EXTRACTION

and
SUGAR INDUSTRY
APPLICATIONS
EXTRACTION

1-LEACHING(SOLID EXTRACTION)

a) GENERAL INFORMATION

b) FACTORS INFLUENCING THE RATE OF EXTRACTION

c) LEACHNG EQUPMENT

2- LIQUID-LIQUID EXTRACTION

a) EXTRACTION PROCESS

b) CLASSIFICATION OF EXTRACTION EQUIPMENT

- STAGE-WISE EQUIPMENT FOR EXTRACTION

- DIFFERENTIAL CONTACT EQUIPMENT FOR EXTRACTION

EXTRACTION IN SUGAR INDUSTRY APPLICATIONS

1- THE FXED-BED OR ROBERT DFFUSON BATTERY

2- CONTNUOUS DFFUSON BATTERES

 EXTRACTION
Extraction is the method of removing one constituent from a
solid or liquid by means of a liquid solvent.Extraction techniques
fall into two categories.The first is called leaching or solid
extraction and the is second called liquid extraction.
 LEACHING (SOLID
EXTRACTION)
A-GENERAL INFORMATION
Leaching is concerned with the extraction of soluble constituent
from a solid by means of a solvent.The process may be used
either for the production of a concentrated solution of a valuable
solid material,or in order to remove an insoluble solid ,such as a
pigment ,from a soluble material with which it is contaminated.
B-FACTORS INFLUENCING THE
RATE OF EXTRACTION
The selection of the equipment for an extraction process is
influenced by the factors which are responsible for limiting the
extraction rate.There are four important factors to be considered:

Particle size: The smaller the size ,the greater is the interfacial
area between the solid and liquid,and therefore the higher is the
rate of transfer of material and the smaller is the distance the
solute must diffuse within the solid.
Solvent:The liquid chosen should be a good selective solvent and
its viscosity should be sufficiently low for it to circulate freely.
Temperature:In most cases,the solubility of the material which is
being extracted will increase with temperature to give a higher
rate of extraction.Further ,the diffusion coefficient will be expected
to increase with rise in temperature and this will also improve the
rate of extraction.
Agitation of the fluid:Agitation of the solvent is important
because this increases the eddy diffusion and therefore the
transfer of material from the surface of particles to tha bulk of the
solution.
 LEACHNG EQUPMENT
When the solids form an open ,permeable mass
throughout the leaching operation ,solvent may be
percolated through an unagitated bed of solids.With
impermeable solids or materials that dissintegrate during
leaching,the solids are dispersed into the solvent and are
later separated from it.Both methods may be either batch
or continuous.
Leaching by percolation through stationary solid beds

Stationary solid-bed leaching is done in a tank with a

perforated false bottom to support the solids and permit
drainage of the solvent.Solids are loaded into the
tank,sprayed with solvent until their solute content is
reduced to the economical minimum,and excavated.
In some cases the rate of the solution is so rapid that one
passage of solvent through the material is sufficient ,but
countercurrent flow of solvent through a battery of tanks is more
common.In this method, fresh solvent is fed to the tank
containing the solid that is most nearly extracted;it flows through
the several tanks in series and is finally withdrawn from the tank
that has been freshly charged.such a series of tanks is called an
extraction battery.
 Moving-bed leaching

In the machines that are used for this type of

leaching, the solids are moved through the solvent with
little or no agitation.The bollman extractor (figure a)
contains a bucket elevator in a closed casing.There are
perforations in the bottom of each bucket.At the top
right-hand corner of the machine ,the buckets are
loaded with flaky solids such as soybeans and are
sprayed with appropriate amounts of half miscella as
they travel downward.Half miscella is the intermediate
solvent containing some extracted oil and some small
solid particles.As solids and solvent flow cocurrently
down the right-hand side of the machine ,the solvent
extracts more oil from beans.
Simultaneously the fine solids are
filtered out of the solvent, so that clean
full miscella can be pumped from the
right hand sump at the bottom of the
casing.As the partially extracted beans
rise through the left side of the machine
,a stream of pure solvent percolates
countercurrently through them.It
collects in the left-hand sump and is
pumped to the half-miscella storage
tank.Fully extracted beans are dumped
from the buckets at the top of the
elevator into a hopper from which they
are removed by paddle conveyors.

Bollman extractor
 In the Rotocel extractor,illusrated
in figure b, a horizontal basket is
divided into walled compartments
with a floor that is permeable to the
liquid.The basket rotates slowly
about a vertical axis.Solids are
admitted to each compartment at
the feed point;the compartments
then successively pass a number of
solvent sprays, a drainage section,
and a discharge point at which the
floor of the compartment opens to
discharge the extracted solids.The
empty compartment moves to the
feed to point to receive its next load
of solids.To give countercurrent
extraction, fresh solvent is fed only
to the last compartment before the
discharge point, and the solids in
each preceeding compartment are
washed with the effluent from the Rotocel extractor
succeeding one.
 Dispersed solid leaching

Solids that form impermeable beds, either before or during

leaching , are treated by dispersing them in the solvent by
mechanical agitation in a tank or flow mixer.The leached residue is
then separate from the strong solution by settling or filtration.
Small quantities can be leached batchwise in this way in an
agitated vessel with a bottom drawoff for settled residue.
LIQUID-LIQUID EXTRACTION
The separation of the components of a liquid mixture by
treatment with a solvent in which one or more of the desired
components is preferentially soluble is known as liquid-liquid
extraction. In this operation, it is essential that the liquid-mixture
feed and solvent are at least partially if not completely immiscible
and, in essence, three stages are involved:

1-Bringing the feed mixture and the solvent into intimate

contact,
2-Seperation of the resulting two phases,
3-Removal and recovery of the solvent from each phase.

It is possible to combine stages 1 and 2 into a single piece

of equipment such as a column which is then operated
continuously. Such an operation is known as differential
contacting. Liquid-liquid extraction is also carried out in
stagewise equipment, the prime example being a mixer-
settler unit in which the main features are the mixing of the
two liquid phases by agitation, following by settling in a
separate vessel by gravity.
 Important applications of liquid-liquid extraction
include the separation of aromatics from kerosene-based
fuel oils to improve their burning qualities and the
separation of aromatics from paraffin and naphthenic
compounds to improve the temperature-viscosity
characteristics of lubricating oils. It may also be used to
obtain, for example, relatively pure compounds such as
benzene, toluene, and xylene from catalytically produced
reformates in the oil industry, in the production of
anhydrous acetic acid in the extraction of phenol from coal
tar liquors, and in the metallurgical and biotechnology
industries.
 EXTRACTION PROCESSES
All liquid-liquid extraction operations, may be carried out either
as a batch or continuous process.
In the single-stage batch process illustrated in the figure, the
solvent and solution are mixed together and then allowed to
separate into the two phases-the extract E containing the required
solute in the added solvent and the raffinate R, the weaker solution
with some associated solvent. With this simple arrangement mixing
and seperation occur in the same vessel.

Fig.single-stage batch extraction

 A continuous two-stage operation is shown in figure, where the
mixers and separators are shown as separate vessels.

Fig.Multiple-contact system with fresh solvent

 CLASSIFICATION OF
EXTRACTION EQUIPMENT
Essentially there are two types of design by which effective
multistage operation may be obtained:

1-Stage-wise contactors, in which equipment includes a series

of physical stages in which the phases are mixed and separated,
and;
2-Differential contactors, in which the phase are continuously
brought into contact with complete phase separation only at the
exits from the unit.
STAGE-WISE EQUIPMENT FOR
EXTRACTION
The mixer settler

In the mixer-settler, the solution and solvent are mixed by some

form of agitator in the mixer, and then transferred to the settler
where the two phases separate to give an extract and a
raffinate. In the settler the separation is often gravity-
controlled, and the liquid densities and the form of the
dispersion are important parameters.
 Combined mixer-settler units
Recent work has emphasised the
need to consider the combined mixer-
settler operation.Thus WARWICK and
SCUFFHAM give details of a design,
shown in the figure in which the two
operations are effected in the one
combined unit. The impeller has swept-
back vanes with double shrouds, and
the two phases meet in the draught
tube. A baffle on the top of the agitator
reduces air intake and a baffle on the
inlet to the settler is important in
controlling the flow pattern.This
arrangement gives a good performance
and is mechanically neat. Figure.Mixer-settler
 The segmented mixer-
settler.In segmented mixer-
settler specially designed
KnitMesh pads are used to
speed up the rate of
coalescence. The centrally
situated mixer is designed to
give the required hold up,
and the mixer is pumped at
the required rate to the
settler which is formed in
segments around the mixer,
each fed by individual
pipework.
Figure.Segmented mixer-settler
 Kuhni have recently
developed a mixer-
settler column which is
a series of mixer-
settlers in the form of a
column. The unit
consists of a number of
stages installed one on
the top of another,
each hydraulically
separated, and each
with a mixing and
settling zone as shown
in the figure. Fig.Khni mixer-settles column
 Baffle-plate columns
These are simple cylindrical columns provided with baffles to
direct the flow of the dispersed phase, as shown in the figure. The
efficiency of each plate is very low, though since the baffles can
be positioned very close together at 75-150 mm, it is possible to
obtain several theoretical stages in a reasonable height.

Figure.Baffle-plate column
 The Scheibel column
One of the problems with perforated plate and indeed packed
columns is that redispersion of the liquids after each stage is very
poor. To overcome this, SCHEIBEL and KARR introduced a unit,
shown in the figure, in which a series of agitators is mounted on a
central rotating shaft. Between the agitators is fitted a wire mesh
section which successfully breaks up any emulsions.

Figure.Scheibel column
DIFFERENTIAL CONTACT EQUIPMENT FOR
EXTRACTION
Spray columns

Two methods of operating spray columns are shown in next

figure. Either the light or heavy phase may be dispersed. In the
former case (a) the light phase enters from a distributor at the
bottom of the column and the droplets rise through the heavier
phase, finally coalescing to form a liquid-liquid interface at the
top of the tower. Alternatively the heavier phase may be
dispersed, in which case interface is held at the bottom of the
tower as shown in (b). Although spray towers are simple in
construction, they are inefficient because considerable
recirculation of the continuous phase takes place. As a result
true countercurrent flow is not maintained and up to 6 m may
be required for the height of one theoretical stage.
Figure.Spray towers
Packed columns

The packing increasing the interfacial area, and considerably

increases mass transfer rates compared with those obtained
with spray columns because of the continuous coalescence and
break-up of the drops. Packed columns are unsuitable for use
with dirty liquids, suspensions, or high viscosity liquids. They
have proved to be satisfactory in the petroleum industry.
Rotary annular columns and
rotary disc-columns

With these columns

mechanical energy is provided
to form the dispersed phase.
The equipment is particularly
suitable for installations where
a moderate number of stages
is required, and where the
throughput is considerable. A
well dispersed system is
obtained with this
arrangement. The figure
shows a rotary annular
column. Figure.Rotary annular column
Pulsed columns

In order to prevent coalescence of the dispersed drops,

VAN DUCK and others have devised methods of providing
the whole of the continuous phase with a pulsed motion.
This may be done, either by some mechanical device, or by
the introduction of compressed air.
The pulsation markedly improves performance of
packed columns. There are advantages in using gauze-type
packings since the pulsation operation often breaks ceramic
rings.Pulsed packed columns have been used in the nuclear
industry.
Centrifugal extraction

If separation is difficult in a mixer-settler unit, a centrifugal

extractor may be used in which the mixing and the separation
stages are contained in the same unit which operates as a
differential contactor.
In the Podbielniak contactor,the heavy phase is driven
outwards by centrifugal force and the light phase is displaced
inwards. Referring to the next figure, the heavy phases enters
at D, passes to J and is driven out at B. The light phase enters
at A and is displaced inwards towards to shaft and leaves at C.
The two liquids intermix in zone E where they are flowing
countercurrently through the perforated concentric elements
are separated in the spaces between. In zones F and G the
perforated elements are surfaces on which the small droplets of
entrained liquid can coalesce, the large drops then being driven
out by centrifugal force.
Figure.Podbielniak contactor
 The Alfa-Laval contactor shown in the
figure, has a vertical spindle and the
rotor is fitted with concentric cylindrical
inserts with helical wings forming a
series of spiral passages. The two
phases are fed into the bottom, the
light phase being led to the periphery
from which it flows inwards along the
spiral, with the heavy phase flowing
countercurrently. High shear forces are
thus generated giving high extraction
rates.

Fig.Working principle of
Alfa-Laval centrifugal
extractor
 EXTRACTION IN SUGAR
INDUSTRY APPLICATIONS
Extraction is needed for sucrose extraction from beets
and cane.
Beets are washed and seperated from any remaining beet
leaves before processing.
The processing starts by slicing the beets into thin chips.
The slicing is done with sharp knives which cut a V selection
slice 4 to 5 mm thickness to increase the surface area of the
beet to make it easier to extract the sugar.
The extraction takes place in diffusers. The two well
known diffusers for sucrose extraction are The fixed-bed
or Robert diffusion battery and Continuous diffusion
batteries or Silver continuous diffuser.
 THE FXED-BED OR ROBERT
DFFUSON BATTERY
This was developed primarily in the beet-sugar industry, but is
also used for the extraction of tanning extracts from tanbark,
for the extraction of certain pharmaceuticals from barks and
seeds, and similar processes. It consists of a row of vessels filled
with the material to be extracted and through which water flows
in series.The piping is so arranged that the fresh water comes in
contact with the most nearly extracted material, and the strongest
solution leaves from contact with the fresh material.Since each
cell is filled and discharged completely ,
one at a time, each cell in the battery changes its position in the
cycle,and therefore the piping must be so arranged that water can
be fed to any cell, and the thick liquor drawn off from any cell, as
circumstances may dictate.The arrangement of valves and piping
became standardized in the beet industry and is generally found
an all forms of diffusion battery. Figure shows that is a
diagrammatic illustration of the principle of a diffusion battery.For
every vessel or cell there is a heater, because the diffusion
process takes place more rapidly at higher temperatures.Two main
headers are necessary .One handles water and the other handles
solution;and for every cell there must be three valves.In figure
shows that the valves that are open are shown as circles and the
valves that are closed are shown in solid black.
Fig.Diagram of diffusion battery
Consider figure; Cell 1 is nearly exhausted and the cell 3 has just
been charged.The space between the cossettes in cell 3 is
therefore filled with air.Water is introduced into cell 1 and flows
down through cell 2, and up through its heater.It would not be
convenient to pass the solution down through cell 3 because of
the air which would be entrapped;and the charge is cold,
therefore additional heating is desirable.Consequently, the liquid
flows from the heater of the cell 2 through the solution line, down
through the heater of cell 3,and up through cell 3. A vent at the
top of this cell discharges air.When liquid appears at this vent,
the valves are quickly changed to the position shown in
figure.Liquid now flows down through cell 3, up through its heater,
and out t the process.The operation shown in figure continued
until cell 1 is completely extracted.By this time another cell to the
right of those shown has been filled, cell 1 is dumped, water is
introduced to cell 2, and the process continued.In a diffusion
battery for beet cossettes there may be from 10 to 15 cells.
 CONTNUOUS DFFUSON
BATTERES

The next figure shows the Silver Continuous diffuser.The figure

shows only three units; but actually the battery consists of 20 to
24 units arranged in two tiers, one above the other.The battery
consists essentially of a series of closed troughs A,A,A, each
provided with a helical screw B.Cossettes are intoduced into the
battery through chute C and are carried together with the liquid in
the direction indicated by the arrows.At the end of the first trough is
a Wheel D with inclined perforated buckets on the inside.It is so
arranged that the screw B discharges the cossettes into this wheel,
where they are picked up by the buckets;drained free from juice
lifted, and discharged through chute E which takes them into the
second trough A. Here the helix carries them in the opposite
direction discharges them from this to another wheel which in turn
forwards them to another trough A, and so on until they are
exhausted and leave the battery.
Silver continuous diffuser:A,A,A, extraction trougs;
B,conveyor for moving cossettes; C, feed chute; D, transfer
Wheel; E, transfer chute for chips.