STRA

SULPHUREX F
Continuous S03 sulphonation and sul-
phation plant for detergent alkylates,
fatty alcohols, ethoxylated alcohols, al-
pha-olefins, methylesters etc.

INTRODUCTION 3

PLANT LAY-OUT 5

PROCESS BLOCK DIAGRAM 7

AIR DRYING 8

S03 PRODUCTION 12

FILM SULPHONATION 16

NEUTRALIZATION 22

EXHAUST GAS TREATMENT 24

CONTROL SYSTEM 26

PLANT INSTALLATION 28

PLANT SKID-MOUNTING 28

OVERALL PLANT DIMENSIONS 28

BALLESTRA S.p.A.
Via P. Portaluppi, 17 - 20138 MILANO - Italy - Tel.: +39 02 50831 - Fax:+39 02 58013221/5083327 - Tx: 311519INGBA1 - E-Mail: [email protected]
INTRODUCTION

The technology of S03 converter gas sulphonation Today's concept of "product quality" is associated
was first introduced on the market by Mr. Mario with the precision and reliability of the control of
Ballestra in the late 50's. The original concept has the process. Ballestra has accordingly developed a
remained substantially unchanged up to the pre- computer process control system that ensures
sent day. The technology is based on the use of easy and reliable plant operation also for plant
gaseous S03 (the sulphonating agent), which is start-up, shut-down and product change-over.
produced from elemental sulphur, in a continuous
reaction, at a controlled mole ratio, with organic Ever since it was first introduced, the Sulphurex F
feedstock materials such as detergent alkylates, plant has represented the process plant of refer-
fatty alcohols, fatty ethoxylated alcohols, fatty ence for the production of Anionic Surfactants in
acids and their esters, alpha olefins, etc. line with the most demanding market requests;
more than 200 sulphonation units, based on the
The process was introduced to the surfactants Ballestra Multitube Film Reactor (in a range of
and detergent industry under the trade name production capacity from 50 to 10000 kg/h),
SULPHUREX. have been put successfully into operation.

The basic feature of the original Sulphurex plant The main features of the standard Sulphurex F
was the reaction section, which consisted of a cas- plant, its performances and the available options
cade of stirred tank reactors, where the gaseous for the plant configuration are described in this
reactant (S03 diluted in air) is fed in parallel to brochure.
each reactor at a pre-set rate and the organic feed
enters the first reactor and the liquid mass, under However, various other plant configurations, such
steady state running conditions, overflows by as the connection of the Film Reactor
gravity from one reactor to the next. Sulphonation Unit with existing S03 sources (ei-
ther from H2S04 or other sulphonation plants),
The Sulphurex plant is still today a reliable and can be developped according to Client's specific
economical plant for the sulphonation of deter- requirements.
gent raw materials and many plants of this type
are in operation, some from over 30 years. Ballestra services are performed in accordance
with the applicable International Standards/Regu-
In 1980 Ballestra introduced the SULPHUREX F, a lations.
sulphonation plant based on a new Multitube Film
Reactor which is capable of producing sulphonated
or sulphated products of the highest quality, even
those products which are the most difficult and
sensitive to process, such as products for the cos-
metic industry, where clear and bright product are
needed without additional bleaching.

All the process sections of the Sulphurex F plant

have been designed to assure the best possible
quality for the full range of feedstocks.
Multitube Film Reactor n Reactor
S03 Production, Exhaust Gas Treatment and Tank farm
 PROCESS AIR BLOWER

GLYCOL SOLUTION
RECIRCULATINC PUMPS

REFRIGERATING EXCHANGERS
CONTAINER & GLYCOL TANK

REGENERATION EXCI
CONTAINER

REGENERATION
AIR COOLER

SOrSO, CONVERTER 1(
SULPHUR COMBUSTION 1STINTERCOOLER /
*я?л
FURNACE
SULPHUR
tLTING TANK

MOLTEN SULPHUR START-UP „

PROPORTIONING PUMPS PREHEATER 1
MOLTEN SULPHUR
FILTER

COMBUSTION AIR FAN

OLEUM COLLECTING VESSEL ^^ OLEUM FEEDING PUMP

ESP FLUSHING AIR FAN

 SULPHUREX F - Plant for continuous Film
Atmosphere
Sulphonation and Sulphation

Raw material
SULPHONATION MULTITUBE Jl
FILM REACTOR

PROCESS WATER TANK

CAUSTIC SODA TANK

Active
matter

Sulphonic
acid

Effluents
to reprocessing
 FILM SULPH(ON)ATION
Process Block Diagram

| | Final Products
Raw Materials
[ | Process unit

HEAT
RECOVERY

I
SULPHUR S02/S03
PRE-TREATMENT PRODUCTION

'
SULPHONATION
& •*! EXHAUST
GAS
SULPHATION TREATMENT

AGEING
&
STABILIZING

SSING J_
I
2ND STEP 1 caustic
•PING
NEUTRALIZATION! soda

I i
SLES LAB
DEAREATION sulphonic acid

Active Matter
Paste
 Regeneration Ьхспапдег container

Air Dryer and Regeneration Group

SULPHUREX F - Air drying

CHILLING GROUP AIR DF

PROCESS AIR BLOWER

AIR GLYCOL
COOLER

к AIR WATER
* COOLER

GLYCOL SOLUTION
RECIRCULATING PUMPS

REFRIGERATING EXCHANGERS
CONTAINER & GLYCOL TANK

Dry air REGENERATION

to S03 production AIR HEATER

REGENERATION1
AIR COOLER

Hot;
from SO,
 10

AIR DRYING

Air drying is a fundamental step in the sulphona-

tion process. The process air to be used for S03
generation and for its subsequent dilution must
be dehumidified to keep moisture from reacting
with S0 3 which can lead to the formation of
oleum and give rise to such problems as corrosion
and the reduction of sulphonation reaction con-
Atmosphere version yield.

The air required for sulphur combustion and the

production of S03 is filtered and dehumidified to a
dew point which is lower than -70°C.

In the Sulphurex F plant this operation is carried

out as follows:

The air, which is filtered to eliminate dust, flows

to the process air blower, which conveys it to the
cooling unit where it is cooled to about 5°C. The
blower operates at a very low pressure (0.6 bar
gauge max.). This low pressure, however, is suf-
ficient for conveying the air both through the S03
production unit and the sulphonation unit.

The process air-cooling unit consists of a chilling

group and two refrigerating exchangers carrying
cooling water and ethylene glycol at a tempera-
•GEI\ERAT!ON EXCHANGERS
CONTAINER ture of around 0°C. This unit is designed to pro-
vide constant humidity condensation in the
process air, regardless of the existing climatic con-
ditions. At this stage the air is cooled and partially
dehydrated.

The cooled, compressed air is then subsequently

dried with a desiccant (silica gel or alumina) in
Hct air
two parallel absorbers operating in sequence, i.e.
m S03 coolers one on air drying and the other on regeneration.
Switching over from the absorption phase to the
regeneration phase occurs automatically; the time
intervals, however, are constant. Part of the heat
generated by sulphur combustion and the conver-
sion from S02 to S03 can be utilized for regenera-
tion.
 11

The most outstanding characteristics of this

process section are:

- Simple design and mechanical reliability

- Low operating pressure
- Oversized absorption beds for longer operating
cycles
- Lowest dew point with highest energy efficiency
Process Air Blowers Refrigerating Exchangers Container & Glycol Tank

Four Ways Valve Detail

Chilling Group
 12

S03 PRODUCTION

The dried air is conveyed to the sulphur combus- Conversion of S02 to S03 by the above de-
tion furnace where it meets the liquid sulphur in scribed converters is even higher than 99%.
counterflow, and converts it to S02, by burning it.
At plant start-up, the S02 cooler is used to pre-
If sulphur is available as solid the plant is heat the process air so to bring the catalyst to
equipped with a melting tank which is provided the right conversion temperature in a very short
with a set of filters to retain impurities. time (two to three hours).
The sulphur burner does not need to be pre-
Sulphur dosing is carried out by special propor- heated for the start-up operation.
tioning pumps at controlled temperatures, so as
to maintain the viscosity at optimum and constant One great advantage of this plant section is
values. the absence of any diverting or by-pass valves
in the process line where corrosive gas at rela-
Sulphur combustion takes place in a refractory- tively high temperature is produced thus
lined, vertical furnace. After being ignited by eliminating the possibility of leakages and re-
means of a pilot lighter, the sulphur is uniformly lated problems.
distributed over a bundle of refractory balls, with
the combustion air counterflowing over it. This
simple system permits complete sulphur combus-
tion. The diluted sulphur dioxide leaves the sul-
phur combustion furnace at a temperature of
about 650°C, after which it is cooled to about
430°C by means of a S02 cooler.

The S02 at this temperature enters the converter

for oxidation to S03. The converter contains four Molten Sulphur
тщ
layers of special oxydation catalyst interspaced
with coolers which remove the heat of conver-
sion.

Dry air is directly added through the 3rd and 4th

catalyst bed inlet to complete the S02 to S03 con-
version at controlled temperature.

The S03 gas leaving the converter is cooled (nor-

mally with ambient air) below 50°C by one or
more heat exchangers.

The cooling air reaches temperatures higher than

300°C: the heat is recovered for silica gel regen-
eration and/or for other purposes such as steam
generation in a specially designed heat recovery
unit.
 13

Sulphur Melting Tank Sulphur

SULPHUR COMBUSTION
FURNACE
SOZ-SO? Converter SULPHUR
MELTING TANK

MOLTEN SULPHUR
FILTER

MOLTEN SULPHUR
PROPORTIONING PUMPS
 14

SULPHUREX F - S03 production

Dry air
from air dryer

Dry air to
sulpnonation
Hot air to
S02-S0, CONVERTER
1ST1NTERCOOLER

COMBUSTION AIR FAN

OLEUM COLLECTING VESSEL Oleum
OLEUM FEEDING PUMP 'to Scrubber
 15

S02-503 Converter snd S03 Coolers Sulphur CombuL

S0?-S03 Production Unit

 16
EMERGENCY
FEEDING TANK

OFF-SPEC/RAW MATERIAL
STATIC MIXER
SULPHONAT10N MULTITUBE
FILM REACTOR
Raw
material

REACTOR INLET
GAS FILTER

OFF-SPEC/WATER
PROPOTIONING PUMP

PROCESS WATER TANK

Dry air
from
air dryer

S03 from OFF-SPEC TANK

coolers

Water to
neutralization
Oleum
to exhaust gas
treatment
Exhaust gas
to electrostatic
precipitator

RXGAS
EFFLUENTS CYCLONE

Sulphonic acid
to neutralization

GAS/LIQUID COOLING WATER

SEPARATOR RECIRCULATINC PUMP

SULPHONIC ACID
TRANSFER PUMP
AGEING VESSEL
О

Sulphonic acid
to storage

SULPHONIC ACID
SULPHUREX F COOLER

Film sulphonation
 17

FILM SULPHONATION & SULPHATION

The Ballestra continuous S0 3 sulphonation and The self-adjustment (patented worldwide) has
sulphation plant for surfactant production (i.e.: been theoretically and industrially proven for reac-
detergent grade alkylates, fatty alcohols, ethoxy- tors having up to 10000 kg/h capacity to be consis-
lated fatty alcohols, alpha-olefins and fatty acid tently in the range of ± 0.005 of more ratio.
methylesters) is based on a Multitube Film
Reactor of proprietary design. The Mole Ratio Control System

This reactor consists of a vertical bundle of long, Sulph(on)ation process control via optimized
small-diameter tubes, the number of which depends mass balance:
on the plant production capacity. The S03-gas is fed
to the upper part of the reactor and equally distrib- The exact mole ratio between the S03 and the or-
uted to each reaction tube. The organic feedstock and ganic feed is essential for obtaining the maximum
S03-gas are fed co-currently. The liquid film which is degree of conversion and excellent colour with all
formed inside the tubes comes in contact with the types of feedstock.
gaseous reactant. The length and diameter of the
tubes have been optimized through a computer mod- The best theoretical sulphonation yield for a given
el to provide best product quality performance. organic feedstock is obtained by optimizing the
SOa/organic mole ratio and equally distributing
The special design of the Ballestra reactor ensures the reactants in the sulphonation reactor.
accurate dosing of the organic feedstock and S03
gas keeping the exact mole ratio between them. Any excess S03, especially in areas of the reactor
where the cooling is critical, will cause local char-
Each individual tube is machined with utmost me- ring, which will degrade both the product colour
chanical precision so to ensure identical perfor- and the degree of conversion.
mance in gas and liquid flow distribution. Mole Ratio Control System

The liquid flow can be actually checked and fur-

ther adjusted to dosing accuracy within ± 0.5%.
This accuracy is achieved with metal washers and
nozzles of special design which ensure high preci-
sion within the entire range of feedstock charac-
teristics and production capacity.

In addition to these mechanical features which en-

sure as such the best possible geometric distribu-
tion, the reactor design has unique performances
of gas liquid self-adjustment.

Even in case of differences in the liquid flow, the

corresponding gas flow is proportional to the
overall film thickness, which is established by the
viscosity p r o f i l e as a direct f u n c t i o n of the
sulph(on)ation degree in each single tube. PROPORTIONING
PUMP
\~(Щ 'TRANSFER
PUMP
 18

Sulphurex F, Top of Reactor

Sulphurex F Plant Sulphurex F Plant

 19

so3 gas Multitube

j—, Film Reactor

Organic feed

Cooling
water

_к Cooling
water
\A/ator

Product and exhaust gas

 20

In fact, optimum conversion of raw material to The sulphonic acid and exhaust gas leaving the re-
sulphonate is nearly a direct function of mole ra- actor are sent in a high efficiency gas liquid sepa-
tio, while at mole ratios even slightly higher than rator and cyclone.
optimum (usually in the range of 1.02-1.05 mole
S03 to 1 mole organic), the product darkens
rapidly and coloured by-products are generated. let Gas Filter and MFR Head

To further improve product quality Ballestra has de-

veloped and successfully implemented an SO/or-
ganic Mole Ratio Control System based on the use
of mass flow meters.

This system operates as follows:

The mass flow of organic feedstock to the film

reactor is detected by a mass flow meter which
automatically controls the speed of the feeding
pump.

The sulphonic acid flows with a delay of few

seconds through a second mass flow meter.
The ratio between the mass flows of sulphonic
acid and the organic feedstock is measured and
computed, according to the relevant molecular Mulmuue rum неасюг
weights, as the actual mole ratio of the
reagents. In fact the quantity of absorbed/re-
acted S03 corresponds to the net difference be-
tween the two measured mass flows. The re-
quired mole ratio is maintained by adjust-
ment/reset of the organic mass flow.

The system is therefore also independent of any

fluctuations of the S02 / S03 conversion yield.

The flow of gas and liquid inside the reactor is paral-

lel. The liquid phase forms the film on the inner sur-
face of each tube, and the gas flows through the
tubes at a very high speed. The outside of the tubes,
the shell side, is provided with cooling to ensure a
correct reaction temperature. The cooling water
temperature is precisely controlled to provide the
best values for each specific type of feedstock and
each area of the reactor, considering that the reac-
tion takes place at a very high rate, with about 70
to 80% of the conversion occurring in the first
third of the reactor.
 21

OPERATING CONDITIONS OF BALLESTRA'S MULTITUBE FILM REACTOR

TYPE OF FEEDSTOCK
REACTION PARAMETER
C12-C14 C16-C18 C12-C1S C16-C18 C14-C16
LAB
FA FA 3EOFA ME АО
SOa/organic mole ratio (range approx) 1.01-1.03 1.01-1.02 1.01-1.02 1.01-1.02 1.5-1.20 1.05-1.07

S03 concentration (% vol . ) 5-8 4-5 4-5 2.5-3.5 5-8 2.05-3

Cooling water temperature (C°) 34-36 24-26 45-50 30-32 70-80 15-20

Acid outlet temperature (C°) 45 30-32 50-55 40-42 70-85 38-40

Ageing time (min.) 30-60 - - - 30-60 3-10

Ageing temperature (°C) 50-55 - - - 90 45-50

Hydrolysis temperature (C°) 50-55 - - - - 170-175

The gas is sent to the exhaust gas treatment unit cluding "specialties" such as cosmetic and den-
and then released to the atmosphere. tal-grade fatty-alcohol sulphates.

If for any reason, the flow of organic feedstock to

the reactor is interrupted, an independent emer-
gency system takes over and purges the reactor with
fresh organic. This ensures the complete reaction of
any S03 remaining in the reactor, thus avoiding any
risk of local charring.

A gear pump sends the sulphonated product to

the ageing unit and then to the stabilizing unit
where the reaction is completed. This is what
happens when sulphonating alkylbenzene,
methylesters and alpha-olefins. When sulphating
alcohols, the ageing and stabilization unit is by-
passed and the acid is sent directly to the neutral-
ization unit.

The average operating conditions of the Ballestra

Multitube Film Reactor as regards a wide range of
detergent feedstocks are given in the table shown
on this page.

The Ballestra Multitube Film Reactor system

permits to produce all types of anionic surfac-
tants having the highest quality standards in- Ageing Vessel and Stabilizer
 22

NEUTRALIZATION SULPHUREXF
("NEUTREX")
Neutralization
H20/NaOH
When the sulphonated PROPORTIONING PUMP
product leaves the reactor,
CAUSTIC SODA TANK
it is degassed, and it is ei-
ther pre-treated or immedi-
ately sent to the neutraliza-
tion unit, according to the
type of processed feed-
stock. Active
matter

The neutralization unit is of 1ST NEUTRALIZATION 2ND NEUTRALIZATION

MIXER MIXER
the forced-circulation type
and can be the single or
double-step type.

The single step type is de-

signed to obtain stable neu-
tralized paste without in- NEUTRALIZATION
COOLER
curring the risk of degrada-
Sulphonic acid
tion during the neutraliza- from sulph(on)ation

tion and the need of using

solvents or hydrotropes
during start-up. This com-
pact system includes a spe-
cially-designed multi step
high shear neutralization
mixer which permits ob-
taining an extremely homo-
geneous product with sig-
COOLING WATER
nificant energy economy. NEUTRALIZATION
RECYCLE PUMP :RECIRCULATING
PUMP

The heat of reaction is re-

moved in a loop which consists of a high efficiency stalled when the production program foresees the
cooler and a recycle pump capable of transporting production of pastes at high concentration.
highly viscous pastes. The product is sent to stor- The first mixer is fed with the neutralizing agent,
age under automatic pressure control. The pH is all or most of the sulphonic acid, and all the dilu-
detected and automatically adjusted by acting on tion water. The neutralized mixture (with excess
the piston stroke of a small caustic soda feeder. of alkalinity) is recycled inside this first loop and
cooled to remove the heat of neutralization.
The patented double step type includes two neu-
tralization mixers capable to handle highly viscous The product then flows continuously to the sec-
pastes. This arrangement provides more precise ond neutralization mixer where the balance of
temperature and pH control and is usually in- sulphonic acid and controlled quantity of buffers -
 23

if required - are added to obtain the correct pH

value. This value is automatically controlled by a
pH-meter located on the reactor outlet.

The pH electrodes set-up has been specially devel-

oped for in-line pH measurement of extremely
viscous pastes even at high process temperatures
and pressures. A self-cleaning device allows auto-
matic in-line periodical cleaning for long term reli-
ability.

Single Step Neutralization

Double Step Neutralization

 24

SULPHUREX F Exhaust gas from

cyclone
Exhaust gas
ELECTROSTATIC
treatment PRECIPITATOR

SO, SCRUBBER COLUMN

Oleum from
S03 production

ESP FLUSHING AIR FAN

Effluents
to reprocessing'

S02 SCRUBBER
RECIRCULATING PUMP

EXHAUST GAS TREATMENT

The exhaust gas, containing small amounts of non- The potential difference established between the
converted S02, unreacted S03 and some entrained electrodes and the walls of the tubes electrically
organic acid, has to be cleaned before emission to charges the impurities located in the gas stream.
ambient atmosphere. These forces cause the particulates to migrate to-
The organic aerosol and fine S03/ H2S04 droplets ward the positive anode (the tube wall) where
are first separated from the exhaust gas flow in they coalesce on the surface and drain off under
an electrostatic precipitator (ESP) and re- the influence of gravity.
processed in the plant.
The ESP consists of a bundle of tubes mounted The gaseous stream containing the residual un-
vertically with each tube containing an axially- converted S02 is then treated in a packed scrub-
mounted electrode. ber column, where water and caustic soda solu-
 25

tion are continuously added and recycled. The S02 continuously recirculated to the column and is
reacts with the caustic soda to give sodium sul- overflowed to the downstream oxidation unit.
phite, which is discharged as aqueous solution.
The feeding of the caustic soda solution is done Part of the NaHS03 which is oxidized to NazS04 by the
automatically and is controlled so as to maintain excess of air contained in the exhaust gas, is then dis-
the scrubber liquor at the required pH. charged from the scrubbing column at about 10%
concentration and constant pH (about 8.5).
This reaction is performed by means of a specially The amount discharged is directly proportional to
designed packed column where intimate contact the amount of non converted S02. The clean, water-
between the gas and liquid phases is obtained saturated gas is then discharged to the atmosphere.
countercurrently.
The liquid enters the top of the column and flows The maximum content is 5 ppm vol. of S02,15
downward through the column, which is filled with ppm vol. of S03, 25 mg /m3 of organic aerosol
plastic rings to ensure sufficient surface contact and absence of visible plume. Enhanced effi-
and avoid the formation of preferential pathways ciency, for a max value of 5 ppm of total SOx
of the liquid through the bed. (S02 + S03 + RS03H) can be achieved with ad-
The liquid leaving the bottom of the column is ditional high efficiency gas demisters.
Exhaust Gas Treatment Unit
 26

CONTROL SYSTEM

The Plant standard Computer Control System All commands can be given by means of trackball
contains the following main components: or keyboard to manage the following functions:

- a PIC with control function • Motors:

- two or more operating stations, each consisting - start
of one personal computer and one printer -stop
- second speed change
The software has the following standards:
- reset of the operating status after an alarm
- at PLC level, "Ladder Logic" type programming
package • On/off valves:
- at PC level, DOS operating system and Logoview - opening, closing
32 standard software by LOGOSYSTEM a - reset of the operating status after an alarm
Ballestra syster company specialized in process
control S/H, at software application level, a fully • PID Control loops:
standardized and tested application package, - Automatic: set point change directly on screen
which is integrated between the PLC software lay-out
and the Logoview 32 and carries out control - Manual: direct command of the inlet variable
and plant operator's interface operations
Each controller can be set and tuned for high/low
The hardware cabinet contains the PLC, the auxil- action limits of the I/O variables, for actual set
iary circuits and the field instruments terminal point and relevant PID AUTO/MANUAL actions in
board. dedicated video pages.
The cabinet has "IP 51" protection and is immedi-
ately field-linkable to all instruments and trans- The plant is started up with manual/automatic se-
mitters. quences and local or remote actuated actions.
The PLC cabinet can be installed in the control
room or near the Motor Control Center. In steady normal operation, the plant is under PID
The desk-top PC's have to be installed in the con- loop control for what concerns the main process
trol room together with their relative printers. parameters relevant to mass/energy control.

The software performs the following functions: The control system does also perform automatic
(batch) sequences such as the dryer regeneration
- plant control by means of interlocks
cycles and all emergency / interlock procedures
- P1D control loops and automatic sequences
for operation and safety protection.
(such as of silica gel regeneration) and emer-
gency sequence
The plant design and relevant process control sys-
- screen lay-outs, which allow the remote control
tem ensures in case of emergency plant shut-
and survey of the plant during start-up, normal
down redundant and intrinsical safety without
operation and shut-down conditions and allow
need of back up/power generators.
dealing with alarm situations

The operator's interface has a sufficient number The computer system is nevertheless complete
of screen graphic layouts in colour which repre- with UPS which allows additional monitoring and
sent the process P&I. data logging in case of power failure.
 27

When the control and supervision system is in The system can supply reports relevant to alarms,
operation, all variables are visible in the screen performed production, raw materials consump-
lay-outs in real time in numeric form; the alarm tion etc.
condition of the plant components and the devia- The operator can set the plant's main control pa-
tion of the pre-set values of the same variables is rameters (instruments full scale, limits and
shown by means of the colour change of graphic alarms qualification, etc.) by means of password
symbols and numerical indications. protected procedures.

Motor Control Cente Computer Operators

Computer Control Room

 28

PLANT INSTALLATION PLANT SKID-MOUNTING AND

MODULARIZATION
The sulphonation plant can be installed in a single-
story covered area. The sulphonation plant is The Ballestra sulphonation plant can be mounted
completely self-supported. The area required is on skids and what little equipment which is not
indicated in the table herebelow. skid-mounted can be preassembled and checked-
out in the workshop so as to facilitate the on-site
Ballestra has taken extra care in studying the opti-
installation.
mum layout of the equipment so as to provide the
following advantages:
The on-site assembly of the skid-mounted plant is
quite a simple matter, since limited welding is re-
- reduced construction costs and improved ener-
quired and most connections are of the bolted
gy saving through the reduction of the required
flange type.
handling of raw materials and finished products
- easy access for equipment maintenance
The number and size of the skids are determined
- reduction of overall building size
on the basis of the shipping requirements.
In most cases only the sulphonation and neutraliza-
tion units together with control room and air com- In general, skid mounting includes:
pressors are installed inside a building or under a
covered structure; most of the plant and particular- - steel skid frame
ly the S03 production and the exhaust gas treat- - complete mounting of equipment on the skid,
ment units can be installed outdoors, as shown in including process and utilities piping, valves and
pictures of page 4,8 and 15. piping support brackets
- installation of cable trays and conduits, instru-
If required the plant could also be installed com- ments, electrical control equipment (where ap-
pletely outdoor. In this case, however, it is always plicable) and accessories
advisable to provide a shelter for the electrical -thermal insulation
control panel, sulphonation unit and neutraliza- -final painting
tion unit.
The piping connections between the skids and the
Ballestra can also provide alternative equipment lay- plant battery limits are supplied prefabricated.
outs for setting up the plants in existing building al-
so with different floor levels.

OVERALL PLANT DIMENSIONS

Sulphurexiype A-B C-CD D-DE DEE EG GH-H L-M

Plant Capacity
300-500 800-1000 1600-2000 3000 3800 5000-6000 8000-10000
kg/h

Plant surface area

450 560 740 770 1000 1400 1950
m2

Max free height

11 12 12 14.5 15 15 15
m
INDEX
Reference list

Plant performances
Sulphites oxidation

Alpha-olefins hydrolysis
Heat recovery
S03 absorption
Sulphur melting and pre-treatment
Sles paste deaeration
Sles paste degassing / stripping

Ю Vacuum neutralization

TT Active matter drying unit

SOs FILM
so
SULPHONATION =9as
л
Multitube
Film Reactor

Organic feed

Cooling
water

.л Cooling
T' water
\A/ator

Product and exhaust gas

BALLESTRA S.p.A.
VIA P. PORTALUPPI, 17 - 30138 M1LANO - ITALY - TEL.: +39 02 50831
FAX:+39 02 58013221/5083327 - TX: 311519INGBAI - E-Mail: [email protected]

May 1999
S0 3 FILM SULPHONATION PLANTS
SULPHUREX F
Continuous SCb sulphonation and sulphation 1600 A N H U I IMPORT CORP. CHINA
plant of detergent alkylates, fatty alcohols, 1600 * PORT SAID DET. & CHEM. EGYPT
1600 THE EGYPTIAN STARCH EGYPT
ethoxylated alcohols, alpha-olefins etc., based 3000 CONFIDENTIAL INFORMATION E N G L A N D
on Ballestra Multitube Film Reactor. 3500 CONFIDENTIAL INFORMATION E N G L A N D
2000 CHIMCOMPLECT BULGARIA
2000 CHIMCOMPLECT BULGARIA
2000 PING HE ELECTRONIC CO. CHINA
Kg/h 50 COLGATE PALMOLIVE ITALY
4000 ITALSILVA ITALY
250 SAPONERIE F. LAZZERI ITALY 800 ITALSILVA ITALY
800 PANIGAL ITALY 300 COLEMUL COLOMBIA
500 SAPONERIE F. LAZZERI ITALY 2000 BEHDASH IRAN
500 BASER KIMYA TURKEY 5000 U N G E R FABRIKKER A.S. NORWAY
3000 MINTAX TURKEY 3500 HENKEL GERMANY
1500 U N I L E V E R ITALY 3500 H E N K E L GERMANY
50 INTERQUIMICA D O M I N I C A N REP. 100 HENKEL GERMANY
2000 LA CORONA MEXICO 1000 * MANYAR KIMINDO INDONESIA
300 U N I L E V E R THAILAND 3000 CONFIDENTIAL I N F O R M A T I O N GERMANY
1500 HULS GERMANY 1500 LUCKY KOREA
300 DA! ICHI KARKARIA INDIA 1500 LUCKY KOREA
2500 SHELL AEKYUNG KOREA 2000 SHELL ENGLAND
1500 LUCKY KOREA 2000 SHELL HOLLAND
1500 LUCKY KOREA PILOT ESSO FRANCE
1200 PANIGAL ITALY 1600 REWO GERMANY
300 COLGATE PALMOLIVE U.S.A. 3500 CONFIDENTIAL INFORMATION FRANCE
2000 TENSIA BELGIUM 3500 CONFIDENTIAL INFORMATION FRANCE
500 ANTILLES CHEM.MAN.CO. TRINIDAD 2000 FURAT IRAQ
1000 H E N K E L CHIMICA ITALY 1000 SERVO DELDEN HOLLAND
800 CHIMCOMPLECT BULGARIA 1000 GLOBAL SOAP & DETERGENT NIGERIA
100 * U N I C H E M PHILIPPINES 3000 AEKYUNG AND SHELL CO. KOREA
2000 H E N K E L TURKEY (*)TOYO MENKA KAISHA JAPAN
2000 TECHMASHIMPORT U.S.S.R. 3000 CONFIDENTIAL INFORMATION ITALY
150 ALKI TUNISIA 3000 WITCO CHEMICAL FRANCE
500 ITALSILVA ITALY 4000 D.A.C. ITALY
1600 * ROBERT CHEMICALS NEW ZEALAND 300 D.A.C. ITALY
500 MINTAX TURKEY 3000 CONFIDENTIAL INFORMATION AUSTRALIA
2500 COLGATE PALMOLIVE MEXICO 2000 HENKEL BRAZIL
2500 COLGATE PALMOLIVE MEXICO 500 HENKEL BRAZIL
1000 HUBEI IMPORT CO. CHINA 1600 HULS GERMANY
1000 SHANDONG I N T E R N A T I O N A L CHINA 3000 MANYAR K I M I N D O INDONESIA
1500 SHANXI I N T E R N A T I O N A L CHINA HSHANXI I N T E R N A T I O N A L CHINA
1000 SNIC ALGERIA 500 HOECHST BRAZIL
1000 SNIC ALGERIA 500 MASSOY CAROL SPAIN
1000 SNIC ALGERIA 1500 S.E.V.O. IRAQ
1500 ALEXOIL EGYPT 2000 YU KUO CHEMICAL R.O.C.
1000 EGYPTIAN I N D . FOR (*)CONFIDENTIAL INFORMATION PHILIPPINES
SYNT. DET. EGYPT 1600(*)CONFIDENTIAL INFORMATION PHILIPPINES
1000 JORDAN SULPHO-CHEM. JORDAN 1000 ELTAYASAL GUATEMALA
3000 * COLGATE PALMOLIVE PHILIPPINES 2000 * GULF CHEMICAL U.A.E.
300 * COLGATE PALMOLIVE PHILIPPINES 3000 SHELL GERMANY
300 PHILIPPINE R E F I N I N G CO. PHILIPPINES 2000 CONFIDENTIAL INFORMATION PHILIPPINES
3000 PHILIPPINE R E F I N I N G CO. PHILIPPINES 2000 PROCTER 8 GAMBLE ITALY
2000 * HOUSEHOLD PRODUCTS I N D . NIGERIA 5000 CONFIDENTIAL INFORMATION INDONESIA
1000 CHINA HUNAN PROV.IMP.CORP. CHINA 1600 S.E.V.O. (RASHID) IRAQ
1000 CHINA HUNAN PROV.IMP.CORP. CHINA 3000 S.E.V.O. (MAMOUN) IRAQ
500 GODREJ SOAPS INDIA 2000 GODREJ INDIA
500 COLGATE PALMOLIVE MALAYSIA 1600 COLDEQUIM COLOMBIA
2000 CHINA NAT.TECH.IMP.CORP. CHINA 150 U N I T E D COCONUT CHEMICALS PHILIPPINES
1000 C H I N A NAT. MACHINERY CHINA 3000 ALBRIGHT & WILSON ENGLAND
3000 * COLGATE PALMOLIVE AUSTRALIA (*)HENKEL GERMANY
1500 SICHUAN PROV. I M P . CHINA 2000 PAKNAM IRAN
2000 * YEMEN COMPANY Y.A.R. 3000 CHEMSAL GERMANY
1000 XIAN INT. ECONOMIC TECH. CHINA 9000 CONFIDENTIAL I N F O R M A T I O N BRAZIL
1000 LA FAVORITA EL SALVADOR 1500 CONFIDENTIAL I N F O R M A T I O N U.S.S.R.
1600 C H I N A O R I E N T LEASING CO. CHINA (*)CHEIL FOODS & CHEMICAL Co. KOREA
150 * H E N K E L AUSTRIA 1000 C O N F I D E N T I A L I N F O R M A T I O N PAKISTAN
3000 SINOPEC I N T E R N A T I O N A L CHINA 1400 ROYAL I N D . DEV. Co. PHILIPPINES
3000 SAYAP MAS UTAMA INDONESIA 3000(*)PAXAN IRAN
S0 3 FILM SULPHONATION PLANTS
SULPHUREX F
2000 PARS INTERNATIONAL IRAN 500 TUDAB ENG. CO. NIGERIA
750 О COLGATE PALMOLIVE MEXICO 5000 CONFIDENTIAL INFORMATION INDONESIA
1000 BEHDASH CHEMICAL Co. IRAN 6000(^CONFIDENTIAL INFORMATION U.S.A.
2000 ECO CONSULT ENGINEERING CSFR 12000 CONFIDENTIAL INFORMATION EUROPE
4500 CONFIDENTIAL INFORMATION BRAZIL Pilot CONFIDENTIAL INFORMATION EUROPE
1000 HENKEL INDONESIA 1600 OZHAN KYMIA TURKEY
(*)CIABASA ARGENTINA 5000 CONFIDENTIAL INFORMATION SPAIN
3000 * CONSOLIDATED SUIJPHOCHEMICALIND. JORDAN 2000 CONDEA CHIMICA D.A.C. ITALY
150 HENKEL GERMANY Pilot CONFIDENTIAL INFORMATION ENGLAND
2000 CHEVRON CHEMICAL FRANCE 5000(*)!FRACHEM S.A. FRANCE
3800 CONFIDENTIAL INFORMATION ITALY SAUDI ARABIA
2000 ARABIAN SULFONATES CY LTD.
2000 * SICCO SYRIA VIETNAM
1600 DUGGIANG CHEMICAL CO.
1300 N A N J I N G SURFACTANTS CHINA
1400 DAABOUL COMPANY SYRIA
5000 AEKYUNG & SHELL Co. KOREA
12000 CONFIDENTIAL INFORMATION EUROPE
1000(*)UNION QUIMICA MEXICO 1
2000 SOCIETE CHERIFIENNE MOROCCO
1000 HENKEL THAILAND
2000 MANRO BELGIUM
2000 CHINA NAT. MACHINERY CHINA
2000 SARUHAN TURKEY
Pilot CONFIDENTIAL INFORMATION ENGLAND
1600 WEIFANG SYNTH. DET. CHINA 2000 AL RIYAD JORDAN
5000(*)CONFIDENTIAL INFORMATION BRAZIL
3500(*)HOLS GERMANY
3000 FCFC R.O.C. 18000 CONFIDENTIAL INFORMATION U.S.A.
Pilot * CONFIDENTIAL INFORMATION ENGLAND
2000(*)HOECHST BRAZIL
5000 PT SAYAP MAS UTAMA INDONESIA
3800 BOMBRIL BRAZIL
3000 HENKEL CHIMICA ITALY
1500 STANDARD SURFACTANTS INDIA
Pilot * HENKEL GERMANY
2000 SANCHEZ Y MARTIN MEXICO
5000 COLGATE PALMOLIVE U.S.A.
6000OCONFIDENTIAL INFORMATION U.S.A.
2000 COLGATE PALMOLIVE MEXICO
1000 CONFIDENTIAL INFORMATION SYRIA
1600 CONFIDENTIAL INFORMATION VIETNAM
3000 HENKEL TURKEY
SOz/SOi production
Pilot CONFIDENTIAL INFORMATION U.S.A.
12000(*)CONFIDENTIAL INFORMATION MEXICO
5000 P.T. UNGGUL INDAH CO. CONFIDENTIAL
6000(*)CONFIDENT1AL INFORMATION U.S.A.
2000(*)HICKSON MANRO BELGIUM
6000 CONFIDENTIAL INFORMATION THAILAND
5000 HENKEL CHINA
Pilot CONFIDENTIAL INFORMATION U.S.A.
2000 CONFIDENTIAL INFORMATION PHILIPPINES
2000 ORBIT CHEMICAL IND. KENYA
5000 P.T. WINGS SURYA INDONESIA
5000 CONFIDENTIAL INFORMATION THAILAND
5000(*)CONFIDENTIAL INFORMATION PHILIPPINES
1000 AL INTAJ SULPHO CHEM.IND.CO.OMAN
1000 SOCIETE' CHERIFIENNE MOROCCO
3000 JINTUNG PETROCHEMICAL CHINA
5000 CONFIDENTIAL INFORMATION INDONESIA
1000 CONFIDENTIAL INFORMATION CROATIA
2000 GALAXY INDIA
6000(*)CONFIDENTIAL INFORMATION U.S.A.
1000 NATIONAL DETERGENT OMAN
3000 XIAN CHINA
1600(*)GECODA SYRIA
2000 SAN MIGUEL INDUSTRIAL PERU
1600 CHINA HUAYANG TECHNOLOGY CHINA
2000 CONFIDENTIAL INFORMATION SAUDI ARABIA Note:
300(*)CONFIDENTIAL INFORMATION U.S.A. * Plants skid mounted Partial supply
2000(*)BENCKISER CHINA
3000 CONFIDENTIAL INFORMATION (•)S0 3 Film Sulphonation plant supplied by Mazzoni de-
2000 (*) LUCKY KOREA tergent division, purchased by Ballestra in 1991, based
2000 COLGATE PALMOLIVE VENEZUELA on reactor M.
4500 CONFIDENTIAL INFORMATION
5000 LA CORONA MEXICO Ballestra is in a position to service these plants having
available all relevant khow how
 SULPHUREX M (•)
400 THIE-LONG CONG-TY TRACH NHIEM VIETNAM 1000 STE DE PROD. CHIM. DET. TUNISIA
500 DERIVADOS TENSIOACTIVOS SPAIN 2300 LEVER BROTHERS MALAYSIA
500(*)FABRICA DE JABON LA LUZ GUATEMALA 1600 CNTIC (BENX1) CHINA
300 FABR1CA DE JABON LA LUZ GUATEMALA 1600 CHINA LIGHT IND.CO.(GUANZHOU) CHINA
1000 FABRICA DE JABON LA LUZ GUATEMALA 1000 GUANGSHAO DEV.CO.(GHAOGUAN) CHINA
2000 MAN. OF CHEM. DETERGENTS SYRIA 1500 POLIMEX FOR ORGANIKA ROKITA POLAND
500 SUPERIOR SYNDETS INDIA 500 POLIMEX FOR POLLENA GDANSK POLAND
1000 INS-HER ARGENTINA 1600 GZTC (GUANXI) CHINA
1500 ALBRIGHT & WILSON "MARCHON" ENGLAND 1000 PULCRA SPAIN
2000 IBLA ITALY 1000 PULCRA SPAIN
4500 (*) MARCHON ITALIANA ITALY 150 PULCRA SPAIN
3000 (*) MARCHON ITALIANA ITALY 1700(*)HOECHST IBERICA SPAIN
2000 MARCHON ITALIANA ITALY 2000(*)B.P. DETERGENTS LIMITED ENGLAND
150 MARCHON ITALIANA ITALY 3500 PETROQU1M1CA ESPANOLA SPAIN
2000 BOMBRIL BRAZIL 150 PETROQUIM1CA ESPANOLA SPAIN
300 HYNS BABY PRODUCTS EGYPT 2000 SIDOBRE-SINNOVA FRANCE
500 JABONERIA NACIONAL ECUADOR 3500 GRUPO ULTRA BRAZIL
500 IREX COSTA RICA 150 GRUPO ULTRA BRAZIL
500 CONFIDENTIAL INFORMATION 2500 TATA VASHISTI DETERGENTS INDIA
150 "U.G.S." FRANCE 4000 ZSCHIMMER & SCHWARTZ ITALY
1500 THE EGYPTIAN SALT & SODA EGYPT 2000(*)ALBRIGHT & WILSON FRANCE
500 SOCIEDADE DE COMERCIO E
INDUSTRIA DE DETERGENTES PORTUGAL

OVER 130 FILM SULPHONATION PLANTS IN THE LAST 10 YEARS

Sulphurex F 3000, 50з production

Sulphurex F 4000 Sulphurex F 1500
швг

Sulphurex F 4000, SOs production and gas treatment

Sulphurex F 2000 Sulphurex F 5000, Neutrex

Sulphurex F 2000 Sulphurex F 3000 + 300

 PLANT PERFORMANCES
RAW MATERIALS CONSUMPTION
for 1000 Kg of Active Matter

CONSUMPTION (kg)
100% ACTIVE MATTER SOURCE Organic
Feedstock Sulphur NaOH 100%(*)

Linear DDB
mwZ45 718 98 130

Branched DDB
mwZ45 723 98 131

Natural or synthetic lauryl alcohol

mw207 684 110 139
Lauryl alcohol + 2EO
mwZ88 756 89 119

Lauryl alcohol +3 EO
mw339 787 79 106

Natural or synthetic alcohol C16-C18

mw258 741 95 128

AIpha-olefinsCl4-C18
mw237 700 103 137

MethylesterC16-C18
mw262 755 112 153

(*) Including SOz scrubbing

 PLANT PERFORMANCES

PRODUCTS CHARACTERISTICS

A.M. CONC. % FREE OIL S04 °KLETT

RAW MATERIALS
(*) (*) (•*)

Linear DDB:
- acid 97.5-98 0.8-1.2 0.8-1.2 10-25
- paste 30-75 0.8-1.2 0.8-1.2 15-20

Branched DDB:
- acid 97-97.5 1.0-1.5 1.0-1.2 50-100
- paste 30-60 1.0-1.5 1.0-1.2 50-100

Natural and synthetic lauryl alcohol

C12-C14orC1Z-C18 30-75 0.8-1.5 0.5-1.0 2-5

Natural or synthetic ethoxylated alcohol

with 2 or 3EO (***) 27-75 1.0-1.5 0.5-1.0 10-15

Natural and synthetic fatty alcohol

C16-C18 30-65 1.5-2.5 0.7-1.2 20-40

Alpha-olefins range: C14 to C18

single or blend 35-75 1.2-2.0 0.7-1.2 30-50

MethylesterC16-C18 30-65 2.0-2.5 1.2-1.8 40-70

(bleached)

(*) On 100% Active Matter

(**) 5% A.M. solution, 40 mm cell n. 42 filter, unbleached, unless otherwise specified
(***) 1.4 Dioxane (on 100% Active Matter) values are 20-30 ppm. Values below 10 ppm. are achievable with post treatment

BALLESTRA S.p.A.
VIA P. PORTALUPPI. 17 - 20138 MILANO - ITALY - TEL.: +39 2 50831
FAX:+39 2 58013221/5083327 - TX: 311519INGBA1 - E-Mail: [email protected]
SULPHITES OXIDATION

When the sulphite solution cannot be reprocessed The sulphite oxidation cycle is carried out in 7-8
or discharged as such to sewage or water hours.
treatment, a sulphites oxidation unit is necessary.
The oxidation yield checked by laboratory analysis
The oxidation of the sulphites to sulphates is is up to 90%; a Redox value of less than 50 ppm
performed in a packed column, operating sulphite can be achieved by a final adjustment
batchwise, by recycling the solution in the column with NaCIO or HzOz.
where ambient air is fed countercurrently.
The effluent from the sulphite oxidation unit is a
Despite the simple design all the process solution of NazSCUthat can be used as dilution
equipment constituting this unit is selected to water in the synthetic detergent powder
assure the best operating conditions and the production or can be disposed of.
easiest control on the critical parameters, like pH,
recycling rate and air throughput, which mainly In this latter case the impact on the sewage load is
affect the oxidation yield. very limited, being approximately 70 Kg/h the
quantity of NazSCb solution (at 10%
concentration in НЮ) generated by burning 100
Kg/h of Sulphur.
Sulphite Oxidation Column (in green colour)

Sulphite Oxidation Column

and Electrostatic Precipator
ALPHA OLEFINS HYDROLYSIS

During the sulphonation step, alpha olefins give a product from the neutralization section is fed to
mixture of various sulphonates h a v i n g linear, the hydrolysis unit at a pressure of approximately
branched and cyclic C-chain structure. The cyclic 10 kg/cm2 g.
sulphonates (sultones) need a particular chemical
and thermal treatment (hydrolysis) to be converted The fluid flows countercurrently with the already
in linear sulphonates. hydrolyzed product into a heat recovery exchanger
and its temperature rises up to 105-110°C.
More in p a r t i c u l a r , the reaction mass, after
neutralization, requires a thermic ageing treatment The product passes through a steam heater to
(approximately 30' at Т == 165-170°C) to convert i n c r e a s e its t e m p e r a t u r e to the h y d r o l y s i s
( the sultones into Active Matter. temperature (approximately 170°C) and finally it is
To this aim, an additional unit can be supplied for fed into the hydrolyzer, sized to allow an average
c o u p l i n g to the standard s u l p h o n a t i o n / residence time of 30 minutes.
neutralization plant (whose refrigerating group The hydrolyzed product passes through the heat
capacity in the air drying section must be increased recovery exchanger, where it transfers its heat to
for the production of chilled water for reactor the f l u i d to be hydrolyzed, d r o p p i n g its own
cooling). temperature to about 120°C, and then it is cooled
This unit is based on a hydrolysis column, heating down to 70-80°C by cold water in another
and cooling exchanger to be installed downstream exchanger.
the neutralization section.
The hydrolysis of the neutralized AOS paste is
performed as follows: the stream of a l k a l i n e

Alpha Olefins Hydrolysis Unit

Alpha Olefins Hydrolysis Unit, Skid Mounting
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HEAT RECOVERY

The hot air stream out coming the heat limits, while the still hot air exiting the battery
exchangers fitted in the SOz/SCh conversion tower can be sent to atmosphere or conveyed to the
is used for silica gel drying and could also be used silica gel regeneration section.
for the production of saturated steam.
The accurate design and construction features of
The heat recovery system is designed to recover
the heat exchanger allows to obtain
the sensible heat of the hot air stream from the
approximately 2 Kg of saturated steam (at P = 7
SOz/ЗОз coolers and it is based on the use of a
bar) for each Kg of sulphur burnt.
'tinned-coils battery where part of the hot air
stream from S02 coolers is indirectly contacted
This is usually more than sufficient to assure safe
with a proportioned amount of demineralized
and steady operation with no risk of steam-
water.
shortage to the process.
The steam so generated is sent to a separation Optional systems of heat recovery are available
drum where the entrained amount of water is for specific cases, such as the use of the hot air
separated; the steam is then sent to battery stream to feed (adiacent) spray dryers.

Heat Recovery Unit

SULPHUREX F
Heat recovery

SEPARATION DRUM

5\Saturated steam
>^ battery limits

Hot air
from So3 coolers

WATER
RECIRCULATING PUMP!

WATER
EED1NO PUMP

s
V ! Softened
NrJ
water

BALLESTRA S.p.A.
VIA P. PORTALUPPI, 17 - 20138 MILANO - ITALY - TEL.: +39 2 50831
FAX:+39 2 58013221/5083327 - TX: 3115191NGBAI - E-Mail: [email protected]
 50з ABSORPTION (IN HzS04 COLUMN)

Although the Ballestra film sulphonation plant

does not normally require this unit, the SOs
absorption unit can simplify the plant operation;
when the plant is frequently started up and shut
down and/or when very frequent product change-
over are foreseen.
In these cases the SCb-gas stream can be diverted
' to the HzS04 absorption column.

HzS04 at about 98% concentration recycles in the

absorption column. The acid concentration is kept
constant by the addition of the required amount
of reaction water.
The HzSCU concentration is monitored and 5оз Absorption Column
controlled by means of an in-line conductivity
analyzer.
The exhaust gases from the HzS04 absorber are
then sent to the standard exhaust gas treatment
unit.

I Construction materials of this unit include Teflon

lined and enamelled piping, special corrosion
resistant steel for pumps and heat exchangers and
ceramic lining and filling for the column.

Alternatively, the SOs gas can be absorbed during

plant star-up, shut-down or emergency
situations, by reaction with L.A.B. under
controlled flow and temperature conditions.
This operation is carried out in a static reactor
provided with SCb distribution device, exhaust-
gas collecting duct, external recirculation loop for
temperature control and load cell system for
accurate control of the alkylate dosing.
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SULPHUR MELTING AND
PRE-TREATMENT

When the solid sulphur quality is very poor, to transfer the treated sulphur to filtration and to
improve it, the addition of a separate melting and the standard sulphur melter.
filtering day tank is foreseen.
After intimate mixing, the molten sulphur and the
Addition of chemicals and/or filtering earths may earths are recycled through the filter (to form a
be required for the sulphur purification. pre-coat on the filtering surface) and then the
I mass is passed through the filter and transferred
The solid sulphur to be purified is loaded to the to the standard melter from where the purified
melter and addition of chemicals and earths is sulphur is dosed to the process.
subsequently done.

The additional melter, usually an underground

vessel to facilitate the loading of solid
pretreatment agents, is therefore provided with a
mixer - agitator and a submersed pump to

Sulphur Pre-Treatment Unit

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SLES PASTE DEAERATION

When Sodium Lauryl Ether Sulphate (SLES) is

produced at high concentration, the paste may
contain a small quantity of air.
A continuous SLES paste deaeration unit can be
supplied to remove the air under reduced
pressure in a special equipment installed down
.stream the neutralization unit, so ensuring the
production of a completely translucent paste.
The deaeration unit is supplied as a complete
package including vacuum pumps and product
transfer pump.
Moreover the high efficiency of the unit allows to
modify significatively the specific weigh of the
infeed paste (i.e.: from 0.7 up to 1.0 kg/dm3)
with parallel decrease of its apparent viscosity,
that results in easier handling and reusing.

SULPHUREX F
Sles paste deaeration
Sles Paste Deaeration Unit
Active matter
from Neutrex

Active
matter

BALLESTRA S.p.A.
EXTRACTION PUMP
VIA P. PORTALUPPI. 17 - 20138 MILANO - ITALY - TEL.: +39 2 50831
FAX:+39 2 58013221/5083327 - TX: 311519INGBAI - E-Mail: [email protected]
 SLES PASTE DEGASSING/STRIPPING

The refining of Ethoxysulphated Alcohols is often chemical characteristics of the SLES product, thus
required to meet the most stringent quality resulting in a consistent improvement of the
specification and in particular for the content of product quality.
1.4-Dioxane.

The system illustrated allows the refining of

concentrated paste of Ethoxysulphated Alcohols Wiped Film Evaporator
I as well as its degassing, to assure the highest level
of physical and chemical specifications to the end
product.

The system is based on a wiped film evaporator

operating as a stripper of the HzO/Dioxane
mixture.

Being the physical and chemical characteristics of

Dioxane such as to allow its removal from water
solution relatively easy at reduced pressure.

The SLES product coming directly from the

storage tank or from the neutralization unit, is
Ifed to the wiped film evaporator which operates
under vacuum.

Low pressure steam is used as heating fluid in

the jacket of the machine.

The HzO/Dioxane vapours are conveyed to the

condenser while the stripped SLES is sucked by an
extraction pump and sent to the adjustment of
Active Matter content or directly to the storage
and buffering tank.

Starting from SLES containing max 50 ppm of

1.4-Dioxane (on 100% A.M.), a yield of removal
of 80% can be achieved by water evaporation
markedly dependent on the applied vacuum
degree.

The evaporation pathway performed by the

Dryex system allows the reduction of 1.4-
Dioxane without any deterioration of the other
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 VACUUM NEUTRALIZATION

The scope of the unit is the neutralization of the acids The amount of caustic soda is controlled by a pH-
coming from the sulphonation/sulphation of alkylates, meter, installed on the out coming product, which
alcohols, ethoxylated alcohols, etc. to obtain operates on the set point of the flow rate controller.
neutralized products at high Active Matter (A.M.) The equipment is maintained under vacuum by a
concentration. vacuum pump and a condenser, while the control
The advantage of this system, compared to the of the vacuum level is self-adjusting.
traditional ones ("loop type") is in the low The neutralized product is extracted from the
residence time and hold-up of product which bottom of the reactor by a volumetric pump and
permits an accurate pH control and a high transferred to the battery limits.
( flexibility during the start-up, shut-down and
production. More than 80% of Dioxane can be The neutralization reaction is exothermic and the
removed in this way. heat is removed by the evaporation of part of the
mixing water.
The system consists of a wiped film type neutralizer,
on the top of which the reagents are fed at controlled The product temperature is controlled with the
rates. Acid, water and caustic soda are mixed by the vacuum level in the neutralizer and by the external
special rotor blades in the top of the reactor. coolingjacket.
The automatic control of the different process
Wiped Film Neutralizer - Bottom view parameters, i.e. flow rate of reagents, vacuum
degree, temperature of thermostatic water, allows
to accurate control and mantain of the product
concentration.

Wiped Film Neutralizer - Top view

 ACTIVE MATTER DRYING - "DRYEX"

The drying of Anionic Surfactants is aimed to from the neutralization unit is pre-heated up to a
increase the concentration of Active Matter and to temperature of 80-85°C and fed to the top of the
make easier their handling and incorporation into downstream wiped film evaporator, designed for
formulated detergents. operation at atmospheric pressure or controlled
vacuum.
The drying system shown in the scheme is based The evaporator is equipped with multi-step
on a specially designed wiped film evaporator heating jacket and connected with a condenser; a
I characterized by: controlled vacuum is provided by a blower, mainly
to convey the vapour to the condenser;
- high process flexibility and mechanical reliability
downstream the evaporator the dried product
- m i n i m u m and narrowly distributed residence ( u s u a l l y in form of l u m p s ) is cooled and
time of the product in the evaporator mechanically treated, before reaching the storage
- close correlation between operating parameter silos or the feeding hopper of the product to the
and product specs agglomeration process.
- optmized energy consumption The multi-step jacketing and the accurate control
of the steam pressure allow to establish and to
- negligible emissions
maintain the best temperature profile along the
- fast start-up/shut-down operations evaporator walls; these parameters can be
The system operates as follows: The paste-like selected and varied according to the nature and
surfactants, coming from storage tank or directly characteristics of the infed product, thus resulting

DRYING J
SOLID/LIQUID
ADDITIVES 1 (CONDITIONING

DRY BRY
SURFACTANT SURFACTANT
POWDER NEEDLES
SULPHUREX F
Active matter drying unit "Dryex'

WIPED
FILM EVAPORATOR

Steam

Active matter
paste

EJECTOR

Conditioned Sr
air

BALLESTRA S.p.A.
VIA P. PORTALUPPI. 17 - 20138 MILANO - ITALY - TEL.: +39 02 S0831
FAX:+39 02 58013221/5083327 - TX: 311519INGBA1 - E-Mail: [email protected]
in the possibility to dry the whole range of anionic
surfactant in paste form as well as slurries and
т
solutions of specialties and thermosensitive
organic products.
The water evaporation takes place downwards
the evaporator in a substantial laminar flow.
Being the whole phenomena driven by the heat
transfer rate, in order to preserve the quality of
the end product, it is crucial to avoid any build-up

t>
Atmosphere

PNEUMATIC
TRANSPORT FAN

PNEUMATIC TRANSPORT
FILTER

i Dry active matter Scraped Film Evaporator

of product on the wall of the evaporator; this
action is assured by the internal mechanical
features of the evaporator, consisting of a
rotating shaft holding a series of movable blades Scraped Film Evaporator, Inner Rotating Parts
supported by appropriate frames.
These rotating blades provide for product
distribution over a wide surface of the
evaporator, as well as for removal -of the dry
product from the wall of the same.
The mechanical energy input provided by the
rotating blades provokes an additional shearing The described system can be sized to afford an
effect that results in a decrease of the apparent evaporation capacity ranging from 20 up to 500
viscosity of the processed fluid, with consequent Kg/h of water (starting from 65-70% A.M.
improvement of the heat and mass transfer. surfactant paste) roughly corresponding to 100-
2000 Kg of 70% A.M. surfactant paste processed.
These factors are particularly beneficial for the
drying of heat sensitive material characterized by The base plant configuration for the surfactant
high viscosity in the range of active matter typical drying unit is indicated in the attached drawings:
of concentrated pastes. the product is obtained by this process in form of
flakes (with moisture content from 1 to 10%
Operation at substantially atmospheric pressure depending on product) that are also the starting
allows to reach the maximum possible drying material for the production of dry powder, needles
degree at the minimum possible temperature, and granules, by means of specific and dedicated
before solidifying the product in the dryer itself process equipment owing an easy coupling with the
base drying plant and operating in accordance to
A further effect given by the system is the
the indicated block diagram.
narrowing of the residence time distribution
of the product in the evaporator thus reducing The advantages of the modification of the
the possibility of local or spot overheating of physical form of the dry surfactant consist in the
the product and consequent bad effect on final improvement or specific application properties
product quality. such as solubility, flowability, bulk density and
Active Matter Drying Unit, Skid mounted easiness in handling, storage and re-using.

The integration of the DRYEX units with the

Ballestra S03 Film Sulphonation Plants allows the
production of a wide range of dry а т о т с
surfactants with the physical and chemical
characteristics capable to meet all market
demands.

Wiped Film Neutralizer - Bottom view