. It is also noted that starch, even at relatively low
concentrations (around 100mg per kg sugar), reduces the filtration
performance significantly. This is why refiners using carbonatation
are so concerned about this impurity; often there is a limit on the Practical impact of starch on
carbonatatlon refineries
starch content (usually 120mg per kg sugar) ofthe sugar that will be
accepted by a carbonatation refinery. Another possibility is to blend
the high starch sugar with other sugars with low starch
concentrations.

-5 3-
Murray et aL (1974) give some indications of possible mechanisms Starch and calcium carbonate
for the incorporation of starch in the calcium carbonate crystal. These crystals

workers show that amylose prevents the agglomeration of the CaC0 3

crystals formed by the reaction between lime and carbon dioxide.
Amylose affects the "close packing" of the precipitated particles, by
decreasing surface charges_ Murray shows that the amylose tends to
be found on the surface of the calcium carbonate crystals while the
amylopectin is found inside the crystals.

Other impurities have been investigated by workers such as Hidi and

McCowage (1984), and Yamane et al. (1965). The different species
will be discussed individually here.

0 Inorganic species such as KCI, K 2 SO4, NaN03 , NaCl, Soluble inorganic species

CaCl2 and FeCl2 had no measurable effects. Similarly, sodium lactate,

citrate and aconitate had no measurable effects.

0 Phosphates, as KH,P0 4, silicates as Na~Si0 3 and aluminium PO„ 530 2 and Al

as AIC13 , affected filterability markedly. This is shown below.

0 3s0 100 150 200

Cone. of Impurity (mgtkgBrix)

0 Gums and dextrans were also investigated. A particular Gums and dextrans
problem here is that these are not specific compounds. Gums consist
of all polysaccharides which are precipitated by the alcohol used in
the analysis, and many different dextrans exist, with molecular mass

-54-
being one of the factors that change. Results obtained with different
types of gums and of dextrans are shown below.

Effects of different gums on

Type of gums Concentration Filterability filtration performance

(mg per kj Brix) 0/9)

Control - 63

Locust bean 100 39

500 4

Karaju 500 21
Carrageenan 250 48

ex factory syrup 500 41

Type of dextran Concentration Filterability Effects of different dextrans on

filtration performance
(%)
(mg per kg Bri x)
Control - 63

Mol. mass 1x10 5 1000 63

Mol. mass 2x106 1000 63

Mol. mass 1x10' 1000 7

ex factory syrup 1000 10

ex raw sugar 1000 20

It is clear that suspended solids, starch, gums, dextrans and many

other impurities impact considerably on the filtration performance of
carbonated liquor. Within a given species, different types can have
different effects. Under practical conditions the influence of
impurities on filtration is thus highly complex and extremely difficult
to predict, but it is well established that the presence of species such
as suspended solids, starch and dextrans is very undesirable.

-5 5-
6.5 Effect of operations on filtration performance

Experience in carbonatation refineries and laboratory work have Effect of operations in the carb
shown that the operations in the carbonatation station impact on the station

filtration performance of the precipitated calcium carbonate. Murray

and Runggas (1975) in South Africa, Bennett (1972) and others
provide information, which is summarised here.

0 pH. Laboratory tests have shown that the highest

pH
filterability was reached at a final pH of 8.2_ It is not usually possible
to have only one saturator in refineries, and with two saturators the
maximum filterability was at a pH of 9_5 on the outlet of saturator
number 1. In the second saturator the pH is then adjusted to suit later
processes and for minimum ash content.

0 Temperature. Laboratory tests show 86 °C as the best

temperature for filterability. Temperature affects the viscosity of the Temperature

liquor and thus the efficiency of gas contacting; it impacts on the

reaction rate, and on the quality of the calcium carbonate precipitate.
Generally the degree of conglomeration of the precipitate increases
with temperature, up to about 82'C.

0 Brix. Brix affects the viscosity of the liquor. Lower Brix Brix

values are believed to result in better quality calcium carbonate

crystals. Like temperature Brix affects the mass transfer rates of
carbon dioxide and may thus affect the nucleation and crystallisation
rates of the calcium carbonate.

Ageing of milk of lime. Ageing of the milk of lime for Milk of lime
about two hours was found to increase the filterability. No further
increases were found when ageing time was in excess of two hours.
The possibility of using calcium saccharate rather than milk of lime
has been mentioned. This possibility is certainly worth investigating.

e Quantity of CaO. This is a critical parameter and it has CaO % Brix in melt
been well investigated. Generally there is an optimum level for
maximum filtration performance; in most cases 0.7 to 1 kg of CaO
per 100 kg of Brix in melt is the range used practically. The optimum
will be within that range and needs to be established by experience or
by laboratory tests.

0 Steady operational conditions. Experience in refineries Steady operation

shows that sudden changes in flow rates, temperature, Brix and pH

-56-
 invariably decrease the filterability ofthe precipitate. This is thought
to be due to changes in the particle size distribution of the
precipitated calcium carbonate.

0 Retention time. Two or three saturators are better than

one, and a continuous process is definitely vastly superior to a batch Retention In saturators

one. Retention is critical in the first saturator where most of the

precipitate is formed. Bennett states that retention in the first
saturator should not be less than 45 minutes. The second and third
vessels should then provide a total of about 30 minutes.

7. DISPOSAL OF CALCIUM CARBONATE CAKE

The calcium carbonate filter cake produced by the carbonatation

station consists of25 to 50 % water and about I% sucrose, depending
on the type of filter used. Large quantities are produced and must be Landfill

disposed of. Since the material is not harmful, it is often possible to

use it for landfill; transport and handling are the main costs.

The calcium carbonate cake can also be recalcined to provide lime Recalcisation
and carbon dioxide. The local conditions determine the feasibility of
this option.

in the beet industry the possibility of selling the cake as a calcium rich
fertiliser has been considered. Details are given in a recent publication
by Struijs et al. (1999).
 BIBLIOGRAPHY

Alexander JB (1971). The evolution of a new look South African Sugar. Proc Int Sac Sug Cane
Technol Assoc 14, 1619-1525.

Alexander JB (1981). VHP caws- some pertinent facts for producers and refiners. Sug Ind Tech, vol
40, 130-143.

Bennett MC (1967). Liquor carbonatation. Int Sug J 69, 101-104.

Bennett MC (1972). Physical chemistry of phosphotation and carbonatation (I and II). Int Sug J 76,
40-44; 68-73.

Bennett MC (1998). Curious phenomena in lime sucrate. Int Sug J 100, 266-271.

Bennett MC and Gardiner SD (1967). Liquor carbonatation. Int Sug J 69, 198-202.

Bennett MC and Gardiner SD (1968). Liquor carbonatation. Int Sug J 70, 136-175.

Chapman FM (1967). Sugar refining - notes on unit processes. Int Sug J 69, 231-136.

Cox MGS, Mohabir K and Bervoets A (1990). Ash gains due to lactic acid formation during
carbonatation. S Afr Sug Technol Assoc 64, 217-222.

Fong Long S (1992). Setting up ofa sugar refinery at Brittania sugar estate. Rev Agric et Suc de l'lle
Maurice. 71, 231-240.

Hidi P and McCowage RJ (1984). Quantification of the effects of different raw sugar impurities on
filtration rates in carbonatation refineries. Proc Sug Proc Res Inst, 186-208.

Honig P (1953). Principles of sugar technology. Vol 1. Elsevier, Amsterdam.

Kaga T, Suzuki K and Yamane T (1966). The filtrability of carbonatation slurries. Int Sug J, 68, 3-5.

Kelly FNC, Mak FK and Lao KC (1973). A comparison of carbonatation and sulphitation
decolourisation in raw sugar syrups. Int Sug J 75, 308-311.

Lamusse JP (1988). Flue gas carbonatation. S Afr Sug Technol Assoc 62, 61-65.

Lee EFT and Donovan M (1995). Filterability of raw sugars. Proc Int Soc Sug Cane Technol Assoc
22, 195-205.

Lionnet GRE (1984). Mud conditioning for good filter operation. S Afr Sug Technol Assoc 58, 39-
41.
Moodley M (2000). Laboratory optimisation of the carbonatation process with regard to colour
removal at Malelane. M Tech thesis. In press.

Murray JP (1972). Filtering quality of raw sugar: influence of starch and insoluble suspended matter.
S Afr Sug Technol Assoc 46, 116-132.

Murray JP, Runggas FM and Vanis M (1974). Filtering quality of raw sugar: mechanism of starch
influence in carbonatation. Proc Int Soc Sug Cane Technol Assoc 15, 1296-1306.

Murray JP and Runggas FM (1975). A study of factors influencing refinery carbonatation. S Afr Sug
Technol Assoc 49, 90-93.

Nicholas B and Smith R (1991). Automatic pressure filtration of carbonated mud at Pyrmont
Refinery. Int Sug 3 93, 9-15.

Nicholson RI and Horsley M (1956). The design and performance of a new test filter. Proc Int Sac
Sug Cane Technol Assoc 9,1271-287.

Ramsay AC and Watts RS (1974). The effect of starch components concentration upon filtration.
Proc Queensland Soc Sug Cane Technol Assoc, 41, 223-228.

Rault J(1960). The juice carbonatation process and repercussions of economics on technology. S Aft
Sug Technol Assoc 34.
Sargent D, Philip E and Cubero MTG (1998). Lime reduction in juice purification. Conf Sug Proc
Res, Savannah, March 1998.

Struijs J, Smook A and de Bruijn JM (1999). Valorization of carbonatation lime. Zuckerindustrie,124

(199), 770.

van Hengel A (1962). Better sugar by remelting. S Afr Sug J, 46, 587-595.

Waegeneers WR (1997). Impact of the upscaling of a carbonatation tank on the quality of the
epuration process. Com Int de Tech Sue, Marrakesch, June 1997.

Whayman E and Willersdorf AL (1976). Effect of starch on carbonatation. Int Sug J 78, 67-68; 99-
100.
Yamane T, Suzuki K and Kaga T (1965). Filtration impending materials in raw sugars of various
origins. Int Sug J, 67, 333-337.

Yamane T, Suzuki K and Kaga T (1966). The effect of insoluble matter in affined sugars on their
filtrability. Int Sug J, 68, 259-261.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation. The fundamentals
6 Evaporation. The practice
7 Pan boiling I
8 Pan boiling 11
9 Diffusion
10 Refinery Carbonatation

In preparation:-

Millin g
Boilers
Sulphitation (refining)
Phosphatation (refining)
MILLING
Sugar Technology For Students

MILLING

Prepared by MJReid

Study Text 11

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 2040

Copyright C 2000 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-27059-4

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 CONTENTS

Page

1, Process of milling
1.1. Introduction 1
1.2. Milling and dewatering after a diffuser 1
1.3. Description of plant 2
2, Cane handling
2.1. Off loading 2
2.2. Cane conveyors 3
2.3. Conveyor controls 4
3. Cane Preparation 6
3.1. Introduction 6
3.2. Description of plant 6
3.3, Measurement of PI
3.4, Factors affecting PI
3.5. Design of shredders 14
4. Process of extraction 11
4.1. Effect of imbibition 11
4.2. Juice screening 13
5. The mill balance 16
6. Juice extraction calculations 17
7, Feeding cane into the mill 20
8. Pressure in mills and mill hydraulics 22
9. Mill roll lift 24
10. Bearings 24
11. Mill rolls 25
11.1. Shaft and shell design 25
11.2. Roll grooving 26
12. Mill drives 27
12.1. Comparison of different drives 27
13. Gearing 29
13.1. Specifications 29
13.2. Lubrication 29
13.3. Loading and overloading 29
14. Construction of the mill 30
14.1. Trashplate 30
14.2. Scrapers 31
14.3. Mill housing 31
14,4. Pinions 31
14.5. Cooling 32
14.6. Roll adjustments 32
14.7. Juice drainage 32
15. Pumping and circulation 32
16. Mill performance 33
16.1. Performance Measurement 33
17. Mill settings 35
18. Capacity of a mill 39
19. Power consumption 40
20. The performance of mills 41
20.1. Fibre in cane 41
20.2. Length of the tandem 41
20.3. State of cleanliness 42
20.4. Load application of the mills 42
20.5. Mill roller speed 42
20.6. Uniform feeding 42
20.7. Imbibition rate and application 43
20.8, Cane preparation 43
20.9. Mill settings 43
20.10. Roll surface condition 43
20.11. Drainage 44
20.12. Proper operation of the mills 44
20.13. Efficiency indicators 45
21. Control and Instrumentation 46

Bibliography 48

LIST OF FIGURES

Figure 1: Diagram of a typical modem 4-roller mill

Figure 2: Diagram of the arrangement and controls of conveyors in atypical mill
Figure 3: Diagrammatic arrangement of cane preparation equipment.
Figure 4: Diagram of a shredder
Figure 5: Graph of extraction vs imbibition
Figure 6: Diagram of milling tandem illustrating multiple compound imbibition
Figure 7: Diagram of milling tandem illustrating multiple simple imbibition
Figure S: Sketch of DSM screen
Figure 9: Diagram of a mill mass balance
Figure 10: Mill juice balance diagram
Figure II: Plot of brix % bagasse leaving each mill
Figure 12: Diagram of a pressure-fed mill
Figure 13: Diagram of a typical mill hydraulic circuit
Figure 14: Diagram of mill rolls showing settings
Figure 15: Measurement of roll opening
Figure 16: Sketch of trash plate setting method

LIST OF TABLES

Table I Extraction calculation spreadsheet

Table 2. Fibre densities
1. PROCESS OF MILLING
1.1. Introduction

The principle objective of milling is to extract as much of the juice out of the
shredded cane as possible. This is done by firstly preparing the cane by
knifing and shredding, and then with a combination of squeezing by the
heavy rolls and washing or maceration using water, called imbibition water.

Historically, sugar cane milling started with two- or three-roll vertical hand HlstarkW
or animal driven machines with wooden rolls. When three rolls were used, a
man had to catch the cane and turn it into the second nip. Development led to
horizontal cast iron rolls placed in a triangular configuration with a fixed
turner plate or trash plate mounted on a so-called dumb turner. Figure 1 is a
diagram illustrating the arrangement of the rolls and trash plate.
Developments over the years were improvements to cane preparation,
addition of more mills to the tandem (up to 7'), imbibition, feeding devices,
steam and electric mill drives, heavy gearing, roIl roughening, drainage, and
new materials. But the basic mill is still very much as it was 154 years ago.

TRASH PLATE
AND DLMB
TURNER

FSgure 1. Diagram of a tyuical modern 4-roller mill

1.2. Milling and dewatering after a diffuser

The bagasse from a diffuser which is sometimes called "megasse" has

Diffeser
different characteristics compared to that from the previous mills of a dewraterdn= ea1Ra
tandem. Diffuser megasse is sorer, slimier, and hotter (65 - 80°C} than the
bagasse from a mill. These differences were originally blamed for an
apparently more difficult dewatering task for the diffuser. However, in
 recent years especially in South Africa the dewatering performance has been
shown to depend more on other factors than on these differences caused by
the diffuser, and the bagasse moisture from diffuser dewatering mills is now
as good as that from a milling tandem.

1.3. Description of the plant

Brierdescdptlon Cane arrives at the mill, where its mass is determined on a weigh-bridge.
of the p The cane is off loaded either direct onto the mill feed conveyor or into a
storage area. The conveyor passes the cane under rotating knives where it is
cut into smaller pieces, mainly to assist in feeding a shredder, which redut
the cane to a pulp by tearing up the fibre and breaking open most of the plant
cells which contain the sugar dissolved in water,

The shredded cane is then conveyed by a steep slat carrier and fed into a
vertical chute which acts as a short-time buffer, and ensures an even feed to
the first mill.

The cane is then squeezed in each of six or seven mills, and through a
process of squeezing and imbibition, described later, most of the sugar
solution, called juice, is removed from the cane. The residue after the final
mill is called bagasse, and is used as a fuel for producing steam, which in
turn is used for driving turbines and as heating steam in the recovery process.

2. CANE HANDLING
2.1. Off-loading

Rz"esdng =d
The method of off loading cane depends on the harvesting and transport used
oftloadrng at a particular mill. In Southern Africa the most common harvesting method
is burning, followed by hand cutting and machine loading into "Hilo"
trailers, one or two of which are towed by a horse or tractor. (These trailers
are so named after the city in Hawaii where they were first used.) The
transport carries relatively clean whole stalks in vehicles that have a `bet" of
chains attached on one side of the trailer and suspended from a loose beam
on the other. At the mill, the trailer is positioned between a spiller crane and
a wide raised table provided with a slat conveyor over its whole width and
length. The spiller crane hooks onto the trailer loose beam, and lifts it up to
20m on a guided carriage, which spills the cane over the side of the table and
onto the slat conveyor.

An alternative method which is being used less is for the cane to be picked
Bundle cane up in the field by a simple winched chain sling (Bell system) that pulls and
bundles the cane onto a small trailer. The chain sling has a quick-release
latch and maintains the cane in a bundle of up to 6 tons. These bundles are
either carried direct to the mill by tractor-trailer, or transhipped at loading
zones into larger vehicles for transport to the mill. At the mill they are stored
under gantry cranes in the cane yard, and can be conveniently used as buffer
stock. However this method is recognised as being very expensive, and it is
being replaced by the Hilo system wherever possible.

Chopper-harvested cane is also on the increase in Southern Africa. Here the

Chopper-
unloading method is usually an adaptation of the spiller system, in which the lwveAed acne
closed container with the chopped cane is lifted by the spiller crane about a
pivot at the top of the trailer on the side nearest the table, hence spilling the
cane onto the table.

2.2. Cane conveyors

The conveyors in a mill usually comprise one or more feeder tables,

receiving spiller cane or bundled cane from the gantry, feeding onto a main
cane carrier that feeds the knives, and a cane elevator to feed the shredder.
The shredder discharges into a slat conveyor that lifts the cane to the
relatively great height to feed into the first mill feed chute.

Feeder Table A feeder table is usually wider than the length of the longest
trailer expected at the mill. Most modern tables are about 14m wide, and are
provided with up to 12 chains running in pairs with slats in between to
Feeder table
convey either whole stick or chopper cane satisfactorily. The head shaft &94M tips
design is important, because it usually has three bearings and requires careful
alignment, Some tables are provided with split head shafts driven by two
motors. The chains are usually of the roller-less type, between 150 and
200mm pitch.

Because the cane tends to form bundles that would cause chokes in the main K3cirer on feeder
cane carrier, the table is usually provided with a "kicker" above the head table
shaft. This kicker comprises a shaft with curved tines about 500mm long,
and rotates against the cane direction to throw bundled cane back onto the
table.

The length of the table depends on the amount of buffer storage required, and
t or the
on the height to which the cane must be raised to feed the main cane carrier. table
This usually works out to a length somewhat greater than the width of the
table.

Main Cane Carrier C The MCC has traditionally been constructed as

Chaiu conveyor
a deep apron carrier with a steel slat deck running on a 152mm pitch roller
chain. This design has been robust enough to withstand the shock loads
caused by cane falling from a fair height from the feeder tables, and also to
act as the lower anvil on which the cane knives cut the carte.

However, in a mill of fairly modern design, the cane unloading is further

away from the cane preparation area than was traditionally the case, and this
means that the main cane carrier is quite long. This would be expensive if
the traditional construction was used. The tendency today is therefore to use
Sect conveyor
heavy duty belt conveyors, and arrange them to feed onto short apron carriers
 which feed under the cane knives. Belt conveyors need to be carefully
designed to ensure that spillage is kept to a minimum, by providing adequate
skirting, belt cleaning scrapers and non-clogging idlers. The areas of heavy
shock loading at the feeder tables should have close pitch idlers of a special
type to absorb the shock. The head and tail pulleys should also be of the type
that do not build up with dirt, as the sticky nature of the dirt in a cane yard
can cause problems on pulleys and idlers.

Shredder feed
Shredder feed conveyor It is also usual today to convey the cane from the
Cooreyor knives to the shredder on a belt conveyor. The design of this belt must also
follow the precautions of that for the MCC. This belt is usually at a fairly
steep angle, because of the need to lift the cane to the top of the shredder feed
chute. It has been found that this steep angle could cause the cane to slip,
and some mills use a rough top belt to avoid this.
chlbandsmvp
Cane Elevator The final conveyor from the shredder to the first mill feed
chute usually has to raise the cane through several metres and is thus
constructed at a steep angle. It is usual in most mills for this conveyor to be
of the chain and slat type, similar to the inter-carriers between the mills.

Des': ar m t rs In designing these conveyors, it is usual to adopt a

standard width of 2,Im. This is determined by the widest belt available from
Conveyor dexip
the rubber companies, and is also the most common width of the rolls of
most mills built after the 1960's. Carriers of this width will be adequate for
cane crushing rates of up 404 tons cane per hour. The speeds are determined
by volumetric calculations, on the assumption that cane density is as follows:

Loosely packed whole stick cane: 150-200 kg/m'

Cane after knives, or chopper harvested cane: 234-280 kg/m'
Shredded cane: 400 kg/m'

Standard power calculations for conveyors usually provide motor sixes that
Power for are too small for sugar mill use. It is usual in the sugar industry to apply a
Conveyors
factor of 1,2 to 1,5 to the final calculated size, and then to choose the
standard motor greater than the calculated size. In addition, if the drive is an
AC variable motor, one standard size larger still should be chosen, to allow
for adequate cooling while running at slow speeds.

2.3. Conveyor controls

Figure 2 shows a diagram of a typical arrangement of conveyors and their

controls.

As will be shown below, it is essential that the rate at which cane is fed to the
Controls and first mill be maintained as steady as possible. To achieve this the cane
interlocks
carriers are provided with speed controls and interlocks that are arranged to
minimise chokes and ensure an even feed.
 Conveyor spwd and
interiodc oxfots

an ement and controls of conveyors

Figure 2. Diagram of the trnical an,~

The first mill speed is set constant to a rate that determines the tonnage to be
crushed by the tandem. The level of cane in the first mill feed chute is
measured usually by means of a vertical row of six to ten conductivity Urel
monitors. This controls the speed of the final carrier from the shredder in traaamftters
such a way that the level in the chute is maintained at about 75 to 80°/0.
Some alternative level transmitters have been tried, with varying success, but
the conductivity type is considered to be the best.

The speed of the shredder feed carrier is controlled at a constant ratio to the Carrier speed
speed of the final carrier. The load on the shredder is monitored, and if it control

increases above a threshold which warns of an impending choke, the feed

carrier slows down for a long enough period to avoid the choke.

The speed of the MCC, in a similar way, is kept at a constant ratio with the
shredder feed carrier, and is also made sensitive to load swings on the cane
knives.

The feeder tables are usually driven manually, the operators using them to
keep the MCC filled with cane.

In addition to the controls, the conveyor motors are connected to an

Carrier
interlocking control, in which they can be started automatically in sequence, interlocks
from the last to the first. Also, if any one conveyor stops for any reason, all
the conveyors upstream will be stopped.

Gradener (1973) published a very good paper on thyristor-controlled carrier

Carrier drive
drives in which the primary level measurement was a Hall generator on the
typ«
first mill chute. This device measures the deflection of the large flexible
front plate of the chute, which was assumed to be proportional to the amount
of cane in the chute. Coates (1994) published a review paper of cane
conveying systems in which types and control strategies were covered.

The drives for the conveyors which are required to vary in speed are one of
the following types:

Hydraulic motor, coupled to a variable speed hydraulic pump

 • Variable speed coupling (eg Heenan and Froude)
• DC electric motor with thyristor control
• AC variable frequency control

The last type is likely to be the drive of the future, because it has all the
features of variable speed, good torque characteristic, and ease of control.

3. CANE PREPARATION

3.1. Introduction

In following sections of this guide much will be said about cane

preparation as one of the most important factors that affect the
performance of a milling tandem. In this section the process will be
described and the equipment evaluated.

The objective of
The objective of cane preparation is to rupture all the plant cells in the
Cane cane. This cannot be achieved perfectly, and by measuring the
preparation
"Preparation Index" (PI), it can. b e seen that most mills achieve between
90 and 93% rupture of the cells.

For good milling (and diffusion) it is better not to break up all the fibre
Lan=erofover- into very small bits, because the resulting material would not feed or drain
prepa-Rtion well and juice percolation would be seriously impaired. It could best be
described as "porridge" or "mush", and this is to be avoided. The
laboratory procedure of "digesting" is a good example of almost 100% PI,
but the cane in this condition would be impossible to mill,

The cane stalk consists of a core of pith held in a fibrous matrix,

Cane containing most of the plant cells and hence the juice, surrounded by the
components
rind which is mainly fibre. Accompanying the cane are other materials
such as cane tops, leaves, wax, sand and silt, all of which contribute to the
mushiness of the final prepared product. Good preparation then must try
to keep as much as possible of the fibre intact while rupturing most of the
plant cells.

3.2. Description of the plant

The best way to prepare cane for milling is to pass it through cane knives,
which reduce the mean length to about 300400mm, and then to hammer-
mill it in a custom built puiveriser called a shredder.

In order for the cane to be properly presented to the knives, the main cane
Leveller carrier is normally provided with a leveller, which consists of a light knife
shaft arranged to run about I m above the carrier, and to cut against the
direction of the cane. This serves to throw bundles of cane backwards, and
provide a level bed of cane into the knives.
Typical cane knives consist of rotating shafts fitted with replaceable knife
blades, about 2m wide and 1,5m swept diameter. The rotor is mounted so
that it cuts onto the carrier or a drum with a clearance of about 600mm for
first knives and 50mm for second knives. The cane is passed through this
clearance and the degree of cutting depends on the number of knives, the
clearance and on the power available. Power input varies typically from
200 to 1000 kW, with an exception being that of a turbine driven knife of
1370 kW, and the speed from 250 to 960 rpm. Cane knives were
reviewed in a paper by Reid (1994).

The shredder beats the cane with heavy (up to 25kg) hammers and throws
it against a fixed curved plate containing several anvil bars which serve to Shredder
throw the cane back into the path of the rotating hammers. The shredder
rotor is also about 2m wide, with a swept diameter of up to 2m, and
usually driven at 1000 rpm by a 3000 kW motor or steam turbine. A
modern shredder will have 160 to 200 hammers, all provided with a wear
resistant welded-on layer which lasts for at least one week, but often more
than two weeks.

The anvil bars, or grid bars as they are often called, are attached to a heavy
fabrication that forms part of the casing usually known as the washboard,
and spans an angle between 90° and 120° of the circumference. The
washboard is hinged at its leading edge and is mounted in such a way that
the clearance between the hammers and the anvil bars can be adjusted at
the leading and trailing points. The power absorbed and the shredding
performance are increased as these settings are reduced. The trailing edge
of the washboard should have a safety device that allows it to swing open
should a large rock or piece of tramp iron be fed in with the cane. This can
be achieved by means of shear pins, hydraulic rams, or spring-loaded
toggle supports.

It is good practise to have a spare washboard available for each shredder,

and to be able to change the washboard quickly. The spare is then kept
 ready with a new set of anvil bars and suitably refurbished. It should be
noted that the plate that guides the cane onto the first anvil bar must not
allow any protrusion of the anvil bar or its attachment into the path of the
cane. This could cause bridging of the feed cane with subsequent choking.
Shredders were reviewed by Moor (1994).

WLVDAGE Cllr PLATE

GRID BARS

CANE EXIT

Fizure 4. Sectional view of a shredder

The changing of worn cane knives and shredder hammers is one of the two
Hammer wear
reasons that a mill cannot crush continuously. (The other is the need to
remove scale from the evaporators). Much effort has gone into research
aimed at extending the life of these knives and hammers, (Moult, 1980)
but in the Southern African environment, it seems that two weeks life is
the reasonable limit. Typically each mill has two sets of knives and
hammers, one of which is being refurbished while the other is running.
The wearing surfaces are faced with a welding technique using either
welding wire or rods chosen for their very high wear resistance. Various
proprietary materials are available, most of which have been found to
perform well. The choice becomes a matter for each engineer to decide on
the basis of economics.

Effort should be put into reducing the quantity of soil coming in with the
cane. In certain countries (e.g. Australia) where the soil in cane less than
half that in South Africa, the wear of hammers is less by a ratio of up to 10
to 1. (Wienese & Reid, 1997).
 3.3. Measurement of preparation index

It is useful for the engineer to have a measurement of the amount of

preparation that the cane has been subjected to, and for this purpose,
various methods have been tried and applied in different countries. In
South Africa, the method currently adopted by the Industry is Preparation
Index (PI), as described in the SASTA Laboratory Manual (1985). This is
an empirical measurement, based on the ratio of the brix of juice extracted
from a sample in a limited time to the total brix in the cane juice.

The technique, briefly, consists of dividing the sample of prepared cane MetLad of PI
into two portions, A of 5409, and B of 3338. A is mixed with 30009 of mmsarement
water, placed in a plastic bottle, and tumbled in a special rotating frame
apparatus for 30 minutes. The brix of the liquid is measured using a
precision refractometer and called Br(a). Sample B is placed in the bowl
of a cold disintegrator to which is added 20449 of water and the sample is
stirred for 20 minutes. The brix of the extract is measured and called
Br(b). The PI is calculated by using the following formula:

PI = Br(a)Br(b)* 100

For a modern, well-designed and maintained plant the PI should be at least

92%.

The Sugar Milling Research Institute (South Africa) is developing a new

instrument that should simplify and speed up the measurement of PI and
give readings which are more repeatable and reliable. This apparatus is
described in a paper by Reid and Hastie (1994).

3.4. Factors affecting PI

The following factors are likely to influence the PI of a particular cane

preparation plant:

Wear on hammers and knives

Wear on anvil bars
Uniform feeding of the knives and shredder
Setting of the gap between the hammers and the anvil bars
Fibre content of the cane
Numbers of knives and hammers fitted to the rotor

To ensure that these factors are always given attention, the engineer should
Monkorhg of
monitor the PI continuously. It is also possible for an experienced PI
engineer to immediately recognise any variation in the performance by
visually inspecting the shredded cane leaving the shredder. The sound of
the shredder is also a good indication of how it is performing.
 Uniform feeding and choking are closely related. When the hammers or
chol er of cane
p-P-dion knives are worn, there is a tendency to choke. It is essential that the
egmdpment engineer is familiar with all the causes of chokes in his plant. In the cane
preparation area, choking can be caused by even small projections on the
casings into the path of the cane. Chutes that converge, rough unpolished
plates, stagnant corners, and strong air currents are some of the causes of
choking.

The fibre content of the cane sometimes affects the performance of knives
and shredder. When the cane has suffered severe stress such as during a
drought, it becomes more difficult to prepare. At these times, the engineer
may have to resort to reducing the number of knives and hammers to
prevent overloading of the drives, and to avoid choking.

3.5. Design of shredders

The design and manufacture of the cane shredder has undergone

DeLmOs order considerable development in the past 30 years, and many types and makes
are now on the market. In South Africa the most popular has been the
Tongaat-Hulett shredder which has proved itself in many mills to be robust
and well-engineered. The hammers are attached to the shaft using
alternate star-shaped plates, bored to suit pivot bars made from a high
grade of martensitic steel, and keyed to the shaft. The plates are held in
position by "Ringfeder" clamps at each end. The bearings are chosen so
that the speed and load-bearing ratings are compromised. If the bearing is
chosen for speed, it cannot take the load, and vice versa. The bearings
must be lubricated and cooled by circulating oil through them, and the
control system must be arranged to trip the shredder if the oil pressure or
temperature departs from set values.

The shredder can be fed with knifed cane either ahead of the shaft or over
the shaft, the former being the arrangement illustrated in figure 3.

A recent alternative for South Africa is the whole-stick shredder, in which

the feed is horizontal. The cane stalks are gripped between a slat carrier
and a feed drum, and pushed into a shredder rotor cutting upwards, and
carrying the cane through the washboard over the top.

These shredders are proving to be reasonably effective, but the power

consumption, particularly surge power, is higher than originally allowed
for. It is now recommended that for 300 to 350 tons cane per hour, the
drive should be 4000 kW. Although the wear rate of the hammers is also
much higher than that of conventional shredders, it should be compared to
that of both hammers and knives in that arrangement. This shredder is
discussed in a paper by Crossman (1994).

Power
In general, the PI depends on the power consumption of the cane
eurummptfon preparation equipment, which is also a function of the fibre loading of the

10
plant. Renton (1974) proposed an equation relating these variables, which
can serve to illustrate the principle.

PI = 67,3*(W)^0,09

Where W = kW/ton fibre/hour

The installed power on most shredders in South Africa is 40 to 68 kW/ton

fibre/hour and that for knives, in total, is 28 to 70.

4. PROCESS OF EXTRACTION

4.1. Effect of imbibition

Extraction in a milling tandem takes place through a combination of

mechanical squeezing and dissolution. If juice extraction is carried out by Dry min a
squeezing only, the bagasse will contain juice equivalent to 50% of its
weight. (This procedure is referred to as dry milling), It has been shown that,
even with very high pressure, it is not possible to reduce the moisture % cane
below about 45% by pressure only. To overcome this limitation, water is
added to take the place of, as well as to dilute, the juice in the bagasse.

In the first mill,the juice is squeezed out of the shredded cane to such an
extent that only about 30% of the sucrose is left in the cane leaving this
mill. In subsequent mills, the sucrose and other soluble compounds are
dissolved in a hot weak solution and then squeezed out in the same way,
and this is repeated a number of times. In order to provide sufficient
liquid, water is added to the process before the last mill

The added water, called imbibition, with some remaining sucrose, is

squeezed out of the last mill, and this final expressed juice is pumped onto Imbibition

the cane entering the second-last mill. The juice from this mill is pumped
onto the cane entering the third-last mill, and so on. The juice from the
first and second mills, known as mixed juice, is pumped over screens, and
thence into the factory for further processing.

The bagasse from the final mill will contain very dilute juice and the mill Imbibition
extraction will be greatly improved. An important point is that imbibition can ,mdy
be effective only in cells that have that have been ruptured. To maximise
i mbibition efficiency, the following points must be noted;

• The water (or diluted juice) must be evenly distributed through the
bagasse layer.
• Maximum penetration of the layers must take place.
• The bagasse must be finely prepared.
• The first mill extraction must be good.
Amount or The weight ofthe water used varies from 45 to 60% of the weight of cane or 300 to
imbibition 400 % on fibre in cane. In practice the amount o£ imbibition is usually limited by.

The mill itself juice capacity, drainage, etc.

Juice heater and evaporator capacity.
Steam balance ofthe factory.

)Figure 5. Graph of extraction vs imbibition

The effect of changing the imbibition rate is best illustrated by the graph shown.
Variation of
extmcdon with
This change is due to the diluting effect of the extra water being added to the cane at
imbibition each stage. Note that the graph has an asymptotic shape, which means that it
approaches a maximum (of 100%) without ever reaching it. Thus when the
extraction is already at a high level, it requires a large addition of imbibition to
Makiple
compound
achieve a very small increase in extraction.
imbibition
The more usual method of applying Imbibition is known as Multiple Compound

re fi. Di of i ' tandem illustra

multiple compound imbibition

Imbibition, as described above. This is clearly shown in figure 6.

12
 Simple imbibition is that in which water is added to each mill in the tandem, and the
juice from all mills is mixed together and taken into the factory. This method is no
longer practised, but for information, it is illustrated below. MuMple simple
bmbibltion

I drE 7. Diasrram of melF nZ tandem i7lusti t'sr, multiple simple imbibition

Because of the gradient of brix down the milling tandem, which will be
Pumping and
illustrated later by means of a practical example, it is important that the cireolation to be
i mbibition juices be pumped to the appropriate mill, with no by-passing or c&MMIIY
maintained
short circuiting being allowed. This would change the dissolving effect of
the juice and performance would suffer.

Imbibition water is usually provided by condensate from the lower level

sow or
effects of the evaporator, which would be available at a temperature of 70- imbibition
84 oC. It is theoretically beneficial to extraction to use hot imbibition,
because hot water will dissolve sugar more readily and will tend to break Hat lmbmi8on
down cell walls to get at sugar inside the cells. This does introduce some
difficulties, such as slippage and excessive vapour which impedes
visibility, but they can be overcome. The main reason that more mills are
able to use hot imbibition is the improved roller roughening technique
introduced since the mid-1974's, using a new type of welding rod
developed in Australia, and described below.

4.2. Juice screening

The mixed juice pumped from the trays of the first and second mills contains
Need for Jake
a large amount of fibrous material and dirt (going by the quaint name of cusp screening
cosh) originating in the cane. Before this juice can be clarified, the rush cosh
should be removed. If not it could foul the mixed juice heaters, and overload
the clarification system, employing an excessive quantity of lime and
flocculant, and overload the mud system and vacuum filters.
 The most popular screen is known by the name of `DSM" which stands for
r15M scrercm
Dutch State Mines, which organisation apparently developed it. The
screening element consists of wedge wires of trapezoidal cross-section
wrapped around a rod in such a way that the gap increases from front to back
of the screen. The whole screen is then mounted in a vertical frame with the
screen forming an arc starting from vertical and ending up with a tangent
about 45° to the vertical. This is illustrated in figure 8.

One of the advantages of this type of screen is that it is self cleaning and can
self-leanIng
be operated with very little supervision. However, in the interest of hygiene
it should be regularly washed down with hot water. The whole installation is
best mounted at a high level so that the Gush cusp can be washed or "flumed"
into the No I interearrier by the maceration juice from No 3 mill.

The gap in the screen depends on the nature of the cane and the preparation,
and also on the downstream clarification requirement. The gap varies from
0,5 to I mm with 0,75 being the more common gap.

FROM SCREEN PUMP

USH

TO MIXED
JUICE PUMP Pgure & Sketch of a DSM screen

The screen area to throughput ratio used in South Africa is about 0,05 m 2/ton
Screen Isak dze
and area cane per hour for a diffuser and about 0,1 for a mill with a 0,75 mm DSM
aperture screen and somewhat higher for 0,5 mm aperture.

14
The distribution of juice across the width of the screen is very important.
Julce
The more usual feed consists of a fan shaped trough above the screen dbWbntion an
followed by a large radius sill on the weir feeding the screen. Some mills
have arranged mechanical agitators or "stilling" pots in the troughs to ensure
even flow. The juice leaving the weir must impinge tangentially onto the
screen without any gap between the stream and the screen. Such a gap could
result in "stapling" of the fibre, which is the fibre sticling straight up in the
screen gap and causing choking ofthe screen.

The BSES in Australia have found that the DSM type of screen is quite
satisfactory, but that the rotary screen is to be preferred for future
installations. (See Brotherton et al. 1981)

The rotary screen consists of a cylinder of screen material running on

Rotary Kreem
trunnions and driven by a roller or chain drive. It is called a "Peck" strainer
in its older form with a wire or punched plate screen. The wedge wire rotary
screen is known as a "Contra-shear" screen and has much improved
performance over the older type. The juice is fed into one end over a small
weir so that it meets the screen as nearly tangentially as possible. The fibre is
carried to the outlet by means of spiral flow diverters.

Sand removal is also a problem, more serious in some mills than in others.
Sand drops out in tanks where the flow velocity slows down, and has to be sand remaval
dug out by hand every week. A lot of sand comes out in the clarifier, which
is probably the best place to remove it from the handling point of view. Sand
settling tanks are not wise because the extra residence time can cause sugar
losses.

Trials have been carried out with liquid cyclones but without much success.
The underflow from the cyclone still has to be separated and washed in order
to return the sucrose to process.

In a diffuser, most of the sand remains in the bagasse and ends up in the
boilers where it is disposed of with the boiler ash,

Screen performance

Poor screening efficiency can be disastrous in its effect. The usual problem
is that the screens become choked with bacteria, or with very fine fibre and
Effec! of screen
the mixed juice is prevented from passing through the screen and ends up blocUng
with the cush cusp. From here it finds its way back to the first mill and a
R ip of
degree of re-circulation takes place. It can be shown by calculation that, joke
with certain assumptions, for a 20% increase in juice re-circulation, the
tandem extraction would reduce by 0,7°/o.

Screen eMciency
If too much fibre passes through the screens, such as when they have worn
to a larger slot size, the efficiency of the clarifier will suffer, and often it
takes a long time for the problem to be discovered and rectified.

15
 5. THE MILL BALANCE

mvWou of The tons of sucrose in mixed juice pumped from the extraction plant into the
Proceeds
factory is the most important measurement required for the distribution of the
Juice ma„ proceeds from the eventual sale of sugar. In order to establish this figure as
accurately as possible, the mass of the mixed juice is determined on a batch type
scale. The juice is pumped into an overhead tank, from where it discharges

Fizure 9. Diagram of mill m ass balance

through an actuated naive into a weigh tank or "hopper" the mass of which is
determined when it is full by means of load cells connected to a totaliser. The
hopper empties, the tare or empty mass is subtracted in the totaliser, and then it
refills from the overhead tank in a repeated process controlled from the
totaliser. The juice is carefully sampled after the scale and analysed for pol,
brix, and suspended solids. The total mass of sucrose is calculated from this by
applying the current pol to sucrose ratio.

The bagasse leaving the last mill is also carefully sampled, and analysed for pol,
fibre, moisture and (usually) ash. The total mass of cane entering the mill is
accurately known from total cane coming over the weigh-bridge, and the pol in
cane is calculated from the direct analysis of cane (DAC} sampling carried out
by the cane testing service. The fibre in cane is also calculated from the same
analysis.

It is assumed that sucrose in imbibition is zero. A mill mass balance is then

calculated using the mass relationships below:

Mme fibre in bagasse = fibre in cane - suspended solids in mixed juice

fvrmulke
bagasse = fibre in bagasselfibre % bagasse x 100
imbibition = bagasse + mixed juice - cane

16
 pol in bagasse = pol % bagasse x bagasse 1100
pol in cane .-_ pol in juice + pol in bagasse

The pol in cane from the DAC calculation expressed as a percentage of the pol
in cane from the mass balance is called the pol factor, and is carefully monitored
to determine whether there are excessive losses of sucrose between the weigh-
bridge and the juice scales.

Allowance must be made for evaporation loss, which reduces the accuracy of
the above calculations slightly.

6. JUICE EXTRACTION CALCULATIONS

By sampling and measuring the bagasse and juice through the tandem, it is Meaauremeret. a f
tndtvWuar mM
possible to calculate not only the performance of the tandem as a whole, Pe rfo a
but also the performance of the individual mills in the tandem. This is a
highly recommended practise that can be rewarded by improved performance
for the engineer.

Although the calculations are simple, because of their quantity, they can
become tedious if done by hand. However, with spreadsheet programmes
available on computers, the whole calculation can be done on one spreadsheet,
an example of which is given in Table 1.

The diagram in figure 10 should serve to clarify the individual mill mass
balances.
 Table 1. Extraction calculation spreadsheet

CA NE
Given. Tons cane Pol % fibre in cane 93.33
Fibre % cane I mbibition % fibre 300.00
Tons imbibition Extraction 97.98
IM % cane
Brix% first mill juice
Brix % mixed iuice
Mill juice balance 2 3 4 5 6
Moisture % bagasse - this 11611 law
Brix 1% begasse
Juice Q bagasse 6910 6310 51140 5410 5150 47.00
Fibre 96 Bagasse 3010 3610 41.80 J 4510 4150 53,01
Tons fibre 3010 3010 30.00 30.00 30.04 30.00
Tons begasse 9816 8134 ® 6150 600 56.80
Tons juice in bagasse 6&36 51.74 42.12 35.50 30.61 26.60
Tons juice i nfo mill 17010 18150 157. 26 14111 129.50, 120,61
Tons juice i nto juice tray 101.64 131.76 115A4 105.51, 98-901 94.00
Mill juice extraction 59.79 71,8
Tons mixed juice 233.40
Tons brix in mixed juice 33.14

Mill p al balance 1 2 3 4 5 6
Pol 51 bagasse z.: a. Vii. a
Tons Q leaving mill 7.38 4.113, 1.51 0.97 0,57
Tons pol entering mill 28.00 11.1 4 3.46 1.91 0.97
Tons pol into juice tray 20.62 6.81 . ® 1.96 0.941 0.40
Mill pof extraction 73.65 81.12 5017 5612 *124L 4113,
Tons pof i n mixed juice 27.43 --
Tandem pM extraction 9718
Mill brix balance 1 2 3 4 5 6
Tons brix leaving mill 9.3.4 5.15 3.17 2.10 1.52 1.13
Tons brix entering mill 33.14 1&36 7.19 4.14 2.48 1.52
Tons brix into tray 23.80 8.21 412 2.04 OM 0.38
Pol extraction 1 2 3 4 5 6
Pol 56 bagasse 7.50 530 310 2.30 1.60 1.00
Fibre % bagasse 30.50 36.70 41.60 45.80 49.50 53.00
Pol 96 fibre 2419 14.44 8.41 5.02 3.231 1.89
Progressive individual extraction 7315 84.53 90.99 94.62 96,541 97.98
[ Unit individual extraction 73.65 10.87, 6,46, 3.63~ 1.92

Note. The highlighted figures are measured and inserted into the spreadsheet, and
all other figures are then calculated.

18
The equations applicable to the spreadsheet are as follows:
FormaLAe for
1. Juice % bagasse = moisture % bagasse + brix % bagasse ext: adlon
cau ui. don.
2. Fibre % bagasse = 100 -juice % bagasse
3. Tons fibre ( assumed to be equal to the tons fibre in cane
throughput the tandem) = fibre % cane x tons cane 1140
4. Tons bagasse = tons fibre 1 fibre % bagasse x 140
5. Tons juice in bagasse = tons bagasse - tons fibre
6. Tons juice into mill = tons cane - tons fibre (for first mill)
7. Tons juice into mill obtained from individual mill juice mass balances
8. Tons juice into juice tray obtained from individual mill juice mass balances
9. NO juice extraction = (8)1(6 or 7) x 100
10. Tons pol leaving mill = pol % bagasse x tons bagasse
11. Tons poi entering mill = tons pol in cane (for first mill)
12. Tons pol entering mill obtained from individual mill pol mass balances
13. Tons pol into juice tray obtained from individual mill pol mass balances
14. Mill pol extraction = (13)1(11 or 12) x 100

The brix balance is obtained from individual mill brix mass balances, and poi exbadion
this could be used to calculate individual mill brix extractions. However,
the pol extraction is more important from a financial point of view, and this
i n completed by applying the following formulae:

16. Pol % fibre = pol % bagasse / fibre % bagasse x 100

17. Pol % fibre in cane = pol % cane 1 fibre % cane x 100
18. Progressive individual extraction = (pol % fibre in cane - poi % fibre
leaving ) / pol % fibre in cane x 100
19. Unit individual extraction = (pol °Io fibre entering - pot % fibre leaving)
/ pol % fibre in cane x 100

Another very useful report for the mill engineer based on these calculations
is the plot of brix % bagasse leaving each mill, An example of this curve is a,ix carve
given in figure 11. The shape of this curve is ideal, in that the brix drops
more in the early mills than in the last mills, and the curve is relatively
smooth from first to last. If in an actual curve, any of the points are either
above or below this ideal, the engineer can infer the following:

If the point is higher than ideal, the previous mill is under-performing.

If the point is lower than ideal, the next and/or subsequent mills are under-
performing.
 Mill Brix Curve

10.00

9.00

a.o0
7.00

4
e.a0
5.00

m 4,00

3.00

2.00

1-00

0.00
1 2 3 4 5 6
Mill number

Figure 11. Plot of brig °/0 6ap-asse leaving each mill

7. FEEDING CANE INTO THE MILL

Over the years of mill technology development it was recognised that the
efficient feeding of the mill is of paramount importance and many devices were
invented and tested to improve this. Those which have survived are:
Donnelty chutes
Donnelly chutes consist of tall (3 to 6 m) rectangular section chutes in which
the cane feeding the mill is forced by its own weight (static head) into the mill.
The chute must be divergent to avoid choking (Usually 2°). These chutes
require long steep inter carriers, and are thus often difficdt to fit to eadsting
tandems.

Underfeed rolls Underfeed rolls are light rolls usually of smaller diameter than the main rolls and
arranged above the feed roll and almost touching it. This roll is usually driven
by a chain and sprockets from the feed roll or by a light gear drive from the top
roll, at a surface speed equal to that of the mill rolls. It is usually grooved in the
same way as the mill rolls, and the grooves are roughened, although much less
than the mill rolls.
 TRASH ATE
AND FUME
TURNER

A two-rot pressure feeder (PF) was developed in Australia and has become Pressw* feeder

almost standard in that country for all mills. The PF rolls are usually the same
size and diameter as those of the mill, and are arranged to feed the cane into a
high pressure chute which in turn forces the cane into the mill. The PF rolls are
driven either from a separate prime mover and gearing (as at Felixton MR in
South Africa) or from the same gearing as the mill, from a gear pair on the final
drive shaft. The PF is illustrated in figure 12.

In Australia the PF has been shown to improve the mill performance roughly in Perfoemance of
a PF
proportion to half an additional mill in the tandem for every PF added. A 5-mill
PF tandem is equivalent to a 7-mill conventional tandem. It is also fairly
common to find an underfeed roll included with a PF, thus maling a six-roll
mill, as illustrated in figure 12.

A common problem with the PF is that the pressure inside the chute sometimes Hiab PF
pressure can
rises until the chute either bursts, is pulled from its mountings, or becomes so efflue serlow
choked with compressed cane that it has to be removed and cleaned out. This problems
operation can take several hours, and can only be carried out with the whole
tandem off-Line. Various devices have been designed to warn the operator of
increasing pressure, based either on chute pressure or drive torque. Some
designs have been introduced in which the chute is extremely robust, and the
drive control sufficiently sensitive to trip the mill before any damage can occur.
In one design the PF is constructed in such a way that the whole assembly can
be hinged open in order to easily work on it.

21
Other feeding devices were used in the past but since they are now obsolete
they will not be discussed.

In Southern Africa and also fairly generally elsewhere, except Australia, it has
become common to have a Donnelly chute and an underfeed roll ahead of each
mill in the tandem. It is particularly so with dewatering mills, in which it has
become common practise to have two four-roller mills with Donnelly chutes in
series, thus providing the best dewatering combination. The PF has in fact
fallen out of favour, and new mills are being installed without it. Those mills
that still have PF's are not reporting good bagasse moistures.

8. PRESSURE IN MILLS AND MILL HYDRAULICS

When cane is fed without slipping into a sugar mill, the feed rolls force cane
into the space below the top roll and generate enormous pressure. This
pressure creates high stresses in the roll shafts, mill housings and other
components, and high bearing pressures. Since the performance of a mill
depends on this pressure, it is important to keep it as high as possible, without
causing stresses to be so high as to break shafts, gears or housings.

For a comprehensive treatment of the subject, the student is referred to the

excellent chapter by Hugot (1972) "Pressures in milling" (p 113 ). The summary
that follows is intended to give the student an overall grasp of the subject.

The magnitude of the pressure depends on two main factors:

1. The compression ratio, or the ratio between the thickness of the
bagasse blanket before the rolls to the work opening between the
rolls.
2. The reabsorption coefficient, which is discussed elsewhere. This in
turn depends on cane preparation, roll roughness, and drainage.

If the reabsorption coefficient r = I (which is not the case in practise), the

formula for the resultant hydraulic pressure in kg on the roller, is
(Hugot p 155):

F (30LD4e,)1 C6 1 D6
Where F Load resulting on each roll, kg
L length of roll, cm
D diameter of roll, cm
sn specific work opening, eAID,
ea actual work opening, cm
C compression ratio, en/l-1
H thickness of bagasse before the rollers, cm

The effect of reabsorption coefficient is included in the second formula (Hugot

p 158):

22
 F (1300LD4EA) x ((q.ds)/(r.eA.f )} X (1+4 (r-1))
Where q fibre loading, kg/dm'
dB density of bagasse, kgldm3
r reabsorption coefficient
f fibre per unit weight of the bagasse

The way in which the mill has been designed to control this pressure is to allow ayarionbc
the top roil to lift against a known force provided by hydraulics. The top roll kmUltag of Mill
roBs
bearings are located in vertical slides where they are constrained by hydraulic
rams which force the roll down onto the cane. The rams bear down on the
bearing caps via spherical seats which eliminate sideways thrust of the bearings.
The hydraulic circuit is provided with an accumulator which usually consists of
a vessel with a nitrogen-filled bladder which because of its compressibility
maintains the oil within it at a practically constant pressure even though the
volume changes. A diagram of the hydraulic circuit is given in figure 13.
ayaMUNC
Pressures in the rams are maintained in the order of 20 to 30 MPa, which presaare

would provide total loads of 8 to 12 MN on the top roll. Adjustments in the

hydraulic pressure are sometimes necessary to keep the roll floating during ail
conditions.

MILL
CHEEKS

FTQure 13. Diazrm of a tynk al mill hydraulic circuit

The pressure can be adjusted by either releasing oil from the accumulator back
to the sump, or by running a pump to force more oil into the accumulator.
 9. MILL ROLL LIFT

Ron lift gad The top roll is forced upwards against this hydraulic cushion by the cane, by a
"
nost
'"e `°"' distance called "roll lift" which is usually about 10 nun. If the roll is lifted
through the full travel of the hydraulic rare, it comes against stops, usually
about 25 mm from the bottom position. When lifted to a position below these
stops, the roll is said to be "floating" or "live". It is essential to good milling for
the top roll to be floating so that the mill settings are being used correctly, and
to ensure that the pressures in the mill are neither too high nor too low.

Other variables which could affect roll float are roller roughness, feeder roll
effectiveness, imbibition quantity and efficiency, drainage, trash plate setting,
cane preparation and uniformity of throughput.

Rol CRb or It is essential that a roll lift indicator of some land be installed and maintained
on every mill bearing. The main purpose of this indicator is to ensure that the
top roll is always operating in the floating position, and as close as possible to
the level allowed for in the mill settings calculation.

A simple lift indicator consists of a vertical rod arranged to slide in a fixed tube,
and touching the bearing housing of the top roll. At the top of the tube, an
indicator arm is arranged with a fWcrum close to the tube so that the other end
multiplies the travel by a factor of about 10.

10. BEARINGS

ME bmftv mW
Mill bearings are made of bronze with a high aluminium and phosphorous
content. A high quality of casting is necessary to ensure adequate wear and
pressure resistance. The pressure on the bearings can be calculated from the
hydraulic pressure in the accumulator.

Bearing pressure accumulator

( bearing length x diameter)

For the usual size of bearing this pressure should not exceed 12 Ml?a which
pressure is however often reached in large mills.

see
tabdcattare
Lubrication of bearings is effected by a high viscosity oil which has been
developed by the major oil companies especially for sugar mill use (e.g. ASMR
heavy by Castrol). This oil is delivered to most mills in bulk tankers and
pumped to high level storage tanks above the mill house. From there it
gravitates to oil feeders which are connected to all the bearings in the tandem,
thus ensuring an even and continuous flow to each bearing. The oil is fed into
the bearing via an oil groove which is carefully located about 45' ahead of the
extreme pressure point of the bearing.

24
Oil leaking from the bearings is collected in trays and is usually poured into the
lubrication troughs of the mill pinions, which do not require as pure a lubricant
as the mill bearings.

Cooling of the bearlngs is carried out by water being led into chambers built
into the bearing housings. The cooling water is returned to the cooling tower
through tundishes which are convenient indicators of the flow and temperature
of the water emerging fiom the bearings.

Different materials have been tested in mill bearings, such as white metal and MMMM
bming
plastic. White metal is expensive, but reduces the friction and thus the
temperature of the bearings. However they require very good sealing to
prevent ingress of juice and grit, which can quickly destroy the surface of the
bearing and aggravate shaft wear.

Plastic bearings require no lubrication, but they have an inherent disadvantage

in that they do not conduct the heat away to the cooling water and cannot
effectively be cooled. If the cooling water could be rendered non corrosive, it
could be pumped through the lubrication ducts and these bearings may then
succeed. But it seems that none have been completely succmU to date.

Roller bearings for mills are commercially available (See Hugot, 1986), but
have also not been widely accepted. The main reason is that sugar juice is
notorious for finding a way through any seal, and would quickly damage a
roller bearing in that event.

11 .MILL ROLLS

11.1. Shaft and shell design

The design of the sugar mill roll has been developed over the years to a MM roll design,

satisfactory stage which generally withstands wear and stresses for at least one spedficauona
and stream
full season and usually for much longer. The roll shell is made from a
close-grained cast iron, which is poured vertically to ensure correct segregation
of blow holes. It is bored to size and shrunk onto the shaft with a diametrical
interference fit of up to 0,0008 times the shaft diameter. The shaft is forged
from mild steel which needs to be carefully annealed before being finally
machined. Because the stresses in the shaft are often higher than the fatigue
endurance limit of the steel, it is very important to eliminate all possible surface
imperfections which could cause fatigue failure.

The stresses in the shaft are caused mainly by a combination of torsion and
bending. The maximum stress can also be increased by a poor fitting tailbar
coupling, or by excessive lift of the top roll. These factors could cause frequent
failures of the shafts, which can seriously affect the output of the mill, and
 should be avoided by all possible means. Some of these are:

Proper care of the sham surface to avoid stress raisers, particularly at the
Cam of the 3haft high stress points
Careful specification, and quality control in manufacture and re-shelling
Good maintenance and fitting of the tailbar couplings, or using a coupling
that can allow for large axial and angular mis-alignment without causing
undue stress (Tosio, 1988)
Adequate sealing o£ the flange to the top roll shell to avoid corrosion
Using the largest practical radius for the fillets at every change of diameter

For a more complete treatment of this subject, the reader is referred to two
papers Reid (1988), and Anderson & Loughran (1999).

i X.Z. Roll grooving

The surface of the roll is provided with circumferential grooves that serve
several purposes:

P or . They assist in gripping the cane

The roots of the grooves provide drainage channels
They maintain performance even if damaged by tramp iron, etc
The grooves break up the cane at each squeeze and break more cells

The grooves of the meshing rolls do not intersect with each other, as can be
seen from the grooves in figure 15. Thus the opening between the rolls can be
smaller than the depth of the groove, and in the latter mulls of a tandem the
discharge openings usually are less.

The pitch of the grooves varies from 20mm to 60mm. Choice of pitch is to a
large extent a matter of personal preference or tradition for a particular mill. In
South Africa the pitch is usually either 25, 30 or 5flmm. The main advantage of
a small pitch is that the number of drainage paths for the juice is greater. Thus,
if drainage is a problem, a smaller pitch should be used. The disadvantages of a
smaller pitch are that the teeth are more fragile, and as they wear it is more
difficult to maintain the tooth profile. Arcing is more difficult, and the drainage
groove often becomes cluttered with stray weld spatter. Also, the grip on the
cane is better with a large pitch.

Several mills have adapted a compromise, in which the top and discharge rolls
are half the pitch of the back and under-feed rolls. Care must be taken in this
case to ensure that the set openings are still measured between the average
diameters of the rolls, ie, half the depth of the groove, regardless of the pitch.

The angle of the grooves also varies. The principles are the same: the smaller
the angle, the better will be the drainage, but the more difficult to maintain the
grooves. Angles between 35° and 55° are usual, with 35° or 45° being the

26
more common.

12. MILL DRIVES

The performance of a sugar mill can be greatly affected by poor selection,

design or operation of the driving train, from prime mover to coupling.

Although much work has been done in the past to ensure that mills are
provided with the most efficient and economical drives, there has been a
tendency to follow the turbine drive route, although increasing attention is
being paid to the advantages of electrical and hydraulic drives.

The requirements of a sugar mill drive are low and variable speed, with a flat Requirements
torque curve over the whole speed range. Although it is desirable to have a For a mud drive
high inertia drive because it handles variation in load easily, it cannot be stopped
quickly in the event of a problem. Law inertia drives, however, could cause
problems if the load variation is excessive and frequent.

12.1. Comparison of different drive units

The main types of mill drive prime movers that have been used to the present Diirererit drive
time are as follows: Unib

• Steam Enne

The steam engine causes oil contamination of exhaust and thus of the
condensate for boiler feed. It is heavy in maintenance cost, and because of
obsolescence is now difficult to keep running. Also with higher boiler pressures
being generated engines would be prohibitively expensive to replace.

The last steam engine drive in South Africa was replaced with a turbine at the
end of 1990.

s Electric Motor

Electric motors were used on mill drives from about the mid 1924's and have
been well accepted wherever they are used. Development has gone through
various stages, listed below roughly in historical order.

Slip ring Induction

• AC Commutator motor
• DC with Thyristor drive
• Cascade Drive as at Noodsberg mill, in South Africa
• AC Variable frequency Induction

The torque characteristics have been improved to the stage where the AC
AC vsriabk
variable drive can be specified to provide an almost ideal torque curve. As mpeed drive

27
 electrical technology improves, the electric motor could become the most
popular drive.

Note that with the electric drive, the steam has already been used to produce
energy in the power station, so it should really be called a turbo-electric drive.

Turbine

This has all the advantages for operation on a sugar mill. However, installation
costs and maintenance tend to be high. Also, it does tend to make the mill
house uncomfortable, as regard heat, noise and safety. One thing to remember
about a turbine drive is that its efficiency drops off considerably as the load
drops from maximum and also as the speed decreases (or increases) from the
designed speed.

This is not a problem where there is a large exhaust steam demand, but as mills
become more exhaust steam dependant, the inefficiency of turbine drives can
become an embarrassment.

Hydraulic Drive "turbo-electro-hydraulic drive")

In South Africa, there have been a few poor experiences with hydraulic drives,
which have tended to give them a bad name. However, a properly designed,
specified, and installed hydraulic drive can have some exciting advantages over
other drives. In one example that the writer has viewed, at Union St Aubin in
Mauritius, the final drive gear is driven by three pinions, each driven by two
hydraulic motors. These in turn are fed by two variable displacement pumps
each driven by a 260 kW motor. (See Raffray, 1986)

Typical hydraulic drives are described in two papers, the first by Jorgensen et
al, (1986) and the second by Shield et al, (1995). In both these cases and in
others that have been reported, the experience of the hydraulic drive has been
good.

Some of the advantages of a hydraulic drive are:

Advantages of r Step-less variable speed at full torque from zero to maximum rpm and also
hydrantic drive fully reversible.
In a multiple pump/motor arrangement, the mill could still limp along in the
event of failure of any one component.
The space requirements are far less because of fewer and smaller gears.
The arrangement of pinions as in the example can reduce the tooth load on
the final drive gear.
When the drive is stopped, there is no over-run caused by inertia.
13 .GEARING

Much has been written in Sugar Technical journals about gearing, mainly by
gear suppliers. Papers by Partridge (1978), and Beale et al (1993) cover a
wide range of gearing. The latter paper describes the modern development
of a dual pinion drive, which is considered to be the drive of the future.
Important points to note about sugar mill gearing are:

13.1. Specification

The gear manufacturer usually specifies the details of the gearing, The specification of
gearing
customer generally asks for a certain minimum standard based on life and
service requirements and the supplier does the rest. The major South African
manufacturers have moved away from British Standard 436 and now use the
AGMA standards for gear design, which are basically more conservative
than the minimum requirement of BS 436. A factor of about 1,25 applied to
the latter would roughly equalise the two designs. This factor provides a
"life" for the BS 436 case of 52 000 hours but in the ALMA case, the "life"
calculation is actually based on infinity, and the limitation to the life then
depends on bearing selection.

13.2. Lubrication

Mills in South Africa have been fortunate in having had excellent service Gear lubrication
from lubrication suppliers. This service has included a free annual gear
inspection. Nevertheless, the importance of lubrication can never be over-
stressed, and maintenance of the lubrication equipment is as important as that
of any other of the sugar mill.

The lubrication of high speed gears differs from that of low speed gears in
the viscosity requirements, heat generation and rapidity of wear. The higher
speed gearing usually has recirculating oil systems with oil coolers, while the
slower gears use a higher viscosity lubricant applied by gear immersion.

13.3. Loading and Overloading

In respect of gear life, steam turbine drives have a distinct disadvantage: the
Danger with
torque which can be generated by a turbine at low speeds can be extremely turblne drives
high, especially if the facility of opening additional nozzles is available.
Figures of up to four times the full load torque have been quoted by some
turbine suppliers. This fact is a constant source of concern to gear
manufacturers. However, it should be remembered that to overload the
gearing, the load on the mill must be increased. The turbine over-rating
merely makes this possible.

29
Torque loading Whenever torque measurements have been carried out, excessive torque has
of gears never been found for prolonged periods, on any mill. However, there is a
cyclic variation, caused by the poor meshing of roll pinions, and by the
rotation of the box couplings on the tail bar. It is suspected that this causes
far more trouble than over-rating of the steam turbine. It is preferable to rate
the gearing based on the facility to be able to slow down the mill
considerably. This would not be expected to increase the torque by more than
that required to improve the milling performance. Provided that the
lubrication at slower speeds is adequate, the life o£ the gearing might not be
affected all that much. But there would be a danger of catastrophic failure in
the event of a jamb up, which would occur because of the greater available
torque from the turbine.

14.CONSTRUCTION OF MILL

Details of the main components of a mill and their functions, for example,
rolls, cheeks, bearings, trash plate and dumb turner, scrapers, hydraulics,
settings, and adjustments should be read with reference to the diagrams
included with these notes.

14.1. Trash plate

The method of setting the trash plate for good performance is covered in
section 17.

We ar or trash
plates of all the items in a mill the trash plate is one that can suffer from the most
wear, and is also the most difficult item to replace. Any procedure that can
extend the life of the trash plate will therefore be well rewarded.

Trash plates are made from cast iron, malleable iron or cast steel. In a recent
survey, cast steel was found to be the more common material, but the other
Material of
trsah plates two were quite significant. The material itself is perhaps less important than
its ability to accept hard facing using one of the proprietary welding
techniques, and all three of the above-mentioned materials will be adequate
for this purpose.

The top surface of the trash plate is hard faced by are welding using
proprietary rods or wire. The roots of the teeth should not be hard faced as
this could wear away the tips of the grooving on the roll and thus affect the
performance.

Two factors cause excessive wear: over-tightening and bad setting. Wear
due to tightening, or adjustment against the feed roll must be traded against
leaking or dribbling of fibre through the opening in front of the trash plate.
Ideally, there should be no dribbling with minimum wear.

Trash plate If the trash plate is set too high or if the sweep is wrong it can also wear
setting excessively. Some engineers today are finding that the wear can be much

30
reduced by lowering the trash plates below the commonly accepted position
by as much as 50 mm. Note that the purpose of the trash plate is merely to
turn the bagasse into the discharge nip and it should not be required to exert
any pressure on the bagasse. It makes sense therefore to set it as low as
possible, provided that the mill does not choke,

The trash plate is mounted on a large beam which spans the width of the mill
and which in turn is carried on adjustable supports so that the angle, height
and horizontal position of the trash plate can be easily adjusted.

14.2. Scrapers

The trash plate is a special case of scraper to ensure that the roll grooves are Scraper wear
and setting
kept clear of fibre, working on the feed roll. The top and discharge rolls have
scrapers fitted, which are flat plates with teeth arranged with suitable
adjustments at the discharge of the mill on each roll. These also have to be
protected against wear by means of hard facing, but also need to be soft
enough not to damage the roll grooving and to wear into the shape of the
grooves. Scrapers are usually made from mild steel.

14.3. Mill Housing

Mills are rated by the length of the working portion of the roller and its
maximum diameter. Most mill rolls are 2134 mm long by 1170 mm
diameter. The heart of the mill consists of three rolls, top, feed (or back) and
discharge. The bagasse passes through the opening (or nip) between top and
feed rolls, from where it is "turned" by the trash plate (or turning plate) into
the opening between the top and discharge rolls. The bagasse is given two
squeezes, during which time the juice is expressed, and drains down into the
tray below the mill.

The mill cheeks (or head stocks) which are the frames holding the bearings,
Mill cheeks or
are today made of cast steel, and are bolted to the bed plate. There are many
different constructions of mill cheek, each claimed to be better than the other.
However, common features are: heavy bolts holding the bearing caps in
place; adjustable bearings, in order to vary mill settings; incorporation of
hydraulic rams on the bearings of one or more of the rolls-usually the top
roll. Mounting brackets for the trash plate support, scrapers, juice trays, juice
seals, etc.

14.4. Pinions

The top roll is driven by the tail bar coupling, and it drives the feed and ROOL pinions
discharge roils through pinions which have specially designed teeth to permit
variation between the centres. Pinion designs and materials vary widely, and
the life of the pinions reflects the choice of material and the design of the
teeth. The material is usually cast steel, but ductile cast iron has been tried
with some success. The tooth shape is usually cast in, and no machining is

31
 required. The wearing-in of the teeth is rapid, and the subsequent life is
usually adequate. Some mills apply hard facing to the teeth to combat wear,
but this is often at the cost of frequent breakages caused by heat-induced
residual stresses in the material.

145. Cooling

The bearings are provided with water jackets through which cooling water is
circulated, to maintain a reasonably cool bearing surface for the rolls.

14.5. Roll Adjustments

The feed and discharge rolls can be moved relative to the top, by adjusting
Mill settings
tapered slides or by inserting packing underneath the bearings.

The positioning of the rolls and the trash plate is important for chill
performance, and this positioning is known as "mill setting". The calculation
of mill settings will be demonstrated in section 17.

14.7. Juice Drainage

Juice drainage As the juice is squeezed out of the bagasse blanket, it must be able to drain
freely out of the nip between the rolls and into the tray under the mill. The
path of this juice is mainly over the back of the feed roll, and between the
back of the trash plate and the discharge roll. This drainage is assisted by
means of Messchaert grooves cut in the feed roll, and sometimes also in the
discharge roll. These grooves must be kept clean by means of knives which
are arranged to clear accumulation of bagasse.

Another method of drainage that has been tried but has not become popular
was the "Lotus" roll, which has small holes between the grooves, which
communicate with longitudinal channels built in the roll.

15. PUMPING AND CIRCULATION

Juice collected in the tray below each mill is pumped onto the bagasse being
fed into the previous mill. This is described in more detail in the section on
compound imbibition.

Chokeless
The juice collected in the trays is full of fibrous material coming from the
PUMPS cane, which would tend to choke pumps and piping if not dealt with
properly. This is achieved by collecting the juice in a "swirl tank" next to the
mill, which keeps the material in suspension. The pumps are "chokeless",
have simple, open impellers, and all the piping is designed to minimise
choking. The swirl tanks are provided with overflow channels so that they
will overflow to a previous mill if the pumps cannot cope with the flow for
any reason. In this way, juice is not wasted. But if the overflow occurs, the

32
pumps must be quickly brought back into service, otherwise mill
performance will suffer.

16. MILL PERFORMANCE

mutual milling
The South African Industry has had considerable success in improving control project
milling performance over the years. One of the major influences in this
was the Mutual Milling Control Project (MMCP) which was undertaken
by the Sugar Milling Research Institute in the 196O's The last progress
report was published by Buchanan et al (1965) in which it was shown that
over the duration of the project the overall milling performance of the
industry improved dramatically. The conclusions of that project were that
the main contributors to good performance were:

• Good cane preparation especially using two cane knives and a shredder
before the first mill
• Promotion of good feeding into each mill
• Maintenance of a rough roll surface
• High first mill extraction
• Good juice drainage

It was also found that the two-roll pressure feeder was not as good as the
investment in it would lead one to expect.

16.1. Performance measurement

Various parameters to indicate the performance of a milling tandem are used Measures or
throughout the cane sugar industry. The most common, particularly in performance:
Southern Africa is:
Extraction
Extraction = Tons sucrose in mixed iuice x 100
Tons sucrose in cane

Extraction of up 98,5% is commonly achieved in this region. This figure

does not allow adequately for changes in the sucrose % cane. Cane with a
high sucrose content will yield a high extraction. Similarly low fibre in cane
facilitates good extraction. Many mill controllers regard the sucrose to fibre sucrose to fibre
ratio
ratio in cane to be a good indicator of the potential extraction that can be
achieved from that cane.

To correct for these effects of sucrose and fibre on extraction a formula for corrected
reduced
corrected reduced extraction (CRE) was proposed (Rein, 1975) and this extraction
has been adopted by the South African Industry for comparison of
performances independent of cane quality.

A standard fibre % cane of 15,5% and poi % cane of 13,0% are selected as
the basis for uniformity. The formula is as follows:-

33
 CRE = 100 - 0.03936 x (100 - E) x (100 - FJ-X-P,,, °,b
Fk
where E _ % poi extraction
P. = poi % cane
FC = fibre % cane
Fb = fibre in bagasse % cane

Moisture and Parameters that affect the extraction are moisture % bagasse and ,pal
poi In bagasse
These are reported hourly to the mill operators to enable them to
correct adjustments in good time.

In atypical example, an increase of one percentage point of bagasse moisture

would cause a decrease of about 0,13% in extraction, while an increase o£0,1
percentage point in poi % bagasse would decrease extraction by about 0,25%

Other indicators of performance listed in Hugot (1972) (p3l2ff) that have

been used in the past, but which have now been largely discontinued are:

milling loss poi % bagasse x 100

fibre % bagasse

extraction ratio (100-extraction} x 100

fibre % cane

l ost iuice °Io fibre brix % bagasse x 10 000

brix % primary juice x fibre % bagasse

lost absolute juice %fibre absolute juice in bagasse % cane x 100

fibre % cane

The latter measurement was used as the main performance parameter to

compare mills during the MMCP mentioned above. This was taken one step
further with the following ratio by which the mills were ranked (Table 2 of
Buchanan et al):

Relative mill performance - 100 lb fbre/(hr) (try)

Lost abs juice % fibre

Where trv total roll volume

On this basis, in the 1964-65 season, the South African mills varied fiom
196,8 for the best to 102,3 for the worst.

A further variable that is used in many cane sugar industries as a basis of

cane payment is the Java ratio. This is given by the formula:

Java ratio 100 x poi % cane

poi % first expressed juice

34
17. MILL SETTINGS

The relative positions of rolls, trashplate and feed chute in a mill are
adjustable. The gaps between the rolls and other components are known as
the mill settings (see figure 14). These settings should be carefully calculated
and adjusted at the beginning of each season, and should be checked as often Natal method or
as possible during the season. Several methods of calculating the settings mill settings
exist, the one used most frequently in South Africa being known as the Natal
or Sugar Milling Research Institute method. Details of this will be given for
the student, on the understanding that it is adequate for this region. Details of
the other methods may be found in the literature: Van Hengel et al (1958)
and van Hengel (1964), and also Hugot (1972).

14. Di of mill rolls sho ' sett s

It should be emphasised before going into the detail of mill settings that they
are only true when the top roll is floating in its pre-calculated position. Also,
the purpose of pre-setting the mill rolls is to ensure that the ratio between the
gaps in the feed and delivery openings is equal to what is required. The top
roll will be lifted to a height determined by the feeding efficiency, hydraulic
pressure and structure of the cane, which then determines the ratio. The

35
settings are therefore seen as being subservient to these other factors in
determining the performance of the mill.

The formula to calculate the work opening between the top and discharge
rolls (DWO) is as follows:

K(mm) = 286 X104 x Cf

nDLF

Where C Tons cane crushed per hour

F Fractional fibre content of the cane
n Speed of the top roll, rpm
D Diameter of top roll, mm
L Length of top roll, mm
F Fractional fibre content of the discharged
bagasse

The set opening is that which exists between the two rolls when they are at
rest, with the mill empty. It is the set opening that the mill artisan has to
apply to the rolls at the beginning of the season.

Because of the geometry of the rolls, the relationship between the work and
set openings is given by the formula:

K,y ,,,k - 0,8 x Roll Lift-

Figure 15. Measurement of MY opening

The roll lift is usually expected to be 1Omm, so there would be a difference in

the above figures of 8mm.

36
The opening is measured between the average diameters of the two rolls,
making an allowance for the grooved surface. Physically the measurement
is probably easiest from the tip of the top groove to the root of the bottom
groove. This is illustrated in figure 15.

The value of F is a matter for the engineer to determine through experience.

Mills that have been crushing for several years will have collected a history
of mill settings that would be used to determine F for each mill at the
beginning of a new season. For a six-mill tandem, the following target Fractional fibre
content of the
values for mills 1 to 6 respectively are given as a guide: 0,30; 4,39; 0,43; bagasse
4,46; 0,48 and 0,50 (van Hengel of al, 1958).

The work opening between the top and feed rolls (FWD) is calculated by
applying a ratio to that o£ the discharge work opening calculated above.
Again the choice o£ this ratio is a matter for the engineer to determine
through experience, but a figure of 2,0 is usually regarded as a good starting
point.

The setting of the underfeed roll work opening and that of the width of the
Setting ratios
Donnelly chute at the entry to the mill is covered in the paper by van Hengel
(1964). These settings are also calculated using ratios of the DWO as given
in Table 2:

Table 2. Settings ratios for a six-mill tandem:

Mill No. Rl Rx
1 7,0 1 l,0
2 6,6 ~_
3 6,2
4 5,8 9,2
_ 56. . ._ r 5,4 ~_ 8,6
5,0 8,0

Here the underfeed roll setting = Rl x DWO, and the Donnelly chute width
= Rz x DWO.

The trash plate setting is carried out with fairly simple geometry, but is best
Trashplate
done full size on a drawing board, or if a good CAD programme is available,
Setting
it can be done with a computer. This technique is best illustrated by means
of the sketch in Figure 16.

The circles representing the average diameters of the three rolls are drawn on
a large sheet of paper in their correct working positions. The centre of radius
for the trash plate `A' is determined by moving a distance `D' from the
centre of the top roll on the horizontal axis. The position for the toe of the
trash plate is determined by the intersection of the feed roll diameter and a
radius of the feed roll 13° in a clockwise direction from a line joining the

37
 centres of the top and feed rolls. The trash plate radius is then drawn from its

TOP ROLL (in

working position)

Figure 16. Sketch of setting of trash plate

centre, starting at the point of the toe and ending at the discharge roll. The
trash plate section can then be completed, and the sharpness of the toe can be
removed as shown in the scrap detail. The rear of the trashplate should have
a clearance starting at about 20mm to the tip of the discharge roll grooves.

The value of `D' is calculated from the formula:

D = PI100x (R+S)
Where P = % drop over length of trash plate, normally 4 or 5%
R = radius of the top roll, mm
S feed roll setting, mm

38
1&CAPACITY CALCULATION

The capacity of a milling tandem is influenced by the following factors:

1. Fibre content of the cane

2. Dimensions and speed of the rollers
Factors affecting
3. Number of rollers capacity o! WAS
Cane preparation
5. Imbibition
6. Grooving and the effect on drainage
7. Hydraulic pressure
8. Roller surface
9. Feeding devices
10. Design and condition of the mills
11. Personnel - control of mill, and evenness of operation

Capacity has been shown to be primarily related to the total roll volume of
the mill. This applies only on the assumption that the extraction performance Total roll
is maintained at an acceptable level. For example it would be easy to double volume (rRV)
the capacity of a tandem if the performance was allowed to decrease
considerably.

A capacity survey of South African mills shows that the dependence on roll
volume holds reasonably well for milling tandems, but is too erratic for
diffusers. Other factors must therefore be considered for the determination of
diffuser capacities.

A number of empirical formulae for capacity exist, the preferred one being
that from Hugot (1972):

A= 0,022cnLD2 (1-0,018nD)'sk
f

Where A = Mill capacity in ton cane per hour

c = coefficient of preparation
(c =1,1 for poor PL and
c = 1,22 for good PI)
n = speed of rotation
N = number of rollers in the tandem
D = diameter of the rollers, m
L = length of the rollers, m
f = fibre content per unit of cane.

This formula is correct for a speed of 5 rpm. For any speed n' other than 5
rpm, multiply by n' x (1-0,018n'D)1(5 x (1-0,09D))
 It should be emphasised that performance and capacity are intimately linked
and any claim to capacity ratings must be accompanied by a statement of the
expected performance.

19. POWER CONSUMPTION

Measurements have been carried out many times by several people, (see Reid
Power
measurements and Wienese, 1985) in which accurate methods of torque and speed
using torque measurement were used. Torque measurement is best done by using strain
gauges and a telemetry link between the rotating shaft and the receiving
instrument. It is usually placed on the square tail bar so that only the mill
bearing friction needs to be allowed for in determining the torque on the rolls
of the mill.

Power consumption is between 9 and 12 kW per ton of fibre per hour. The
loss of power in the reduction gearing is close to 20 °Io.

The first and last mills are usually arranged to carry out more work than the
Power intermediate mills. The first mill is required to remove a major portion of the
Consumption of
different mills
sucrose, and it is generally accepted that a high first mill extraction is
essential to good overall performance. The last mill is required to give a low
bagasse moisture which in turn will assist in keeping the extraction high, but
is also important for good boiler performance. The power for first and last
mills is thus 11 to 12 kWltfh, while that for intermediate mills is usually
below 10.

Various formulae have been proposed to allow the calculation of mill power
Power
consumption. The power consumption is in two parts, friction and rubbing
conusmption between the components of the mill, and the forces of milling caused by
formula
compression of the bagasse in the working mill.

A formula has been proposed by Hugot (1985) which adds the compression
and friction factors. The formula given in his book allows for the
compression in one "nip" of the mill, whereas this writer believes that the
compression in both the feed and discharge nips should be added.

The whole formula would then be:

P = nD/O (F(Re + 0,075) + 4L)

Where n =rpm
D = roller diameter, m
- gearing efficiency
F = hydraulic load of the mill, tons
R = reabsorption factor
_ (6r-5)1(gr(I+Ar-1)))
r = reabsorption index

40
 e = settings factor
= 4,3 (4(ef+ ed))
of = specific opening ofthe feed gap
= opening/diameter
ed= specific opening of the discharge gap
= opening/diameter
L = roll length, m

20.THE PERFORMANCE OF MILLS

In general terms, the most important factor for the engineer to apply to his
mill is "TLC" - Tender Loving Care. A sugar mill will respond remarkably to
intelligent and common sense care in all areas. It just requires attention to
detail and adequate keeping of records.

The following list of factors is provided as a basis to assist the engineer in

applying this attention to detail.

24.1. Fibre Content

The milling tandem is handling a composite material, consisting of fibre,

Fibre •. cane
juice, sand and extraneous matter such as rocks, tramp-iron and trash. The
higher the fibre content relative to the total, the lower the juice that can be
extracted, because the mill is sized for a certain volumetric throughput of
total cane. This is recognised in the mill control variable known as
"Corrected Reduced Extraction", (CRE) which gives a value of mill
extraction modified to allow for the effect on the performance of the mill by
differences in fibre and poi contents of the cane. This formula is given in a
previous section.

20.2. Length of the Tandem

As a general rule, the more times the cane is squeezed, the greater will be the
Extration
extraction of the tandem. Thus a 7 mill tandem should give a higher depends on
extraction than a 5 mill tandem. number of
squeezes

Hugot(1972) has proposed a formula based on the number of rolls in a

tandem, which is very empirical, but which will serve to illustrate the point:
Extraction is given by:

E = 100 - 7o/N

where N = the number of rolls in tandem

 20.3. State of Cleanliness

Spillage of juice and cane, and leakage from the mill into inaccessible areas
Mill hygiene is a source of direct loss of sucrose, and also sucrose destruction due to
inversion and bacterial activity. These losses are difficult to detect by the
normal methods of milling control, but they will reveal themselves by smell,
and by the slimy appearance of parts of the mill caused by "Leuconostoc
mesenteroides" bacteria. The determination of lactic acid, a by-product of
bacterial activtiy, can be used.

Regular inspection of the mills to detect leaks and sources of spills is

essential. Also, regular steam and hot water cleaning should be carried out.

Bactericides are available, but are expensive, and should only be used when
the other methods have failed.

20.4. Load Application of the Mills

Roll pressure The pressure exerted on the cane in the roll nip has a direct bearing on the
amount of juice squeezed out of the bagasse in each mill.

Of course the maximum pressure is limited by the strength and the design of
the mill, but it is important to maintain pressures as high as feasible, as long
as the top roll runs in its "floating" position. This has been more extensively
covered in section 8 on mill pressure.

20.5. Mill Roller Speed

Roll surface
The drainage of the bagasse in the mill is time dependent. Thus, an increase
speed in mill speed would shorten drainage time for the same blanket thickness,
and extraction would thus decrease. Normally, the slower the speed, the
better the performance.

However, in some circumstances, an increase in speed will slightly improve

extraction, but only if conditions prior to the speed increase were
unfavourable to feeding or roll lift or one of the other factors.

20.6. Uniform Feeding

Good mill performance depends on the maintenance of uniform conditions in

each mill.

Steady running
Firstly, the moisture of the bagasse entering each mill must be fairly constant.
If the flow of juice from one of the mills should be interrupted, the imbibition
effect will be lost. This could easily happen if the feed to the first mill was
highly variable; The squeeze in subsequent mills would create a disturbance
which would be accentuated down the tandem, and ideal conditions would be
temporarily suspended.

42
Secondly, the blanket of bagasse going through the mill should have the
minimum of voids, which could interfere with drainage and cause
momentary reabsorption.

Uniform feeding is assured by automatic control as described below. In older

mills where uniform feeding depends on manual operation, the operators
should be well trained to maintain an even chute level at each mill.

20.7. Imbibition Rate and application

it was shown in the section on imbibition that extraction depends on the rate
at which water is added to the bagasse before the last mill in the tandem. An
increase in imbibition will lead to an increase in extraction provided that
other factors such as cane preparation, roll roughness and drainage are
optimum.

The efficiency with which the imbibition is absorbed by the cane must be Imblbltlon rat&
maintained at as high a level as possible. Shredded cane or bagasse can affects
extractlon
absorb from 5 to 10 times its weight of water. Thus even very high
imbibition rates do not saturate the bagasse. However it is important that the
imbibition be distributed on the bagasse either by sprays, or as is more
commonly applied, in a thin film across the width of the intercarrier. This is
achieved by arranging a trough with an overflow weir spanning the carrier,
into which the imbibition is pumped. Baffles are arranged in the trough to
prevent excessive turbulence, and to ensure an even flow over the weir.

20.8. Cane Preparation

Since this subject was covered above, it will suffice to say that improved
cane preparation, as measured by "Preparation Index" will improve mill
extraction more or less in proportion,

20.9. Correct Mill Settings

The setting of the openings between the rolls of a mill and the position of the
trash plate, as detailed in the previous section, are of prime importance to
ensure that the mill performs as it was originally designed.

20.10. Roll Surface Condition

As the season progresses the rolls wear at a fast rate determined by the
amount of sand and soil that inevitably comes in with the cane. The effect of
this wear is to polish the roll surface causing slippage or "reabsorption" and it
reduces the ability of the rolls to feed.

To compensate for this wear and prevent slippage the roll surface must be
maintained in as rough a condition as possible. This roughness must have

43
 "hill/valley" dimensions measured in mm rather than microns, and must be
able to resist wear.

Because the roll shells are made of cast iron, they tend to have a naturally
rough surface, and until the 1970's a technique known as "arcing" was
applied in which a carbon electrode connected to an arc welding machine
was applied to the roll surface. This had the effect of combining the iron and
carbon into small globules of iron carbide which adhered to the roll and
provided a measure of roughness. However, for modern milling, this
technique was far from adequate, and the surface of the roll is now
roughened by a welding technique using high hardness electrodes at high
amperages. It is still called "arcing". A special welding rod was developed
for this purpose in Australia in the early seventies, known by different code
names. In South Africa the more popular make is called "CR70". It contains
a high proportion of chrome, and various other elements to improve its
adhesion to cast iron. If the arcing is carried out satisfactorily, the surface is
covered with globules of weld material, which are extremely hard, adherent
and able to resist abrasion.

Arcing is applied while the mill is running, and the newer mills are
specifically designed to facilitate this operation with the minimum of
discomfort for the welder. The roots of the grooves are left smooth in order
not to interfere with the juice drainage path.

20.11. Drainage

The importance of adequate drainage from the high pressure region in

between the rolls must be emphasised very strongly. Any blockage of the
drainage path which consists of the root area of each groove and the
Messchaert grooves will adversely affect the performance and should be
avoided.

One method which is being reintroduced by many mills in South Africa is to

reduce the pitch and angle of the grooves, particularly on the last two or three
mills of the tandem. If 25 mm pitch is used instead of 50, the number of
drainage grooves is doubled, and a smaller angle will increase the cross-
sectional area of the drainage path.

20.1.2. Proper Operation of the Mil!

Attention to
In this section, it is necessary to summarise those areas of mill operation
detail and good which need to be continuously monitored to ensure proper operation of the
records mills:

Uniform feeding of each mill

Sufficient pressure on top roll, but roll must "float"
No by-passing o£ juice in imbibition stages
Imbibition to be properly applied to the bagasse
Roll roughness to be maintained
Mill settings to be regularly monitored
Maintenance of shredder and knives in good condition

In order to ensure proper operation, it is essential to maintain adequate

records of all the variables pertaining to the mill. Weekly checks of mill
settings, shredder and knife condition, and many others should be kept on
record, and compared with the performance achieved.

20.13. Efficiency Indicators

Murry and Holt (1967) have presented the results of several years of research
into the mechanics of the crushing of sugar cane that was carried out at the
Sugar Research Institute in Australia.

They have suggested several ideas or concepts that affect the efficiency of
milling that are worth adding to this list, and the student could benefit from a
deeper study of the subject. Several subsequent papers have continued to
report on this work notably Edwards (1995) and Kent (1997), in which the
concepts are further explored and refined.

Briefly, the indicators are:

Reabsorption
factor
Reabsorption factor = Vb / Ve

Where Vb Volume rate of the delivery

bagasse from the mill
And Ve - Volume escribed by the top
and delivery rolls of
the mill in unit time

This phenomenon may be described as the reabsorption of juice by the

bagasse blanket as it is allowed to expand after the nip between the rolls. It
can be prevented by good drainage and by ensuring that slippage between the
bagasse and the rolls is eliminated. It could also be called the forward slip
factor. A formula is given in Hugot (1972) by which the reabsorption factor
may be calculated. Since it is a function of the peripheral speed of the rollers
and of the fibre index, the formula is written -

r - Z + 0,0171 v + 0,000624

Where Z = Constant for each mill,

0,75 for the first mill
0,65 for the second mill
4,60 for subsequent mills
v = Peripheral speed of the rollers, m/minute
= Fibre index, kg per cubic m.

45
 = weight of f bre passed through the opening
escribed volume of the opening

The values obtained from this empirical calculation should not be used as
indicators of current performance. For this purpose, the reabsorption
factor derived from actual measurement would be better. However, the
actual volume of material passing through the mill is difficult to measure
continuously, and thus the factor can really only be calculated when the
cane weights from the weigh-bridge become available. Also, single
measurements of the roll lift will give unreliable calculations of escribed
volume. A recording of the roil lift would be preferred for this purpose.

Imbibition Coefficient is a measure of imbibition efficiency which

Imbibition
coefficient has been mentioned above, and also in the section on extraction using
imbibition. It is defined as the ratio of the actual brix extraction at a mill
and the brix extraction that would result if the imbibition liquid and the
juice in the feed bagasse mixed perfectly at that mill. This can be
i mproved by good preparation and by careful application of the imbibition.

First mill extraction. Another important performance

First mill
measurement is the extraction of the first mill, or the dry extraction portion
extraction of the total. This can be calculated from the pol or sucrose in mixed juice,
first mill juice, second mill juice and the extraction of the tandem. It is
difficult to obtain good samples of the juices from the first and second
mills, but with suitable equipment, or frequent and careful sampling, it can
be done. Care- must be taken not to mix returning juice from the screens
with the first mill sample. The formula for first mill extraction attributed
to Stuart is:

FME = P_i(Pq. P) x E
NP 1 - P2)

Where P,p - Pol % mixed juice

P1 = Pol % first mill juice
P2 = Pol % second mill juice

It should be noted that "vet" extraction using imbibition applies only to

the second and subsequent mills, and acts on the brix remaining after the
first mill. The lower this brix, the greater will be dilution effect of the
imbibition, and the higher will be the extraction. Thus, F ME is extremely
important.

Another measure of mill performance is the brix curve, plotted from brix
measurements taken for each mill of the tandem. This, and FME require
the discipline of taking juice samples from every mill of the tandem as
many times as are possible every day, preferably twice per shift.

46
21.CONTROL AND INSTRUMENTATION

The following mill variables are usually displayed on the mill control panel,
or are at least visible to the operator.

For the cane conveyors and cane preparation

Conveyor run/stop indications and amperages
Knife and shredder drive amperages, or steam pressures and speeds
Control variables and settings for the conveyor controls

For each mill of tandem

Mill speed
Donnelly chute feed height
Roll lift
Hydraulic pressure
Steam pressures and temperatures
Turbine nozzle box pressure
Pump and conveyor motor amperages

For the whole tandem

Imbibition water flow and temperature

If electric motors are used instead of turbines, the drive amperages and other
important variables need to be displayed.

The crushing rate is usually set by the speed of the first mill, and the feed
conveyor is then controlled by the feed height in the first mill Donnelly
chute, which is measured by a row of conductivity sensors. This is described
in more detail above in the section on the control of the cane conveyors.

Subsequent mill speeds are controlled by the feed height in each of their
respective chutes, also measured by means of a row of conductivity sensors
in the Donnelly chute.

Where a pressure feeder is used, it is possible to monitor the internal

pressure, and to use it as an indication of the feeding efficiency of the mill.
Or the pressure chute can be protected by warning of an increase in torque.
Torque can be measured either directly using strain gauges, or by dividing
nozzle box pressure on the turbine by the speed.

Various attempts have been made to measure the quantity of fibre passing
through the mill at any instant but without much success. This measurement
would be very useful, as it would provide means of calculating the
"reabsorption factor" which is described elsewhere. The other variables
required in this calculation are roil speed and roll lift, which can be easily
measured at present.

47
 BIBLIOGRAPHY

Anderson, SI and Loughran, JG (1999) Mill roller design and operational stress states.
Proc Aust Soc Sugar Cane Technol 21: 301- 306

Anon (1985) Laboratory manual for South African Sugar Factories. S Afr Sugar Technol.
Ass. Durban. P238.

Beale, RF and Jamieson, R (1993) Mill drive gears - more sophisticated approaches? Proc
Aust Soc Sugar Cane Technol 15: 71-76

Buchanan, EJ, Douwes-Dekker, K and van Hengel, A (1965) Mutual Milling Control
Project - Progress report No. 4. Proc S Afr Sugar Technol. Ass 39: 85-95

Coates, D (1994) A review of cane conveying systems. Proc S Afr Sugar Technol. Ass 68:
1 56-158

Crossman, MT (1994) A review of modified shredder systems. Proc S Afr Sugar Technol.
Ass 68: 166-168

Edwards, BP(1995). Extraction performance of milling trains - imbibition processes and

calculations. Proc Aust Soc Sugar Cane Technol 17: 346-351.

Gradener, A (1964) Comparison of various electric drives suitable for cane crushing mills.
Proc S Afr Sugar Technol. Ass 38: 74-77

Gradener, A (1973) Report on an automatic control system for sugar cane carriers employing
thyristor-fed DC drive motors. Proc S Afr Sugar Technol. Ass 47: 106-108

Hughes, DL (1964) Sugar mill drives. Proc S Afr Sugar Technol Ass 38: 66-73

Hugot, E (1972) Handbook of cane sugar engineering. Elsevier, Amsterdam.

Jorgensen, GM, Johnstone, JA and Cant, CC (1986) The application of high-torque low-
speed hydraulic motors in the sugar industry. Proc Aust Soc Sugar Cane Technol 8: 269-278

Kent, GA (1997) Modelling the extraction processes of milling trains. Proc Aust Soc Sugar
Cane Technol 1 9: 315-321

Moor, B SIC (1974) An evaluation of very fine shredding. Proc Int Soc Sug Cane Technol.
15:1590-1601

Moor, B SIC (1973) The Tongaat shredder. Proc S Afr Sugar Technol. Ass 47: 100-105

Moor, B SIC (1994) Review of cane shredding. Proc S Afr Sugar Technol. Ass 68:162-165

Moult, JM (1980) Performance testing of wear resistant materials used on shredder hammers.
Proc S Afr Sugar Technol Ass. 54: 40-44

Murry, CE and Hoit, JE (1967). The mechanics of crushing sugar cane. Elsevier,
Amsterdam.

48
Partridge, JR (1978) Sugar Mill Gearing. Proc Qd Sac Sugar Cane Technol 45: 349-358

Raffray, R (1986) Hydraulic drives for a Mauritian cane mill. Int Sugar Journal Vol 88, No
1050:110-112

Reid, MJ (1994) Review of cane knifing. Proc S Afr Sugar Technol Ass. 68:159-16l

Reid, MJ and Hartie, AGJ (1994) A method of measuring cane preparation index using a
computer. Proc S Afr Sugar Technol Ass. 68: 133-136

Reid, MJ (1988) Analysis of the causes of recent roll shaft failures in Natal sugar mills. Proc
S Afr Sugar Technol Ass. 62: 74-78

Reid, MJ and Wienese, A (1985) Use of strain gauges in the measurement of pressure
feeder torque and internal chute pressure. Proc S Afr Sugar Technol Ass. 59: 83-88

Renton, RH (1974) A preliminary survey of power requirements for cane preparation. Proc
Int Soc Sug Cane Technol 15, 1575-1581

Shield, AG and Cant, CC (1995) A new hydraulic drive unit for a 2,13m crushing mill.
Proc Aust Sac Sugar Cane Technol 17: 332-338

Tosio, CT (1988) A new sugar mill drive coupling_ Proc S Afr Sugar Technol Ass. 62: 70-73

Van Hengel, A_ (1964) Suggestions for the setting of vertical feed chutes. Proc S Afr Sugar
Technol Ass. 38: 33-36

Van Hengel, A and Douwes Dekker, K (1958) Some notes on the setting and operation of
mills. Proc S Afr Sugar Technol Ass. 33: 57-65

Wienese, A (1995) A milling review. Proc S Afr Sugar Technol Ass. 69:192-195

Wienese, A and Reid, MJ (1997) Soil in cane: its measurement, its effect on milling, and
methods of removal. Proc S Afr Sugar Technol Ass. 71: 130-134
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation: The fundamentals
6 Evaporation: The practice
7 Pan boiling I
8 Pan boiling II
9 Dif sion
I fl Refinery carbonatation
I I Milling

In preparation:-

Boilers
Sulphitation
Phosphatation
SULPHITATION
Sugar Technology For Students

SULPHITATION

Prepared by G R E Lionnet

Study Text 12

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 2001

Copyright 0 2001 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISSN 0-620-27293-7

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 SO2 and
SULFITES
CHEMISTRY
RESIDUA
S02

REACTIONS

J
LIIVIE SUGARS
BEET
SOLUBILITY'S COLOUR
 1. INTRODUCTION

Sulphur, which is burnt to produce most of the sulphur dioxide gas used in Sulphur
the various clarification or decolourisation processes of the sugar industry, is
considered a major chemical of the industry. In Southern Afr ica many
refineries use sulphur dioxide as a secondary decolourisation chemical. It was
Sulphur dioxide
used extensively in the Natal raw sugar industry up to the mid 1950's, but was
then abandoned basically because of chemical costs and because of severe
scaling in heaters and in evaporators. It is still used extensively in many cane
processing countries, such as India and Colombia to produce what is termed
a mill white sugar.

In the beet industry sulphur and sulphur dioxide are not very important
chemicals. This is made clearly evident when the beet literature is reviewed; Beet
there is an abundance of information, both theoretical and practical on carbon
dioxide and carbonatation for example, but this is not the case for sulphur
dioxide

There is however a large body of information from the chemical literature, Food and beverages
more particularly that which covers foods and beverages. This information has
probably not been well utilised in the sugar industry.
 2. CHEMISTRY

2.1 Sulphur
Brimstone
Sulphur, called brimstone (bryne : burning in old English) by the ancients, is
found underground as a brittle, yellow, non-metallic element.

It can be prepared from some of its compounds (SO 2, sulphides, sulphites,

etc.) and is present in natural gas, petroleum and coal.

Four isotopes (iso : Greek for equal; topos : Greek for place, here in the
Isotopes
periodic table) of sulphur are known. Isotopes have atoms whose nuclei have
the same atomic number but different mass numbers; thus, the nuclei have the
same number of protons but different numbers of neutrons. With sulphur we
have .-

MASS
NUMBER

s s
NUMBER

16 a Isotopes OF S

ATOMIC

The first isotope listed above (S32) shows a natural abundance of 95%.
Generally all isotopes, for any one element, have virtually identical chemical
properties and their relative proportions are essentially constant everywhere
the element is found on earth. The element generally behaves as though its
atoms had a mass equal to the average. In the case of sulphur the proportions
of the isotopes does vary more at different locations, than for most common
elements.

Sulphur also exists as a number of different allotropes ( allotropos : Greek for

Allotropes
another form). Allotropes are different molecular or crystalline farms of the
same element. Four sulphur allotropes are common :-
 Two common allotropes are different crystalline forms of
cyclooctasulphur, S8, namely orthorhombic and monoclinic sulphur. Both are
crown like.

Crown form of s,

The density of orthorhombic sulphur, a common form, is 2.06 g/cm3 .

f An amorphous, plastic sulphur.

0 Liquid or molten sulphur.

For simplicity we use S rather than S8.

When heated, so as to break the S-S bonds in S 8, sulphur can be made to Reactivity of S6
combine directly with all the elements, except the noble gases, gold, platinum,
nitrogen and iodine.

2.2 Sulphur dioxide

Joseph Priestley, an English scientist, prepared S0 2 in 1770 using mercury as

reducing agent

Joseph Priestley
Hg + 2H 2S04 => HgS0 4 + S0 2 + 2Hz0

Both environmentally and economically the most important reaction ofsulphur

is with oxygen to produce gaseous sulphur dioxide
 SO 2(g)
+ 0 2W =>
S (s)

At 250 to 260 ' C, sulphur ignites and burns with a bright blue flame to give
gaseous sulphur dioxide. The heat of combustion is 9.2 kJ/g.

Sulphur dioxide has a sharp, acrid and choking smell. It readily liquefies; at Physical properties
atmospheric pressure and -10 'C, it will turn into a liquid. It freezes at -72 °C,
to a white solid.

It dissolves in water by forming hydrates, S0 2.nH20, where n varies with

concentration, temperature and pH. The hydrates are in equilibrium with the
hydronium ions (H 3O+) and hydrogen sulfite ions HS03+, whose presence has
been explained simply in terms of H 2SO3 (.,,) or sulphurous acid. Actual
molecules of H2S03 have never been detected in or out of water. For
convenience we still write H2S03 and the traditional first ionisation of
sulphurous acid

H2SO3(aq) a H + (aq) + HSO3 (aq)

lonisationa

should really be written as

SOz.nH2O <* H3O+(aq) + HSO3(aq)

while the second ionisation is

HS03(aq) a H+(aq) + S032-(aq)

HS03 does exist in solution.

Again using the convenient H2SO3 simplification we can write

H2SO3(aq) e* H + (aq) + HS03(aq)

with an ionisation constant, K,, equal to 1.2x10 - at 25'C, and

HSO3(aq) <* H+(aq) + S032-(aq)

x, and K2
with K2 equal to 6.6x10 -8 at 25 'C.

The values of K 1 and of K2 show that sulphurous acid, although classified as

a weak acid, is a relatively strong acid- It is much stronger than carbonic acid
(relevant to liquor or juice carbonatation) which has K, = 4.5x10' at 25 °C.

We see that K, is much larger than K 2 , a property of most diprotic (two H+

ions per molecule) acids. The reason for this is that an H" is lost more easily
from a neutral molecule than from the HA - ion, where the negative charge
inhibits the second ionisation.

Ionisation constants, dissociation and pH can be used to investigate equilibria

in aqueous solutions. A number of simplifying assumptions are needed as we
consider the following systems

S0 2 + H 2 O a H 2 S0 3 System: sulphur dioxide

in water

H2S0 3 a H+ + HS03 ........KI

+ So
<::> H+

HSO3 32 K,andK2maybed finedasfol ws

[H + ] [HSO3-
K, ..................(1)
[H,Sq3]

[H + J [SO3 2- ]
Kz ....................(2)
[ HSO 3- 1
Where the [ ] represent concentrations.

From (1)

~H iSO 3
+ ................. (3)
H Ki x
HSO3'
I

Dissocoation ratio
We define a dissociation ratio, a, as

number of dissociated H 2 SO, molecules definition

a
total number of H M SO, molecules

Let the total number of H 2 SO3 molecules be A. Then, at equilibrium

H 2 SO 3 <z> H } + HSD3_

and, the number of undissociated molecules = A - aA

the number of H+ molecules - aA
the number of dissociated H2SO3 is - aA

or

I H2SO3] - A(1-a)
[HSO ' - ] aA

in (3) .

~H - K, x 1 a ...................(4)
a
We know that pH is a function of [H']. Thus (4) gives us a relationship
between pH and a, for a given value of K, .

For an aqueous system, at 25'C, the literature gives the following relationship.

Reiatiouship between
dissociation and pH
c
0
a
b
vv
ae
a

.2 0 2 4 B 8 10
pH

For the above system, namely an aqueous solution at 25 'C, the following
points may be made.

0 At a pH of 9.5 and above, only 50 32" can exist.

0 Over the pH range 9.5 to 4.5, both S032- and HS03 can exist; the
interpretation
concentration of HS03 will increase as the pH approaches 4.5.

0 At pH values of 4.5 and lower no sulfite can exist.

2.3 Sulfites

Sodium sulfite (Na2S0 3) is the most important sulfite Large amounts are used
in the manufacture of paper pulp. A small amount is used in foods, to prevent
bacterial effects.

It can be prepared as a salt, either as the anhydrous form or as the

Various sulfites
heptahydrate, Na2S03. 7H20.

Sodium bisulfite, or sodium hydrogen sulfite, Na 2HSO3, is often Na2S205, also

called sodium metabisulfite. In an acidified solution Na2HS03 and Na2S205
are chemically equivalent because of the equilibrium

S2052
2HS 03(aq) tv tav + H2O
2.4 Reactions between time and sulphur dioxide

These will be discussed for aqueous solutions. Two specific cases are
considered, namely the addition of sulphur dioxide to an aqueous solution
Ca(olj), + SO,, in water
containing calcium hydroxide, and the addition of a calcium hydroxide slurry
to a solution of sulphur dioxide in water. Again simplifying assumptions will
be made.

2.4.1 Addition of sulphur dioxide to an aqueous solution of calcium

hydroxide.

In the aqueous medium a small amount of Ca(OH) z dissociates as Ca" and

OF and the pH is around 12.6 at 30 'C.

2
When S02 is added, H2S03 is formed, dissociating to H+ and S03 ", as
indicated in the figure on page 7, at the high pH values. As soon as the
product of the concentrations of Cat+ and of 50 32' reaches a value greater than
the solubility product, Ksp, CaS0 3 precipitates.

Ca (OH) 2 (,q) a Ca 2+ (,q ) + 20H - (aq) .............. (i) SOLUBILITY PRODUCT:

equations sad definitions

as a sideline far
information
CaS03(=q) q Ca. t+ (•q) + so 3 z (sq) ... ... . .. . . . . (U)

K = [ Ca"(,q) l [OH (,q) l 2 = 6.5 x 10-6 at 25° C

sp

KSP = f Ca 21(,q) l IS03 2 (•v l = 3 x 10' at 2Y C

OH from Ca(OH)2 and H' from H2 SO3 form water and the pH drops. More
2"] is equal
and more CaS0 3 precipitates until the product of [Ca?' ] and [S0 3
to the KP value and the precipitation is complete. We can represent these
reactions as

Ca(OH)2 Cat+ + 20H

S02 + H2 0 r H2S03

H2SO3 21r+ S032-

 Ca' + S032" ;iF' CaS0 3(5)

20H" + 2H' 2H20

The original concentrations of some of the ions are very small (eg Ca2 ' and
OH), but as ions are removed from solution by precipitation the reaction
moves to the right and more reagents are transformed. The net result is

Net result
Ca(OH)2 + H2SO3 CaS0 3 + 2H20

If further S0 2 is added after the neutralisation of Ca(OH} 2 is complete the pH

moves further towards the acidic side in the figure on page 7. H,S0 3 then
dissociates according to the second curve and more HS03 goes into solution Excess so,
while the concentration of SO3 2- decreases. But the system tries to keep the
concentration of 503x" at a level dependent onthe solubility product of CaS0 3
and this can only be done by the solid CaSO 3 dissociating into Cat' and
5032 "; this is shown below.

Reacting system
S02 + H2O r H2S03

H2 S03 2H' + S032-

CaSO3( ,
q) Cat- + 5032

SO 32- + H+ HS03

CaS0 3(,) CaS0 3(,,)

the net result being

Net result
CaSO3(5) + H2SO3 ~ Ca2" + 2HS03

and since the Ca(HS0 3) is soluble, calcium goes into solution.

2.4.2 Addition of lime to an aqueous solution of sulphur dioxide

The initial pH is now low, being around 2, and reference to the figure on page
7 shows that the solution will contain undissociated H2 SO3 and HSO3 ions.

Cat' and OH- are now added. The Cat+ ions react with HSO3 , OH' combines
with H+ to form water and the pH rises. Thus more and more HSO3 goes into
equilibrium with Ca" until all the H 2 SO3 has been split into HS03 and
H'.Then half the neutralisation is complete and the solution contains the
soluble bisulfite.

Further addition of lime increases the pH and brings SO,' - into solution. As
soon as the product of the concentrations of Cat' and 50 3 2" is above the
solubility product, CaSO 3 precipitates. The precipitation is complete when the
concentration of SO,'- is small and the solubility product is not exceeded. The
following equations represent the first neutralisation:

Firit neutraisation

SO 2 + H 20 H2S03

2H2SO3 IT- 211+ + 2H503-

Ca (OH) 2 Ca2+(-q) + 20H-

211+ + 2011' 211 20

which simplifies to

2H2 SO3 + Ca (OH)2 Ca(HSO 3) 2 c.,) + 2H2O First main reaction

The second set of reactions is

Ca(HS03 )2 Cat' + 2HSO3

.
iq
Ca (OH)2 tsf Cat+ ) + 2O11

2HSO3 211+ + 2SO3z-

-10-
 2H} + 2011 2H20

or

Ca(HSO 3)2 + Ca(OH)2 'Ir- 2CaSO3t5, + 2H20 Second set of reactions

Combining both sets gives the overall result :-

Combined results
H2S03 + Ca(OH)2 'q- CaSO,, ) + 2H20

2.5 Solubilities of salts of sulphurous acid

Data on the solubilities of calcium sulfite in water and in sucrose solutions are
not readily available. Chemical literature gives the solubility of CaS0 3.2H 20,
at 18°C to be 0.004 g per 100 g of water; at 90°C it is 0.002 g per 100 g.
Other sources give the results shown in the following figure, where the
sucrose solution contains 15% (rnlrn) sucrose.

Solubility of calcium sulfite

in water and iu 13% sucrose
solution

20 40 60 80 100
Temperature [°C]
These results indicate that the solubility of calcium sulfite decreases as
temperature increases. Calcium hydrogen sulfite on the other hand is readily
soluble. Finally, the various sodium salts of sulphurous acid are usually
soluble.

2.6 Colour

In the cane sugar industry sulphur compounds are used mostly for the removal
Sulphur dioxide and colour
of colour. It is therefore instructive to study the chemistry of some of the bodies
colour bodies which interact with sulphur dioxide and other sulphur
compounds.

2.6.1 Enzymatic browning

Phenols are organic compounds which have one or more OH groups attached
Phenols
directly to an aromatic ring. The simplest of these compounds is phenol itself
with one OH group attached to a benzene ring: -

ox

Phenol

A number of more complex phenols are found in cane and cane juices. The
subject has been reviewed by many workers (Lionnet,198S; Smith, 1982;
Smith et al., 1971, 1981; Godshall and Roberts, 1982); they show that cane
contains many complex phenols such as flavonoids, flavonols, chlorogenic
and caffeic acids, catechol, etc. Caffeic acid and catechol, two typical phenols,
are shown below.

-1 2-
 C- C
Ug CA ff. i t Acid

on

off

CAtechol

Flavonoids (Smith, 1982) are more complex and can account for a large Flarovoid

proportion of the colour in cane juices and in sugar_ A typical flavonoid

structure is shown below.

- 1 3-
 Trivia sad spogenin

HO

When R1 and R2 consist of the OCH, group, the flavonoid is called, tricin;
when RI and R2 consist of an H atom, we have apigenin.

Enzymatic browning is a process through which a phenolic compound, which A pituol is oxidised to
can be colourless or coloured, is oxidised, through one or more steps, to yield tolourtd products

coloured products. The rapid browning of a cut apple or potato, when

exposed to air, is an example of enzymatic browning. The basic reaction which
requires an enzyme, was discovered by Bertrand in 1895. It can be represented
in a simplified way as follows.

-`" G
Phenol o' ~ Diphenol 0'-+ Ketone ----+ Enzymatic browning
-Amino acids, Proteins
Diketone -+ polymers ............... (1)

where the diketones are coloured and the polymers are dark brown.

In a simple case

- 14-
 $ompk en"atic
browning reaction
CATHECOLASE

0,

CATECHOL {calourkas) O-QUINOIVT (coloured)

These oxidative reactions are brought about by enzymes called PHENOLASES Phenolases
or POLYPHENOL OXIDASES. They facilitate the conversion of the phenolic Polyphenol oxidaes
compound to quinones (cyclic di-ketones) which are coloured. Phenolases are
widely distributed in fruits and vegetables.

It is instructive at this stage to consider enzymes. An enzyme is a protein that Definition

catalyses a biological reaction. Proteins in turn are biological polymers of small

molecules called amino acids. Proteins can be very large molecules (molecular
weight 6000 to 250000), and may also contain non-amino acid components
such as metal ions (for example Fe 21 , CU" Mg"), or such as complex organic
molecules.

Amino acids contain an amino group, namely -NH,,, and a carboxyl group, Amino acids

namely -COOH. The building blocks of proteins are alpha amino acids (a-
amino acids), where the NHz group is on the carbon atom next to the COOH
group, that is the a-carbon atom. The simplest a-amino acid is glycine. The
general structure of a-amino acids and of glycine are shown on the next
page.

- 1 5-
 Structure of s mibo acids
H O
1 11
R---C -C-a-H
NH,

A
Glycise k R-H
H - C- COON
I
NH,

Iopsel of iron
Colour can also be produced through a different pathway. Thus in (1) on page
14, the di- or polyphenol can form complexes with Fe(M) ions, which show
deep green, red, blue, brown or blue-black colours.
Phenalnsea in csne
Finally, in living tissues, the phenols and enzymes are separated within the
cells_ When the cells are broken, as in the cane extraction process, they come
in contact, react and generate colour. In cane, the phenolases show a pH
optimum between 4.5 to 7.5; they are known to react with chlorogenic and
caffeic acids. The phenolases can be quite stable; considerable activity has
been found even after heating at 70'C far 15 minutes.

Generally phenolases inactivation is by heating at 80 - C for at least 10 minutes.

S02 gas and sulfites in aqueous solutions and at concentrations above a given
minimum can act as inhibitors. The exact mechanisms for the inhibition are not
clear.
2.6.2 Non enzymatic browning

Non enzymatic browning can be divided into two broad classes:-

0 Caramelisation where sugars dehydrate by a series of steps.

Reactions between sugars, mostly glucose, and amino acids.

In the caramelisation process a series of dehydration takes place, leading to Caramelisaion

polymerisable products of high colour. A very simplified pathway is shown
below.

H -C=0 H-C=0 H-C=a H- C-O

H-C-OH C-0H C
H0--C-H - H2O C-H - RIO CH O
• H,U
31
D
H--- LOH OH-Lou H- -H
H-C-OH H- LOA H- ~OH -]
CH,OH C'tt,off &,OH CH,OH

The original sugar is glucose and the final product is hydroxy methyl furfinal,
which polymerises and is highly coloured. It is possible to utilise a reaction
Blocking with sulfite
between glucose and sodium hydrogen sulfite, NaHSO 3, to slow down or
reduce the dehydration. A simplified reaction scheme is given below.

SD,Na
H -C--O H-C-OH
i
H--C-011 H-C-OH
+ NoM5t7; i
80-C-H H0-C-H
H- [.^ OH H- LOH
H- C-OH H- LOH
&,OH CH'OH

-17-
The sulfite adduct is much less reactive towards the dehydration.

In the reaction between glucose and amino acids, generally falling under Maillard type reactions

Maillard type reactions, the initial step can be between the

group of the sugar and the amino ( -NH2 ) group of a protein or amino acid,
followed by very complex reaction schemes, simplified here as

Glacoee and amino nitrogen

H -C-o
1 + R,IV--R "---R
r f- A---C---OH

Again sulphurous acid salts prevent or retard the initial step by forming non
reactive sugar derivatives. Ifthe reaction has occurred and colour formed, then Hloetdog by auttite
the addition of these salts or of SO2. will not reverse the reaction or reduce the
colour.

The Strecker degradation is another, less known, sugar degradation pathway.

Fructose or glucose react to form dicarbonyl compounds which in turn initiate Streckler degradation

the degradation of amino acids; C02 is produced together with aldehydes and
amino ketones. The pathway to the dicarbonyl compound is shown in a
simplified way below_

- 1 8-
 Pathway to dicarbonyl
x H
I
a-c-o
a- -oH C-off c=a
H -H
+ H,N-R'

. H,O
C-OH 31 1-o
H-LOH H- off tl - -OH
H- LOR H- LOH H- LOH
L1.U11 t_'H,UH H,OH

ENMIOL DICARBONYL

The dicarbonyl then reacts with amino acids, with a molecule of water being
lost, to produce amino ketones. These degrade, losing carbon dioxide, to form
various products, including ring compounds. Generally these reactions are
exothermic and are accompanied by a decrease in pH.

As was the case with caramelisation, SO, and sulfites can inhibit those Blocking by salfites
reactions by blocking the formation of the carbonyl compound through a
reaction with the sugar to farm a carbonyl-hydrogen sulfite additive. It has also
been suggested that the browning reactions are inhibited by sulfites via free
radicals, derived from the sulfite.

2.7 The reactions of sulfites with sugars

Sulphurous acid salts react with the aldehydic ( H - C = G ) open chain

Hydroiysalphonate
form of sugars to yield products to which sulfite is bound chemically to the
sugar. This has been shown on page 17. The product is a hydroxysulphonate
of glucose in the case shown. These types of reactions have been studied by
a number ofworkers, such as Carruthers et al. (1968) and Braverman (1953).
Details of the reaction :-
The following points have been established:-

9 The sulphonate derivatives ofthe bisulphitelcarbonyl adducts are not

generally fermentable by yeast. This can impact on the value of cane molasses
sold to fermenters, if sulfite has been added in the process.

0 As shown in section 2.6, the bisulphitelcarbonyl adducts are less

reactive to browning reactions, which are therefore inhibited or slowed.

- 1 9-
 0 The relative binding strength between sulphur dioxide or sulfite, and
sugars has been found to be arabinose > glucose > maltose > lactose > Reaetivities of Sugare
with
fructose > sucrose. Other workers however state that galactose, mannose and
arabinose were the most active in combining with SO z; maltose, lactose and
glucose were moderately active, raffinose slightly active, and fructose and
sucrose probably inactive. Thus in cane products the glucose/sulfite interaction
can be of practical significance.

e Reaction conditions profoundly affect the glucose/sulfite reaction.

Effects of pH and of
In the laboratory and with pure reactants, good yields ofthe glucoselbisulphite temperature
product are obtained with a pH of 4.5 and at room temperature. Higher pH
values and temperatures can cause different reactions. The situation is
obviously much more complex in cane sugar factories.

3 THE MICROBIOLOGY

In the cane sugar industry SOz and sulfites are not usually considered as
bactericides. This is not the case in the beet industry. Italian workers ( Vaccari
et al., 1987) have used ammonium hydrogen sulphite and found it as good as SO, as batterieide in beet
fonnalin, with the added advantage that some colour was removed. In
England, Oldfield et al. (1968) state that ammonium hydrogen sulphite was
adequate as bactericide if the temperature was greater than 70°C, and if it was
used at concentrations equivalent to 150 to 200 mg of SO, per litre of raw
beet juice.

It should be noted that the use of bactericide in the sugar industry is always
subject to food and health regulations.
 4 THE TECHNOLOGY

4.1 Sources of sulphur dioxide

Gaseous sulphur dioxide is used extensively in the cane sugar industry. The
burning of elemental sulphur produces most of this SO2.

Liquid sulphur dioxide has been mentioned a number oftimes in the literature.
Honig does so already in 1953, but notes that transport and other costs did not Liquid $0,
favour the use of the liquid, and that sulphur burning remained the common
process in the sugar industry. A notable exception has been the use of the
liquid, recently, in South Africa {Moodley et al., 1997}. These authors give the
following reasons for selecting liquid S0 2 as a replacement for the traditional
sulphur burning process in their refinery.

0 The quality of the refined sugar was improved, due to better pH

control. The steady availability and constant good quality of the S0 2 gas Prartieal s6'aataees

produced from liquid sulphur dioxide were the main reasons for the pH
improvement.

* The use of liquid S02 with a dedicated control system, reduced the
consumption of the gas by 69%. This resulted in costs savings of 11%.

0 The smell ofSO 2 in the refinery was eliminated. Sulphur burning was
felt to cause a large proportion of the gas to be lost to the atmosphere.

Mixing between the 502 and the liquor improved.

0 The full scale use of liquid S0 2 has shown that it was economically
attractive as a replacement to sulphur burning in that refinery. But safety
equipment and special storage conditions are needed.

In most of its applications in the cane sugar industry, however, S0 2 is still

produced by burning elemental sulphur in air, using various types of burners.

Sulphur ignites in air at temperatures above 250'C, and burns with a blue Sulphur buroiag
Chemistry
flame. The heat of combustion is 9.2k3/g. The SO 2 content of the burner gas,
under ideal conditions, depends on the flame temperature and varies fxorn 6%
at 800°C to 20010 at 175(1°C.

The burning ofelemental sulphur under the usual cane sugar factory conditions
is not a simple matter. An excess of air is needed, the sulphur vapour and the
air must be well mixed, and a large combustion space is needed. If the

_2 1 _
combustion is incomplete the sulphur vapour condenses and solid sulphur is
deposited, which can cause blockages. It should be noted that this process is sublimation

caused by condensation and not sublimation ( the process through which a

solid changes directly into a vapour).

If combustion proceeds too far, sulphur trioxide, SOP is produced Production of 50,

2 S02 + 02 r-' 2S03

which will form the highly corrosive sulphuric acid with any water present.
Iron oxide can catalyse the above reaction. Finally, this reaction is exothermic.

A good compromise in commercial sulphur burning is to lower the Cooling and drying
temperature of the gases produced by cooling the burner externally; a water
jacket can be used, and to reduce the moisture content of the air fed into the
burner. Of these two steps, drying of the air is the better measure, but both
should be used.

The quality, particularly the purity, of the sulphur impacts on the production
of SO2. Bituminous or carbonaceous impurities form a film on the molten Purity of the sulphur

sulphur in the burner and prevent air from reaching it. This retards the
combustion process or even extinguishes the flame.

The selection of a proper burner depends on the quality of the elemental

sulphur to be burned and on the quantity and concentration of the SO 2 needed.
Sulphur burners
There are many types of sulphur burners, two typical designs being shown
below. A paper by Bhaghat et al. (1999) gives some recent developments.

_22_
-23-
4.2 Sulphitation in raw cane sugar factories

4.2.1 History and process

The use of sulphur dioxide dates back to the earliest days ofthe European beet
S02 tried in cane is !&65
sugar industry. Although the early results obtained in beet may not have been
decisive, they served as incentives to experiments with sulphur dioxide and
cane juices in Mauritius, as early as in 1865. From there the application of S0 2
was introduced in Java.

Technical information on the use ofsulphitation in cane sugar factories started

Historical backgronod
to be published regularly over the period 1895 to 1940. van Gorkum (1895)
reported on work in Java; Prinsen Geerligs published in 1896 and 1905;
Zerban, in Louisiana, worked with the analysis of sulfited cane juice (1908);
Harloff and van der Linden (1911, 1912 and 1916) developed juice
sulphitation processes; Famell in 1924 commented on syrup sulphitation;
Haddon in Mauritius (1933), Neuville in Egypt (1932), Dymond (1936) and
Latham (1931) in South Africa and Fort and Walton (1932) in the United
States of America also contributed.

There were many variations for cane juice sulphitation. The basic processes Basic processes with cane
were as follows.

0 Tank sulphitation. This was a sulphitation process done in tanks, as

opposed to the use of percolation towers. Originally the juice was sulphited
without prior heating. Sox was blown through limed juice to a pH of 7.6, and
the juice was then heated to 103 °C, flashed and settled. Very severe scaling
problems, daze to the late precipitation of CaSO 3.2H2 0, were encountered.

In 1912, Harloffreconunended hot sulphitation. The juice was heated to 70°C,

S02 and milk of time were added simultaneously, with the amount of milk of
lime having been established by experience. S02 was then added until a pH of
7.6 had been reached. Most of the calcium sulfite was precipitated by this
process, thus reducing the scaling problem.

*Tower sulphitation. The juice was heated to 70°C and made slightly
alkaline. It was pumped to the top of a sulphitation tower and percolated
down while the S02 gas was drawn up by means of a gas extractor.

Perk {1973) stresses that the reason for sulphiting at 70°C is to speed up the The importance ofsuipisitiog
at 7u'C
crystallisation of CaS03. 2H2 0, thus reducing scaling problems. That
temperature is a good compromise; it does increase the precipitation rate but
without too high a risk of inversion or of the destruction of fructose and

-24-
glucose.

0 Early Natal process. The juice was heated to TO°C, prelirned with
milk of lime to a pH of 12 and SD, added.

Because of the high original pH, gassing with 502 often could not reduce the
pH to normal levels and this had to be corrected by using a phosphoric acid
paste. This was costly in terms of chemicals. The high original pH also caused
severe destruction of fructose and glucose. The process was discontinued
mainly because of cost.

Finally, it should be noted that an important milestone in the sulphitation Introdoetion or pH

process was the introduction of pH measurement and control in sugar measurement

factories, in 1926. This provided the means for process control, particularly
in sulphitation where pH has a large impact.

4.2.2 Recent laboratory work

Laboratory investigations ( Getaz and Bachan, 1989; Rein, 1988 ) have

concentrated on investigating optimal conditions for decolourisation by using
gaseous sulphur dioxide, from gas bottles. Typical results with cane mixed
juices are shown below.

40 -

decolourisation ohnined by
e 30 r Lsing sulphur dioxide oo
a mined juices
s
.920
v
910 -
0
0
0 1000 2000 3000 4000 5000
Sulphur dioxide added (mgfkg AAJ)

-2 5-
 0 son 1000 1600 2000 2500 3000
Sulphur dioxide (mgtkg MJy

Maximum deeolourisadon
it is evident that, with typical South African mixed juices, a maximum 335'.
decolourisation of about 35% can be achieved. To reach that decolourisation
With 3000 to 5000mg s0,
about 3000 to 5000mg of sulphur dioxide per kg of juice would be required. per kg MJ

In the laboratory stoichiometry is used to estimate the amount of S0 2 added.

This is done as follows. The amount of S02 to be added is decided upon and
Calculation of lime and of
the mass of the juice to be used set. It is then possible to calculate the total S0, quantities in lab work

mass of S02 needed. The following equation is used

Ca(OH)2 + S0 2 -)' CaSO 3 + HO

where 48g of S02 correspond to 74g of Ca(OH) 2. Thus it is possible to

calculate how much Ca(OH) 2 is needed to react with the mass of SO, decided
above. In laboratory work one nom-ally uses chemically pure calcium
hydroxide and the required amount is made up as a slurry. This and the S0 2
are then added simultaneously or separately to the juice until all the slurry has
been used. The final juice pH is normally the same as the original one. This
approach can cause large errors, and scatter, as seen in the figures on pages
25 and 26, is inevitable. Nevertheless useful results are obtained.

Laboratory tests have also shown that juice sulphitation results in sugar Low colour transfer
colours lower than expected from the level of decolourisation achieved on the
juice. This ability of 502 to remove colourants which have a higher than
average affinity for the sucrose crystal has been noted elsewhere (Lionnet,
1990).

Finally, there are indications that mixed juice sulphitation, particularly at the

_26..
higher S02 dosage rates, can achieve better decolourisation than syrup
sulphitation.

Rein (1988) reports on laboratory syrup sulphofloatation tests. Syrup

decolourisation of up to 25%, with about 5000mg S02 per kg syrup, were
achieved. Milk of lime, phosphate and S0 2 were used.

4.2.3 Industrial applications

It is possible to produce white sugar directly from cane raw syrups, without Plantation white
fast making raw sugar. The name plantation white, or mill white, has often mill White
been used for this type of sugar.

To produce these sugars one must use more elaborate chemical processes than
defecation, and sulphitation is often the choice. This is the case in India and in
Colombia for example.

Juice sulphitation, using gaseous S02, is the usual approach, and this is
followed by the sulphitation of syrup. This combination gives a mill white
sugar ofhigher and more regular quality. The amounts ofchemicals needed for
the production of a mill white sugar, as given in various references, are shown
in the Table.

Chemicals needed far

kg per ton cane References mating Moll White

LAME SULPHUR FLOCCULANT

1.6 0.8 - Honig

- 0.25 to 0.45 - Getaz

2.2 0.6 0.004 Indian data

A process for juice sulphitation is shown below.

-27-
 Caar jmiee Sulpbitatiou

Two points are important.

0 Good instrumentation and good control (pH, temperature, flow, etc)

are essential.

0 Liming followed by S0 2 addition has been shown to be more

-28-
efficient for juice deco lourisation, than the simultaneous addition of milk of
time and SO..

For maximum decolourisation a fine precipitate with a large surface area is

Deeolouriutooo vs. rdtatoon
required. This type of precipitate usually settles and filters poorly. There are
however #locculants which can be used to avoid or reduce these problems.
Ting and Hsia (1989) show that for juice sulphitation the optimum degree of
hydrolysis is between 30 and 35%. Magnafloc D or LT26 would fall in this
range. An optimum dosage was quoted as 5mg per litre of juice.

A schematic diagram of a juice sulphiter is given below.

Juice sulphiter

_2g_
Finally, Thangamuthu et al. (2000) give a process for the sulphitation of the
filtrate from conventional Oliver filters.

4.3 Sulphitation in refining

4.3.1 Industrial importance

As already mentioned in the Introduction, sulphur dioxide is not an important

Faoctioa of 5Q, "fib beet
chemical in the beet industry. It is sometimes added to the beet liquor after the
second carbonatation, at rates between 0.001 to 0.002% on beet, that is at
rates which are about 1 to 2% those used in cane. In the beet application the
main functions of S02 are to correct the liquor pH, to block the destruction of
fructose and glucose and to provide a minor colour reduction.

A publication by Clarke (1997) shows that more than half the refiners
sulphitation in cane refining
surveyed at that time used carbonatation and that phosphotation was also
popular. There was little to no mention of sulphitation. The situation is
somewhat different in Southern Africa where sulphitation is utilised in seven
backend refineries as a secondary purification process after carbonatation,
while one back end refinery uses it as its sole purification step.

Rein (1988) reports on laboratory work investigating the gassing and flotation
of refinery melt. This sulflotation process enhanced turbidity and colour
removals at a low lime addition rate of 0.1 % on melt Brix and without the
need for filtration.

4.3.2 Laboratory work

Laboratory sulphitations of refinery liquors, followed by pilot plant

crystailisations show results which have been summarised in the following two
figures.
 40
Deeolourisation with
refinery Hquors
30
C

a:
i 20
0
0
~ 70
O

o lb
o 5oo 1000 1500 2000 2500 3000 3600
Sulphur dioxide (mglkg liquor)

-i 20
Colour transfer with
sdphotatoon

w
0 10 _
C
a-

I: I

490 600 600 790 000 908 1000

Feed colour tICUMSA units)

It is evident that :-

• A maximum decolourisation of 35 to 45% can be expected.

e The decolourisation plateausabove dosages of3000 to 5000W S02

per kg of liquor.

The relation between the afnated crystal colour and the pan feed
0
Colour transfer
liquor colour is linear. This linear trend has been confirmed not only for
sulphitation but for all the main refinery decolourisation . processes tested
(Lionnet and Moodley, 1995). It has been investigated by many workers and
falls under the heading of colour transfer.

Experimental work in South Afi -ica has been used to compare a$inated crystal
colours when the feed liquors had been decolourised by the sulphitation

-31-
process, by the use of ion exchange resins, and by the use of the phosphotation
process. Detailed results are in papers by Lionnet (1991) and by Lionnet and
Moodley (1995); a brief summary of the main findings is given below.

r The afnated crystal colours were linearly related to the feed liquor
colours. All the relationships were highly statistically significant. These
relationships are in the table below.

Relations betrreca crystal

PROCESS Equation mad feed colour
Crystal colour = a + b x feed colour
a b

Carbonatation 7.2 0.022

followed by
suiphitation
Carbonatation 8.0 0.024
followed by ion
exchange
Phosphotation 12.3 0.024
followed by ion
exchange

r These relationships are compared graphically in the following figure.

Grapbical representation of
the relationships

V io
200 300 40o son am
Feed colour (ICUMSA units)

-32-
It is clearly evident that, for the same liquor colour, the sulphitation process
yields the lowest crystal colour. Sulphitation thus has a better ability than ion
exchange or phosphotation to eliminate those colour bodies which have a
higher than average affinity for the sucrose crystal.

4.3.3 Industrial applications

The more common application of sulphitation in Southern Africa is to obtain

Suiphitatooa of brown liquor
a second decolourisation and a de-ashing process, after carbonatation. Filtered
carbonated liquor, or brown liquor, has a pH of 8.2 to 8_5. There is therefore
a possibility to reduce that pH by using sulphur dioxide; this in turn reduces
the ash content by precipitating soluble Ca'' as calcium sulfite. A typical flow
diagram is shown on page 34.

It is also possible to use sulphitation as the sole decolourisation process to So Iphotatioo af melI
produce refined sugar. A flow diagram is shown on page 35.

It is useful to use stoichiometry to calculate mass ratios between the various I mportant mass ratios
species involved in the sulphitation process, as done below.

S + 0 ---~ SO2
2

CaO + H20 ---+ Ca(OH) 2

Ca(OH) 2 + H 2 SO 3 ---~ CaS0 3 + 2H20

yield the following theoretically correct mass ratios:-

S S02 . Coo . Ca(OH)2 . CSS03

0.50 ; 1 0.88 : 1.16 1.88

Theoretical efficiencies are not reached under practical conditions, particularly Theoretical vs. iadaatrial
quantities
industrially, due to physical losses, side reactions, non ideal conditions, impure
reagents, etc. Thus for industrial sulphitation it is usual to budget about twice
the theoretical amount of elemental sulphur needed to be burnt, and the
calcium sulfite formed is usually less than the quantity calculated using the
above ratios. Nevertheless the theoretical values are needed to provide
guidelines through material balances.

-33-
 Tons : 10.9
Purity : 99.6
Colour : 1200

Tons : 17.1 3.8

TONS: 3.4 TONS:
Temp : 80 'C
Colour, 1560

LURE MWER

CARSON DIOXID
SATURATORS I TONS: 0.08

SLIIDSrr
SULPH rsRB

T •U 3.0

GARB LIQUOR

I TONS - 0.71 Tons : 17.3

colour: 693

W SULPSUR DIOJCIDR
rMTERS SULPHITATION 5 % REF SQG : ROB
If9 SO2 : 55S

FILTERS

SwMT
FILTXR CAKE WATFit FILT SULPHUED LIQ
Taws .&45 'roof : 3.4
Tons : 17.3
Colour : 596

EVAPORATORS

PAN FLOOR

FINE LIQUOR
Tons : 15.5
Colour; 638 REFINED SUB
4th JET
Tons : 10.0
Toes 1.15
9274 Colour: 42
Colour :

- 34-
- 3 5-
Some important parameters relevant to partial and full sulphitation are
Dab ror portid and fog
compared in the following table. auiplotatiou

PARTIAL FULL

Melt Brix 70

Melt temperature (°C) 75 to 80

Dosage of SO,: 300 to 400 4000 to 5000

(mg per kg melt)
(mg per kg Brix) 400 to 600 6500 to 7000

kg sulphur per ton of 13 30

refined sugar per hour

Sulphitation vessels 1ary 1"y and 2arr

CaO added (°In) 100 70 30

Exit pH 7.1 8.2 7.1

Decolourisation (% ) 14 45
4.3.4 Filtration

4.3.4.1 Introduction

Sulphitation like carbonatation produces a solid precipitate, namely Ca50 3,

which must be separated from the liquor. There are a number of reasons for Need for sepanting
precipitate from liquor
this separation.

0 The liquor sent to process must be free of suspended matter. Any

remaining suspended matter may cause blockages in downstream processes
and may affect sugar quality.

s Laboratory and pilot plant work has shown that for the highest sugar
decolourisation (as opposed to liquor decolourisation) it is essential to remorse
the precipitated CaS0 3. Otherwise, the colour of the sugar is higher than
expected from the liquor colour. It is believed that the physical removal of the
colour which has been trapped into the precipitate is required if all that colour
is the be prevented from entering into the crystal. The keeping quality of the
sugar can also be affected if the precipitate is not removed.

The filtration process is thus essential with sulphitation~ just as was the case Sulphita6oa yields less
with carbonatation. Sulphitation however yields less precipitate than would be precipitate On
carboostatioo
the case with carbonatation. Nevertheless the following two points must be
considered.

0 Sucrose losses around the filter station must be reduced to as low

as possible. The quantity of low Brix sweetwater must be kept low and the
temperature must be high to prevent microbiological activity. Obviously
spillages and leaks must be avoided.

0 The filtration process must be as efficient as possible in terms of

cycle time. As mentioned above the quantity ofprecipitate is smaller than with
carbonatation and filtration is often reasonably efficient.

4.3.4.2 Types of filters

As with carbonatation two filtration stages are generally needed. The first
Two Tiltrafioo stapes
treats all the sulphited liquor to produce a calcium sulfite sludge and a clear
liquor. The latter may be filtered again, as a safety precaution in case of
accidental failure or poor performance of the main filter. The second stage is
a traditional sludge filter producing sweetwater and cake for disposal. A
typical schematic diagram is shown below.

-3 7-
 5ULPHIT£D LIQUOR
TANK STEAM Solpbitatiom niters
90 'C

WATYA SLUDGE

CAKE

POLTSHTNG
nLTM

ME LIQUOR TO
PROCESS

F7LTKR CAKE SWEET WATER TO

TANK

The first filtration stage can be done in rotary leafy candle or vertical leaf Fiat tiitntioa stage

filters, at a temperature of about SO°C. A design figure is about lOrn' of

filtering area per ton of refined sugar per hour. No filter aid is necessary.

If the sulphitation sludge is mixed with carbonatation sludge, then the

carbonatation filters will handle the sulphitation precipitate without the need
for additional surface area. Usually, the quantity of CaSO 3 is much smaller
than that ofthe CaCQ3. Typical carbonatation sludge filters are the rotary leaf
and the plate and frames.

-38-
When sulphitation is used on its own, the sludge must be desweetened in a
special filter. A rotary vacuum filter can be used, with water at 80°C. A design
figure is 0.25 to 0.50m' of filtration area per ton of refined sugar per hour.

4.3.4.3 Operations

The operations of the filters may be summarised as follows.

r The sulphited liquor is pumped through the main filter and the
filtrate is recycled to the feed tank until it is free of turbidity. The filter is then
put on line.

0 At the end ofa cycle, say after 8 hours, the filter is taken off line and
the liquor remaining in it is forced out with compressed air. Any cloudy liquor
is diverted to the feed tank. When air cannot force out any more liquor, what
is left behind may be drained out and sent to the feed tank.

0 Sweetwater is then pumped through the filter and circulated back to

a cloudy sweetwater tank until it exits the filter as a clear liquid; then it is sent
to the clear sweetwater tank. Desweetening may be completed with hot water.

r When desweetening is complete, the cake is sluiced down; that is it

is washed from the filter into a slurry tank. Hosing down of the filter may be
necessary.

0 The final cake desweetening is done by filtering the sludge through

the second stage vacuum filter. The filtrate obtained is used in the
desweetening process mentioned above.

There can be many variations to the above sequence of operations, depending

Srerose lows
on local conditions. The important points are the complexity ofthe processes, Energy
the need to reduce sucrose losses, and the impact on energy as large quantities
of hot water and of low Brix liquors are involved.
 5. HEALTH REGULATIONS

5.1 Legislation

Two large institutions, namely the Codex Al imentarius, a joint organisation of Codex Alimentarius
the Food and Agricultural Organisation (FAO), and of the World Health
Organisation (WHO) of the United Nations, and the Food and Drug Food and Drag
Administration
Administration, (FDA) in the United States of America provide international
standards for sugar. These include a standard that white sugar of Category A leas than 24mg SO, per
arsugar
must contain less than 2amg SO2 per kilogram of sugar. The FDA quotes a
maximum level of 1 [brig per kg, while a new (1997) Codex maximum level is
15mg per kg, which is also the value quoted in a EU (1997) specification.

It is considered that with good pH control and correct factory operations,

these standards can be met.

General food literature points out that an attractive feature of preservation

through the use of sulfites in food is that they appear to be harmless at the
concentrations stipulated. The safety of sulfites when used in legally allowed
quantities is generally recognised even by workers critical of food additives.

5.2 Analysis of residual S0 2

The official ICUMSA (International Commission for Uniform Methods of

Sugar Analyses) method is the rosaniline method, which is suitable for the Rouniliae method

determination of very small quantities of SO 2 in sugar.

Basically the sugar sample is dissolved in water and sodium hydroxide added,
to yield a fixed solution volume. A rosaniline solution (in water plus
hydrochloric acid) and formaldehyde are added to the solution, the mixture is
allowed to react and the colour read at 5banm under standard conditions. A
calibration graph is used to calculate the concentration of S0 2 in the sample.

The reaction, called a Schiff reaction, proceeds as follows. Rosaniline and

hydrochloric acid in an aqueous solution form a colourless anilinium salt:
 Colourless an! lioinm Wt

+H,N

NY[j.

Sulphurous acid and formaldehyde react as follows:

HCHO f HIS03 =* HO {CHI S03H

hydroxy sulphonic acid

this acid now reacts with the anilinium salt to form

Coloured organic eompouod

03H

CHI

N H+
Cf

namely pararosaniiline methyl suiphonic acid, which is purple. The intensity of

the colour, measured at 56Dnm, depends on the concentration of the
sulphurous acid and, under standard conditions, the reaction yields a
quantitative measure of the SO, content.

-41-
 6. DEVELOPMENTS

6.1 Liquid S02

The use of liquid SO2 has been discussed in section 4.1 and its advantages
mentioned. This is not a new development but its use is not widespread.

6.2 Solutions of ammonium bisulfte

Ammonium bisulphite breaks down into ammonia, sulphur dioxide and water.
It can therefore be a source of SD2 without the disadvantage of adding a
metallic cation such as Na' for example. The aqueous solution is relatively
easy to store and to use. It has recently been made available in South Africa
and applications are being investigated.
 BIBLIOGRAPHY

Bhaghat J J, Chaturvedi P P, Kalia S C and Agarwal P (1999). Use of new generation film type
sulphur burner and PLC based integrated clarification control in a plantation white sugar factory. Proc
Int Soc Sug Cane Technol Assoc 23.

Braverman J B S ( 1953). The mechanism of the interaction of sulphur dioxide with certain sugars.
J Sci Food Agric, 540-547.

Carruthers A, Oldfield J F T and Wootton A E (1958). Studies in the chemistry of sulphitation.

British Sugar Tech Conf, 1- 42.

Chung Chi Chou (Ed) (2000). Handbook of sugar refining. John Whey and Sons, New York, 756
pages.

Clarke M A (1997). Colour removal. Proc Sugar Ind Technol, 1997 proceedings.

Getaz M A and Bachan L (1989). Some ideas on the use of chemical methods for improving the
colour of A-sugar. Proc S Afr Sug Technol Assoc 63, 76-80.

Godshall M A and Roberts E J (1982). Phenolics in sugar products: role in flavor and colour
production. Proc Sug Proc Res Inc, 47-72.

Gross D and Coombes J (1976). Enzymatic colour formation in beet and cane juices. Int Sug J 78,
69-73,106-109.

Honig P (1953). Principles of sugar technology. Elsevier Publishing Company, Amsterdam, 645
pages.

Lionnet G R E (1991). Colour transfer from liquor to crystal during the refining of South African raw
sugar. Com Int de Tech Suc 19, 15-30.

Lionnet G R E (1985). A study of the extraction of non sucrose components of sugar cane. MSc
Thesis. University of Natal, Durban. 142pp.

Lionnet G R E and Moodley M (1995). Colour transfer in the South African sugar industry. Proc Int
Soc of Sug Cane Technol 22, 217-225.

Lionnet G R E (1990). The use of sulphitation and of ion exchange in the refining of cane caws. Proc
S Afr Sug Technol Assoc 64, 228-232.

Moodley M, Bekker D J, Pienaar P J and Pillay R (1997). Replacement of sulphur burner with liquid
sulphur dioxide system at the Maleiane refinery. Proc S Afr Sug Technol Assoc 71, 142-145.
Oldfield J F T , Dutton J V, Grierson D, Heaney R K and Teague H J (1968). Comparison of sulphur
dioxide and formaldehyde as bactericides in diffusion. Int Sug J 70, 296-298, 330-333.

Perk C G M { 1973 ). The manufacture of sugar from sugar cane. C G M Perk, Durban, 212 pages.

Rein P W (1988). The application of flotation clarification in sugar processing. Proc Sug Proc Res
Inc Conf.

Reynolds T M (1965). Chemistry of non enzymatic browning. Advances in Food Research, vol 14,
167-283.

Smith P, Patton N H, Delaney H R and Ames R (1981). Colour studies in milling. Proc Aust Soc Sug
Technol Assoc, 71-80.

Smith P (1982). Analytical techniques for the separation of colour components and their application
in sugar processing. Proc Sug Proc Res Inc, 256-264.

Smith P (1982). Analytical techniques or the separation of colour components and their application
in cane sugar processing. Proc Sug Proc Res Inc, 256-264.

Smith P and Hall P M (1971). Sugarcane anthocyanins as colour precursors and phytoalexins. Proc
Int Soc Sug Cane Technol 14, 1139-1146.

Song P S and Chichester C O (1967). Kinetic behaviour and mechanism of inhibition in the Maillard
reaction. Mechanism of the inhibition. J Food Sci, vol 32, 107-115.

Thangamuthu P, Chinnappa N, Subramanian P and Jenekar G M (2000). Need for a new system for
vacuum filtrate clarification in sulphitation factories. Indian Sugar, 963-972.

Ting C S and Hsiao Y C (1989). Evaluation of polyacrylamides flocculants in the sugar industry.
Taiwan Sugar, vol 36, No 5, 21-27.

Vaccari G, Mantovani G and Sgualdino G (1987). Investigations of industrial factors decreasing

sugar crystal colour. Corn Int de Tech Suc 18, 349-368.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

I Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control
5 Evaporation: The fundamentals
6 Evaporation: The practice
7 Pan boiling 1
8 Pan boiling 11
9 Diffusion
10 Refinery carbonatation
11 Mlling
12 Sulphitation

In preparation:-

Applied statistics
Boilers
Phosphatation
Sugar quality
Ion exchange and activated carbons
 Sri'

MUD FILTRATION
 Sugar Technology For Students

MUD FILTRATION

Prepared by G R E Liorrrlel

Study Text 2

Published by G R E Lionnet
Published by G R E Lionnet
25 Haleric Rd
Durban North, 4051
KwaZulu Natal
Rep of South Africa

First published 1999

Copyright 0 1999 G R E Lionnet

Printed in Durban by
G R E Lionnet

ISBN 0-620-23544-6

This text or any part thereof must not be reproduced in any form without the
written permission of the publisher.

This text forms part of a sugar technology study programme. The complete list
of units in the programme appears at the end of this text.

For availability, new study units and other information, please write to G R E Lionnet,
25 Haleric Rd, Durban North, 4051, KZN, RSA.
 SAGASSE
AIR
 i, INTRODUCTION

The outcome of the clarification process in all cane sugar factories

Results of ciarification
consists of a clear juice, which moves forwards to the process, and of
an underflow called mud. This consists ofthe precipitated impurities.

The mud, which appears as a thick fluid, normally contains less than Filtration and return to diffowr
10% by mass of solids. Thus 90°/0 of it is clear juice, which, in
modern and efficient sugar factories, must be recovered. A filtration
process is used to do so, although in factories using diffusion there is
the possibility of routing the mud, untreated, to the diffuser.

For factories with mills, filtration is thus the final clarification objectives
process. It has two main objectives. Firstly, it must separate the solid
impurities from the juice, for them to be disposed of as economically
as possible. Secondly, as much as possible of the sucrose present in
the mud must be recovered.

Sucrose losses during filtration can occur in two main areas. Firstly, Losses of sucrose
there is an unavoidable loss of sucrose in the filter cake. Secondly,
there can be less visible but more severe losses because of
microbiological activity in the filter station.

The use of rotary vacuum filters is now nearly universal in the cane History
sugar industry. A brief review of the literature shows that the
continuous rotary vacuum filter was introduced to the sugar industry
in 1935. The proceedings of the 1934 Hawaiian Sugar Planters'
Association note that an Oliver rotary filter had just been installed in
one factory. One unit (8 x 12 feet) was bought in Trinidad and one
in Formosa, in 1935, In 1936, Fiji reported that this type of filter was
so satisfactory that two more (made in Australia) were being ordered.
In 1939, 90% of the mills in Hawaii had rotary vacuum filters.

Finally, as already mentioned, with cane difffusion it is possible to Mud routing to the dilfbser
route the mud, as is, directly to the diffuser. This eliminates the need
for a filter station and can be economically attractive.
 2. THE MACHINERY

2.1 Mud filtration

2.1.1 Mud handling

The basic principle in mud handling is to prevent mechanical damage No mechanical damage
to the mud particles. Muds contain flocculated and coagulated
particles which are fragile, and which should ideally be moved by
using gravity. If this is not possible, low shear, piston type pumps
should be used.

2.1.2 Sagacillo

Cane muds filter poorly if untreated. It is a universal practice to add Advantages of bagaciilo
bagacillo to act as a filter aid. Hagacillo is available, inexpensive and
works well as a filter aid.

It consists of small particles of bagasse, of which at least 85% will

Separation conveying and mWng
pass through a 4,85mm sieve. Equipment is needed to separate it
from the bagasse, to convey it to the filter station, and finally to mix
it with the mud.

Separation
Three types of separation equipment are common namely screens,
Screens. iouvres and idckers
louvres and kicker type pneumatic systems. Fixed screens under the
bagasse carrier, and inclined screens over which the bagasse tumbles,
have been used. The screens may be made of perforated plate or of
wire mesh. The area needed is about D,1 to 4,2m' per ton of cane per
hour, with mills; the lower value is adequate with cane diffusion.
Louvre separators have been the subject of much work in South
Africa and Australia. Essentially they consists of a feed hopper, a feed
drum with adjustable guide plates, and louvres, the angle of which is
adjustable. Suction is provided in the bagacillo collection chamber.
Sanders et al. i n South Africa describe an efficient system based on
a kicker type separator, using 7m' of air per kg of bagacillo, with a
velocity of 25m./s. The general layout given by these authors is shown
below. The separation chamber is described in detail in the
publication.
In all cases, the driest bagasse should be fed to the separator. Thus Bagarcillo feed to separator
bagasse from storage, rather than directly from the last mill, should
be used. This also results in bagacillo being available during mill
stops. The separator should be as close as possible to the filter
station, to reduce conveying problems, and should be accessible for
maintenance.

Conveying
This is done pneumatically with about 6m' of air per kg of bagacillo.
The air velocity should be about 20m/s.

Mixing with muds

Bagacillo is mixed with the muds in mud mixers which consist of a
Volume of mixers
trough with paddles/disc mixers. For 100 TCH 0,5 to 0,8m3 of mixer
capacity is needed, with milling tandems, resulting in 2 to 3 minutes
of retention time; about half that volume is adequate with cane
diffusion. The tip speed ofthe paddles must not exceed 0,7 to 0,9m/s.
Steam injection may be necessary and the temperature should not be
below 85°C. Lagging is recommended. Mixers are usually messy,
with bagacillo and mud spilling over, good housekeeping is
necessary.
2.1.3 Filters

Rotary vacuum filters are universal for the filtration of cane muds.
The basic principle of operation is shown below.

Schematic diagram of a rotary

vaccum filter

The filter consists of a rotating drum covered with perforated metal Operation
plates, which dip into a trough containing the filter feed. As the drum
rotates suction is applied to the different segments, forming a thin
calve on the plate surface. This builds up to the required thickness and
then passes under washing sprays and drips; it is then dried by suction
and removed by scrapers to a conveyor. The filtrate is conveyed
through metal pipes to the head of the filter and from there to filtrate
receiving tanks.

A low vacuum is used at the cake forming and build up stages. This
allows the proper formation of the cake and reduces the passage of Cloudy and clear filtrates

too much solids into the first portion of the filtrate, which is called
the cloudy filtrate. Thereafter a high vacuum is used to assist washing
and drying; the filtrate produced now is called the clear filtrate.
Finally there is no vacuum to allow the cake to be scraped away from
the drum. Cloudy and clear filtrates are relative terms. Generally both
filtrates contain suspended solids and, in South Africa, it is not
usually possible to route even the clear filtrate to clear juice.
Vacuum pumps, entrainment separators and vacuum regulators are
required. The pick-up or low vacuum is usually around 20kPa while
the high vacuum is about fi0kPa. The high vacuum should not be so
high as to cause the filtrate to flash.

Filtration medium
It is important to note that the filtering medium in rotary vacuum
filters is the cake itself. This is one of the reasons why mud
conditioning is required. It is possible to fit a filtration cloth over the
drum; this improves the quality of the filtrate, but can cause
operational problems such as blinding. The cloth can also tear if not
fitted properly or if it moves out of alignment. It also normally
requires cleaning with hot water sprays.

With milling tandems 0,4 to 0,8m' of filtering area is required per

TCH. About half to two thirds that amount is adequate with cane
diffusion. Wash water at 85°C should be strained to avoid blocking
the sprays. The quantity of water needed is 130 to I5O% on cake, or
enough to give a filtrate brix of 8 to g. Steam spargers may be needed
in the boot to keep the temperature around 85°C. Finally, the drum
rotates at about 3 minutes per revolution and this is adjustable usually
by means of a special pulley.

The main advantage of the rotary vacuum filter is the elimination of AdvaR1ap5 and disadvantages
manual labour, particularly when compared to filter presses which the
rotary filter replaced. Its greatest disadvantage is that it cannot
normally produce filtrate clear enough to be sent to the clear juice. In
South Africa the filtrate is nearly always sent back to mixed juice and
thus represents an increased load of about 20% in milling factories or
about 10% with cane diffusion.

Horizontal vacuum belt filters and solid bowl centrifuges have been New technologies
tested, in South Africa, in India and in Australia, for their ability to
handle cane muds. Recent work in India has shown promising
results, but the new approaches do not seem to be widespread.

2.2 Mud routing to the diffuser

2.2.1 Mud handling

The main requirement here is to convey the mud directly and rapidly
to a scale and then to the diffuser. This is best done by gravity, with
lagged piping, and adequate slope to ensure flow at all times. Care
must be taken to ensure that only mud, and not clear juice, is routed
to the diffuser. Since the process is continuous and does not require Muds and clear Juice

critical supervision by operators, this problem could occur.

Equipment is commercially available to measure the clarity of juice
and this could be used to monitor the flow and signal the presence of
clear juice.

2.2.2 Weighing of the mud

In South Africa the sucrose input into the factory is obtained from the
Impact an sucrose balances
weighing and analysis of mixed juice and from the amount of sucrose
in bagasse. Any sucrose which is recycled must therefore be
quantified. The mud needs to be weighed, sampled and analysed for
sucrose and brix, to allow a correction to be made.

2.2.3 Flow sheet

A schematic representation of the routing of mud to the diffuser is

shown below.
Mud to the diffuser

The equipment is simple and inexpensive, except for the scale and
sampling requirements. A compromise is needed as far as the point Point of addition
of addition in the diffuser is concerned. Ideally the mud should be
added near a set of lifting screws, towards the end of the diffuser.
The brix profile in the diffuser, however, is then disrupted and usually
the mud is returned somewhat forward in the diffuser.
 3 THE TECHNOLOGY

3.1 Terminology

There is often confusion about the meaning of terms used around the
filter station. It is therefore necessary to specify clearly the meaning
given to each term, as done below.

Definitations

Muds Clarifier down flow.

Bagacillo The size classified portion of bagasse.
Generally 85°/0 of the bagacillo should pass a
0,85mm sieve.

Filter feed The mixture of mud, bagacillo, flocculant,

lime, etc., sent to the filter.
Dry mud solids The oven dried, insoluble, bagacillo free
material found in muds or in filter feed.
Dry bagacillo Oven dried bagacillo.

Total dry solids The dry mud solids plus the dry bagacillo.

Bagacillo ratio The dry bagacillo divided by the dry mud

solids, expressed as a percentage.
Suspended Any suspended solids determined by filtration
solids and expressed as oven dried solids.
Filtrate The liquid product, which can contain
suspended solids, from the filter.
Filter cake The solid product from the filter.

3.2 Sampling and analysis

Most of the streams found within the filter station contain suspended
sampling diffic
solids. The different types of suspended matter exhibit different
properties; large particles such as sand settle rapidly, while bagacillo
will tend to float. Thus representative sampling, and more particularly
sub-sampling, are extremely difficult. Samples must be taken from
fast moving streams, preferably by a "cut" method. Sub-sampling
should be done while the material is being vigorously stirred, or
preferably by using a riffler.

The analytical techniques need care, particularly for the suspended Analytical diffic
solids. The use of different types of filter paper, wether filter aid is
added or not, drying techniques, etc., all influence the results
obtained. It must also be remembered that some of the methods for
the determination of pot and brix are designed for clear solutions, that
is solutions which do not contain suspended, insoluble matter, which
by definition may not contain any poi or brix. Relevant analytical
methods and calculation procedures must therefore be used.

3.3 Sucrose losses

There are two main causes for sucrose losses in the filter station. The Direct and indirect losses
first is due to the unavoidable presence of sucrose in the filter cake;
the sucrose in the cake is reduced by using wash water, through the
atomising sprays and then the drips. The water displaces the juice in
the cake, but this is never perfect. Investigative work has shown that
an asymptotic limit for the pot content of the cake is reached as the
wash water increases, as shown below. In South Africa losses in filter
cake are low, at between 0,2 to 0,3% of the sucrose in cane.

Pol reduction as wash water

increases

2.5
ua
2
U
ye 1.5
J
a 1

0.5

0
0 2 4 6 a 10
WASH WATER (kgikg solids in cake)

The second loss, through microbiological activity, is less evident but

can be more serious. Surveys of filter stations can show severe purity
drops between clear juice and filtrate, accompanied by increases in
the concentration of lactic acid, a by-product of the degradation of
sucrose by microorganisms. Some results of surveys done in South
Africa are shown in Table 1.

Table I

Surveys over filter stations

Factory A Factory S
Purity
Limed juice 85,3 81,8
Clear juice 85,0 81,4

Mud 84,4 79,9

Filtrate 83,8 77,8

indfications of microbiological
Lactic acid (mg/kg brix) activity

Clear juice 370 360

Mud 705 465

Filtrate 1500 1670

Temperature (°C)

Mud 93 89

Filtrate 61 63

Follow up work usually confirms that purity drops and increases in

lactic acid concentrations are associated with low temperatures and
long filtrate retention times in the filter station. Hypothermophilic
bacteria have been found to be active in clarifier juice, in muds and in
filtrate.

Filtrate residence times in filter stations can be measured with tracers

Fllfrate residence times
such as lithium. In South Africa the residence times have been found
to range from 14 to 46 minutes. The longer residence times were
associated with low filtrate temperatures and with large purity drops
between clear juice and filtrate. It is accepted that a temperature of
at least 75°C is necessary to suppress hyperthermophilic bacteria. Temperature
This minimum temperature must therefore be maintained at all times,
everywhere in the station. Heat losses must be avoided and wash

-10-
water temperature must be at least SO°C.

Another cause of low temperature has been found to be the poor Temperature in filter boot
distribution and circulation of filter feed in the filter boot.
Temperatures as low as 5a°C have been measured in dead spots in
the boot, at many factories. Modifications to the feed piping and the
use of steam sparging help solve this problem.

Filtrate retention time is affected primarily by installed plant capacity,

especially in factories where diffusers have replaced mills, and also by Filtration We
the filtration rate. Increasing the filtration rate would reduce the
number of filters required which in turn would reduce the filtrate
retention time. This highlights the need for a quantitative measure of
mud filterability.

Finally, a procedure to estimate the magnitude of the sucrose loss in

a filter station is given in section 3.5.

3.4 Mud conditioning

As stated earlier, cane muds do not filter well and bagacillo is used as
filter aid. It is thus possible to improve the filterability of muds and
other ways to do this have been investigated both in South Africa and
i n Australia. The specific cake resistance (a) concept is a quantitative Specific cake resistance
measure of filterability which has been shown to apply to the filtration
of cane muds. It is a measure of filtration rate and a second parameter
is needed to quantify the efficiency of filtration in terms of the quality
Filtration efficiency
of the filtrate produced. This parameter (e) may be defined as the
percentage of suspended solids removed in the filter cake. This
filtration efficiency is difficult to measure experimentally but it has
been found that there is a strong relationship between e and a. Thus
by optimising a the filtration efficiency is automatically improved.

This approach has been used in South Africa to investigate the

properties on cane muds from different regions and to compare mud
from factories with milling tandems to that from cane diffusion. Some
results are in Table 2.
 Table 2

Filterability of raw muds and of filter feeds

Dry mud Dry C1 Suspended

solids (°/o) bag cilo " (mkg' E) solids °l4
filtrate Muds and filter feed
NO
Raw muds 5,3 4 6,Ox 10" 1,3
Filter feed 4,4 2,2 2,5x14" 1,0

The data in Table 3 illustrate the comparison between milling and

diffusion.

Table 3

Filterability of milling and diffusion muds

a (fig '
)
Factory filter feed Laboratory
Milling and diffussion
conditioned muds

Diffusion 4, 5 x 10" 0,4x10 11

Milling 2,7x10" 0,4x10"

These results show that the factory conditioning of muds from cane
diffusion is not as good as that of muds from milling. It is clear
however that both types of muds can be treated further under
carefully controlled laboratory conditions to achieve the same
optimum value of a. There is therefore no basic difference between
muds from milling and diffusion as far as the filtrability is concerned.

More than 80 samples of muds, from nine South African factories

were conditioned in the laboratory and filterability was measured.
Average results are given in Table 4.

- 12-
 Table 4

Raw and laboratory conditioned muds

Raw muds Conditioned muds

Dry mud solids (°/o) 5,3 3,3

Dry bagacillo (/o) 0 2,8

pH 6,9 7,4

Flocculant (mg/kg) 4 4

cc (fig ) 6,0x 10" 0,4x l 0"

Suspended,solids 1,3 4,3

°Jo filtrate .

These results have been used to set the conditions required at the
factory filter station to produce improved mud filtrability and filtrate
quality. In turn this will result in reduced filtrate retention times,
higher temperatures and lower losses.

To produce a specific cake resistance around 0,4xl0" mkg"' and optimum operating coodltfons

suspended solids in filtrate of 0,3 010, it has been found that, in South
Africa, the following conditions are necessary.

Mud solids % filter feed of between 3 and 40/0. The higher

level would be maximum aimed for.

Dry bagacillo % filter feed should be between 2,5 and 3%,

with the lower value being the limit aimed for. This shows that a
bagacillo ratio of 80 to 100 is desirable.

The pH of the filter feed should be adjusted to about 7,5 with

milk of lime. This value should not be exceeded as blinding of the
perforated plates has been reported at high pH values.

The use of a flocculant at 4 to 5 mg/kg can be beneficial. This

is not seen as an essential requirement.

The temperature of the filter feed must be above 85 0C at all

times.

- 13-
The above conditions are well within the range achievable in practice
at factories and will result in all round improvements.

3.5 Mass balances

There are many ways in which mass balances can be conducted,

depending usually on the information which is available, on what is
wanted and on the accuracy required. In most cases an uncertainty of
at least 10% will be the best that can be expected.

There are two basic conditions. The first would be a design stage
exercise when masses are given but quality or performances not
available. At the operation stage, qualities and performances can be
measured but reasonably accurate masses, such as for clear juice or
muds, are not available. Only this second situation will be considered
here.

The following analytical results are taken as readily available.

Brix % filtrate : 9,35

Brix % mixed juice : 11,7
Brix % clear juice : 11,3

Filter cake % cane :6

Mixed juice % cane : 120

Moisture % filter cake : 74,0

Pol % filter cake 1,0

Filtrate purity : 83,0

Dry mud solids % filter feed : 3,5

Dry bagacillo % filter feed : 3,5

The balance is done for 100 tons of mixed juice per hour.

1) Filter cake

Mass of filter cake per hour = 6x1001120

= 5 tons

- 14-
 Mass of moisture in filter cake = 5x74,(}1104
= 3,7 tons

First assumption : Filter cake consists of water, brix and total dry Assumption r
solids only.

Then the mass of total dry solids and of brix in the filter
cake = 5-3,7
= 1,3 tons

Second assumption : The purity of the juice in filter cake is the same Assumption x
as that of filtrate.

Then, brix % filter cake = 1,0183,0x100

1,2

and the mass of brix i n filter cake = 5xl,21100

= 0,06 tons

The mass of the total dry solids in the filter cake is 1,3-0,06
= 1,24 torts

The mass of dry bagacillo in the filter cake = 3,5x1,2417,0

= 0,62 tons

The mass of dry mud solids in filter cake = 3,5x1,2417,0

= 0,62 tons

The mass of filter feed = 100x1,2417,0 Mass of filter feed

= 17.7 tons
Assumption 3
Third assumption: Moisture °Io bagacillo = 50.

The mass of bagacillo = 0,62x140!50

1_24 tons mass or bagacillo

The mass of muds = 17,7 - 1,24 Mass of mud

= 16.46 tons

2) Brix balance

Fourth assumption : Mass of brix in = mass of brix out. Assumption 4

- 1 5-
Fifth assumption: No brix is present in milk of lime and in bagacillo. nw=Pnou s

Then

RLMM CAKE
TONS :s
Rant x : 1,2

TONS :7
srsxx : 11,1

CLEAR AffCE

and tons brix in =100x11,71100

tons brix out = 5x1,21100 + Tons clear juice x 11,31100

Mass clear iuice = 103 tons Mass of Clear juice

3) Balances around the filter

Muds consist of clear juice and of mud solids. Then all the brix is in
the clear juice.

Sixth assumption: All the mud solids and bagacillo in the filter feed
are removed in the filter cake. This implies that
there are no suspended solids in filtrate.

Mass of dry solids in mud = 0,62

Mass of clear juice in mud = 16,46 - 0,62

= 15,84 tons

Mass of brix in mud = 15,84x11,31100

= 1,79 tons

- 1 6-
 BAGACILLO WATER

FILTER CAKE
TONS :5
TONS BRIX :
0,06

Again brix in is equated to brix out, in brix balances, brix in being

equal to 1,79 tons.

Brix out = Tons filtrate x 9,351100 + 0,06

Thus mass of filtrate = 18,5 tons

A material balance, given by mass in is equal to mass out, is now

used. Thus

Mass wash water = 18,5 + 5 - 16,46 - 1,24 Mass wash water

= 5,8 tons

it is now possible to draw a flow diagram as done below,

MIXED JUICE (100)

CLEAR JUICE (103)

--- 10

WATER (5,a)

BAGACILLO
(I,24)
FILTER CAKE
MUDS (5)
(16.46)

FILTER
FEED (17.7)

FILTRATE
(]5.5)

The balance is not perfect and depends on the validity of the

assumptions made and on the accuracy of the analyses. Filtrate for
example always contains some suspended solids, a value of 0,5%
being often found. Iterations may be used in the balance to cater for
that.

Mass balances may be used to estimate the effects of a drop in filtrate

purity on sucrose losses. Two assumptions are necessary. Firstly, the
masses of the various streams are kept constant, and secondly, the
mass of brix is assumed not to change, as the filtrate purity decreases.
It is then easy to generate the results shown in Table 5.
 Table 5

The impact of filtrate purity on sucrose losses in the filter station

83 9,71 0,0498 1,436 0 0,5

Losses in the filter station

82 9,71 0,0492 1,418 0,18 0,7

81 9,71 0,0484 1,401 0,35 0,9
80 9,71 0,0480 1,384 0,54

Thus with a drop of purity of three units, the total loss of sucrose
doubles. Apart from the direct loss in the filter station,
Impact on molasses exhaustion
microbiological activity results in the formation of by-products, such
as lactic acid, which are known to make molasses exhaustion more
difficult. There is thus an indirect, further loss of sucrose.

3,6 Filter cake disposal

This can be a problem both with regards to transport costs and

availability of land for dumping. Filter cake has some fertiliser value
and can be used as a soil conditioner. It is taken by farmers if it helps
them. A number of factories in South Africa include boiler smuts with
the filter cake thus complicating the issue. The possibility of making
compost from filter cake has been investigated.

3.7 The routing of muds to the diffuser

From a sugar technology point of view there are no serious reasons

why muds should not be returned to the diffuser. Since the
introduction of cane diffusion it is clear that filter cake tonnages, and
thus the amount of mud, have decreased to about half the levels
found with mills. Thus, roughly half the suspended solids in mixed
juice have already been retained by the bagasse bed, with no

-19-
insurmountable problem; this begs the question about the other half,

Preliminary results in South Africa show no adverse effects as far as Advantages of routing muds
extraction and processing in general are concerned, with muds being to the diffuser
returned to the diffuser. In all cases significant financial gains have
been identified, due mostly to the elimination of the operation,
maintenance and labour associated with the filter station, to the
elimination of costs associated with the handling, transport and
disposal of filter cake and to small savings in energy due to the
elimination ofwash water at the filters and to the availability of all the
bagacillo as fuel. Reduction in sucrose losses are expected and this
can add to the financial gains.

On the negative side a scale and sampling equipment are necessary if,
like in South Africa, the sucrose input is calculated from mixed juice
and bagasse, for cane payment purposes. There will then be an initial
capital cost with a running cost for the maintenance, sampling and
analytical requirements. All financial analyses done at this stage show
encouraging results.

3.8 Instrumentation

Recent work in South Africa has resulted in the development of

instruments to measure the clarity of juices in the factory (Stone,
1994), and to measure the consistency of the muds (Gooch, 1994).
Both instruments are designed to work in line at the factories and are
used to monitor juice, filtrate or mud qualities.
 BIBLIOGRAPHY

Agius V, Attard R, Paxton T and Shuttlewood L (1977). Areas for improvements in rotary vacuum
screen filter performance. Proc Queensland Sugar Cane Technol 44, 277-281.

Cullen R N (1967). Pneumatic separation and conveying of bagacillo. Proc Queensland Sugar Cane
Technol34, 161-174.

Gooch M A (1994). The development of a method to measure clarifier mud consistency. S Afr Sug
Technol Ass 68, 87-90.

Ivin P C and Cullen R N (1976). Characteristics of a Louvre-type bagacillo separator. Proc

Queensland Sugar Cane Technol 43, 241-247.

Kruger G P N (1984). The application of a horizontal vacuum belt filter to smuts dewatering and cane
mud filtration. S Afr Sug Technol Ass 58, 34-38.

Lionnet G R E (1996). Mud filtration. S Afr Sug Technol Ass 70, 280-282.

Lionnet G R E (1983). The specific cake resistance of South African filter muds. Int Sug J, Vol 86,
80-83.

Lionnet G R E (1984). Mud conditioning for good filter operation. S Afr Sug Technol Ass 58,39-41.

Meadows D M, Schumann G T and Soji C (1998). Farewell to filters: the recycle of clarifier muds
to the diffuser. S Afr Sug Technol Ass 72, 198-243,

Nix K J (1970). Bagacillo for rotary vacuum filters. Proc Queensland Sugar Cane Technol 37, 249-
255.

Sanders R R, Getaz M A and Arthur T (1995). Filter station performance improvements at

Noodsberg. S Afr Sug Technol Ass 69, 155-158.

Stone V C (1994). The development of an instrument to measure the optical density of juice from a
clarifier. S Afr Sug Technol Ass 68, 83-86.
SUGAR TECHNOLOGY FOR STUDENTS COURSE UNITS

1 Clarification
2 Filtration
3 Chemistry of cane and juices
4 Chemical control

In preparation:-

Evaporation
Diffusion
Crystallisation
Pan boiling
Carbonatation (refining)
Sulphitation (refining)
Phosphatation (refining)