Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial

Estate, Sedarapet, Puducherry

BRIEF SUMMARY

1.0 BRIEF SUMMARY

This chapter presents the type, need, location & size of the project, major resources
required for proposed project, project schedule, technological consideration, process
/ technical description and likely environmental effects due to the proposed project
and mitigation measures to be adopted.

1.1 Type of Project

The proposed project of Power Soaps Private Limited is sulphonation of Linear Alkyl
Benzene (LAB) to produce 72 TPD (18,000 TPA) of 96% Linear Alkyl Benzene
Sulphonic Acid (LABSA). The major plant facilities proposed for the project are SO3
Gas Plant, SO3 Absorber System, Sulphonation System and Effluent Gas Treatment
System.

1.2 Need for the Project

The use of Linear Alkyl Benzene Sulphonic Acid (LABSA) in the detergent
manufacturing units have substantial demand in the country and has Export
potential also. The demand for the detergents cakes and powders are increasing due
to the increasing population and their literacy rate. As the project proponents
operating 5 nos. of detergent manufacturing units, they need adequate quantity of
LABSA.

To fulfil the increasing demand for LABSA in their detergent plants and to earn
valuable foreign exchange, Power Soaps Private Limited proposes to install a new
production facility and increase its overall production capacity.

1.3 Project Location & Layout

The project site is located in Plot nos. B – 41, 42, 43, 44, 45, 46, 47, 59, 60, 61, 62,
63, 64 & 65, PIPDIC’s Industrial Estate, Sedarapet, Villianur Commune Panchayat,
Pondicherry district, Puducherry.

1.4 Size or Magnitude of Operation

The proposed production capacity of the plant will be 72 TPD (18,000 TPA). The
estimated cost of the proposed project is about INR. 575 Lakhs. The details of the
resource requirements like land, raw materials, power, water and manpower for the
proposed project is described in this section.

1.4.1 Land Requirement

The total land allotted for this plant at PIPDIC, Sedarapet is 0.9072 ha (2.24 acres).
The land is already an industrially specified area and thus there will not be much
change in the present land use at the plant site. The land use break-up is given in
Table-1.1.

Vimta Labs Limited, Hyderabad/Coimbatore C2-1

 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

TABLE-1.1
LAND USE BREAK-UP

Sr. No. Plant Facilities Area (ha) Percentage (%)

1. Production facilities 0.116 12.79
2. Storage Building & Tank farm 0.139 15.33
3. Greenbelt development 0.240 26.46
4. Open area 0.412 45.42
Total 0.907 100.0

1.4.2 Raw Material Requirement

The major raw materials required for the proposed sulphonation plant are Linear
Alkyl Benzene and Sulphur. The annual requirement of various raw materials and
their sources is given in Table-1.2.

TABLE - 1.2
RAW MATERIALS REQUIREMENT DETAILS
Sr.
Material Quantity Source Transportation Storage
No.
Raw Material
1. Organic Alkylate 55.44 TPD Indigenous By Road C. Steel Tank
2. Sulphur 8.28 TPD Indigenous By Road Closed shed
Other Chemicals
3. Caustic Soda Lye 50 TPA Indigenous By Road S. Steel Tank
4. Vanadium 600 Lit/A Indigenous By Road Closed shed
pentoxide

1.4.3 Power Requirement and Supply

The total power required for the proposed plant is about 900 KW, which will be met
from the Puducherry state grid. To meet the emergency power requirement during
the grid failure, diesel generator set having capacity of 1000 KVA each are
proposed. The fuel required in the plant is only High Speed Diesel (HSD), which is
used as fuel in generators. The requirement of HSD is about 350 lit/hr.

1.4.4 Water Requirement

Water requirement in the plant is for cooling tower make-up, scrubber make-up, DM
plant, floor wash and domestic usages. The water requirement of the proposed plant
will be sourced from PIPDIC. The water requirement details are presented in Table-
1.3.
TABLE - 1.3
WATER REQUIREMENT
Sr. No. Category Quantity (KLD)
1. Cooling tower make-up 32.0
2. Scrubber make-up 8.0
3. DM Plant 7.0
4. Domestic Requirement 1.5
Total 48.5

Vimta Labs Limited, Hyderabad/Coimbatore C2-2

 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

1.4.5 Manpower Requirement

The manpower required for the proposed plant will be 30 nos., which includes
manager, admin staffs, supervisor and workers.

1.5 Technology Adopted

The customary method of production starts with the appropriate alkyl benzene
which is sulphonated and then subsequently neutralised. The sulphonation
reaction can be carried out in various ways. In the past, the reaction has been
carried out using concentrated sulphuric acid or oleum, in either case using an
excess of acid. At the end of the sulphonation the surplus acid and the desired
product must be separated. Alternatively the entire mixture can be neutralised
leading to a product containing a substantial proportion of an inorganic sulphate
salt, e.g. sodium sulphate.

Subsequently, it has become conventional to use sulphur trioxide as sulphonating

agent. US patent 2928867 published in 1960 teaches that at the end of a
sulphonation process carried out with sulphur trioxide, a small amount of water
should be added to the reaction mixture to hydrolyse sulphonic acid anhydrides
present in the reaction mixture so that a stable product is obtained after
neutralization.

During more recent years it has become standard practice to use gaseous sulphur
trioxide as sulphonating agent in an approximately stoichiometric quantity, then
age the resulting mixture during which time the reaction mixture proceeds further
towards completion, and next add a small quantity of water which is believed to
hydrolyse any anhydrides present in the reaction mixture thereby stabilizing
reaction. This current practice is described in, for example, "Sulphonation
Technology in the Detergent Industry" by W Herman de Groot 1991. When
carrying out this conventional practice the sulphur trioxide is normally diluted
with some other gas which does not react. Air can be used. It is possible to carry
out the reaction using an excess of sulphur trioxide but this leads to
disadvantages. One disadvantage is the formation of coloured impurities. If a
substantial excess of sulphur trioxide is used, the mixture obtained contains
unwanted sulphuric acid which must be removed or tolerated as an impurity just
as with the older processes using sulphuric acid or oleum. This is less of a
problem if there is only a small excess of sulphur trioxide but, as will be explained
below, this leads to the presence of undesirable impurities.

When sulphonation is carried out using an approximately stoichiometric quantity

of sulphur trioxide it is found that the conventional ageing period at the end of
the sulphonation reaction gives increased conversion of the alkyl benzene into the
desired sulphonic acid. Nevertheless, it is observed that the alkyl benzene
feedstock is not completely converted into the desired alkyl benzene sulphonic
acid. A small percentage of alkyl benzene remains unchanged and a small
quantity is converted into a sulphone of the formula.

The relative proportions of unconverted alkyl benzene and sulphone impurity

vary. They are affected by the reaction conditions employed and by the mole ratio
of sulphur trioxide to alkyl benzene. Although it is possible to vary the relative
proportions of unreacted alkyl benzene and sulphone it is not possible to avoid
Vimta Labs Limited, Hyderabad/Coimbatore C2-3
 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

both of them simultaneously by control of reaction conditions or mole ratio of

reactants. Thus, if the mole ratio of sulphur trioxide to alkyl benzene is increased
so as to minimise the percentage of unconverted alkyl benzene, the percentage of
sulphone increases.

Failure to convert alkyl benzene to sulphonic acid and conversion to by-product

sulphone both represent a waste of alkyl benzene feedstock. Additionally,
unconverted alkyl benzene can give rise to tower emission problems on spray
drying and there have also been suggestions that residual alkyl benzene is
slightly toxic.

Thus, although the present commercial procedure of sulphonation with

stoichiometric quantity of sulphur trioxide followed by ageing and then the
addition of water to arrest the reaction is very advantageous compared with
earlier processes in that it gives a high level of conversion to the desired product
without introducing large quantities of sulphuric acid into the product mixture,
there is still some scope for further improvement in that it would be desirable to
reduce further the combined levels of alkyl benzene and sulphone below what is
currently achievable.

According to the present invention there is a method of manufacturing alkyl

benzene sulphonate by contacting, as reactants, alkyl benzene with sulphur
trioxide using a molar ratio of alkyl benzene to sulphur trioxide in a range from
1:0.9 to 1:1.3, characterised by incorporating sulphuric acid into the reaction
mixture after bringing the reactants into contact, the amount of sulphuric acid
being not more than 10% by weight of the reaction mixture, and then allowing
reaction in the mixture to continue for at least 30 minutes.

We have found that by incorporating sulphuric acid in this manner it is possible to

achieve an improvement in the overall conversion to the desired product and a
consequent reduction in the undesired impurities. For carrying out this reaction,
the sulphur trioxide is preferably diluted with another gas, as is conventional. This
other gas may well be air. The ratio of sulphur trioxide to other gas may desirably
lie in a range from 3% to 10% by volume. The molar ratio of alkyl benzene to
sulphur trioxide is preferably in a range from 1:0.9 to 1:1 better 1:0.95 to 1:1.
The alkyl benzene which is sulphonated may have a straight or branched alkyl
group which preferably contains from 10 to 15 carbon atoms. Although branched
alkyl benzene has been extensively used for detergent manufacture it is
nowadays usually preferred to employ linear alkyl benzene, that is to say alkyl
benzene in which the alkyl group has a straight carbon chain.

It is known to carry out the sulphonation of alkyl benzene which is provided as a

mixed feedstock also containing some other material which undergoes
sulphonation. Conceivably this invention could be employed when it is a mixed
feedstock which undergoes reaction. However the invention is particularly
significant when the alkyl benzene feedstock is not mixed with a substantial
quantity of any other material so that the feedstock contains in excess of 90% by
weight alkyl benzene.

The sulphuric acid which is added may be in the form of conventional

concentrated sulphuric acid containing 98% of sulphuric acid itself. It would also
Vimta Labs Limited, Hyderabad/Coimbatore C2-4
 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

be possible, although it is not preferred, to employ sulphuric acid which is not

quite so concentrated. Alternatively it would be possible to employ fuming
sulphuric acid containing some oleum.

The amount of sulphuric acid which is employed is preferably at least 1% and

more preferably at least 1.5% by weight of the reaction mixture. The amount is
preferably not more than 5% of the weight of the reaction mixture and quite
possibly not more than 4% by weight of the reaction mixture.

Ageing of the reaction mixture after addition of the sulphuric acid preferably takes
place with some agitation of the reaction mixture and at a temperature somewhat
above normal room temperature, e.g. in the range from 30 to 70°C. The ageing
period will generally not exceed 12 hours although longer periods may be
employed if desired. An ageing period in the range from 2 to 8 hours is preferred.
At the end of this ageing period some water may be added to the reaction
mixture to hydrolyse any remaining sulphur trioxide and stabilise the reaction
mixture, in accordance with conventional practice for sulphonation.

The invention will be further explained and illustrated by the following example in
which all amounts and proportions are by weight unless otherwise stated. Alkyl
benzene having a molecular weight of approximately 218 corresponding to a
formula in which the average value of x is 10 was sulphonated in a commercial
sulphonation plant with a multi-tube falling film reactor. Sulphonation was
affected using sulphur trioxide and air in an approximate ratio of 1.00.

Quantities of reaction mixture leaving the falling film reactor were taken, mixed
with varying amounts of 98% sulphuric acid, and then aged at 50°C for up to 4
hours. Samples were taken out of the mixtures after various intervals of time and
neutralised to the sodium salt of the acid under conditions calculated to give
approximately 25% sodium alkyl benzene sulphonate in the neutralised mixture.
These neutralised mixtures were analysed to determine the actual content of
sulphonic acid and also to determine the content of Non-Detergent Organic Matter
(NDOM). This NDOM consists principally of unreacted Linear Alkyl benzene (LAB)
and of sulphone by-product. The amounts of these materials were determined
from the infra-red spectrum of the NDOM.

1.6. Process Description

1.6.1 Sulfonation

The term “sulfonation” will indicate both the sulfonation and sulfation reactions,
such a term meaning any reaction arising from the addition of SO 3 with an
organic material regardless of the functional group characterizing the end
product.
The sulfonation reaction takes place simple by contact between the organic
substance to be sulfonated and sulphur trioxide. The latter being a highly active
reagent cannot be used in the concentrated form otherwise it would destroy the
organic matter; consequently it is used at an approximate concentration of 4% by
volume in dry air.
Since reaction is highly exothermic the product has to be cooled as the reaction
proceeds to avoid deterioration of the product which is heat-sensitive.
Vimta Labs Limited, Hyderabad/Coimbatore C2-5
 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

The main reactions occurring in the proposed plant are following:

R-H + SO3 R-SO3H --- (1)

Organic Sulfonic acid

R-H + 2SO3 R-SO2OSO3H --- (2)

Disulfonic acid

2R-H + 2SO3 (RSO2)2O=H2O --- (3)

Undesired reactions (2) and (3) take place only when the resulting by-products
are almost entirely eliminated in the subsequent aging and hydrolysation steps.

Vimta Labs Limited, Hyderabad/Coimbatore C2-6

 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

SULPHUR

STEAM
MELTING

BURNING TO PRODUCE SO2

(780oC)

Air/Water COOLING WHB/TEMP-430oC

CATALYST V2O5

4 STAGE CONVERTER / SO 2 TO SO3

FALLING FILM REACTOR

SULPHONATION OF LAB
TO LABSA

DIGESTER

HYDROLYSER

STORAGE VESSEL

DISPATCH

FIGURE – 1.1
PROCESS FLOW CHART

Vimta Labs Limited, Hyderabad/Coimbatore C2-7

 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

1.8.2 Aging

This operation eliminates partly the products of reaction (2) increasing at the
same time the yield of useful products as the excess SO3 reacts with the
unsulfonated organic matter.

RSO2OSO3H + RH 2RSO3H --- (4)

Acid
1.8.3 Hydrolysation

This operation eliminates the excess SO3 both dissolved and contained in the
products of reactions (2) and (3) which would lead later to the acid degradation

(RSO2)2O + H2O 2RSO3H --- (5)

Acid

RSO2OSO3H + H2O RSO3H + H2SO4 --- (6)

Acid

1.9 Environmental Effects and Mitigation measures

The proposed project would comprise various production facilities such as SO3 gas
plant, SO3 absorber system, Sulphonation system and Effluent gas treatment
system. These would therefore lead to release of emissions to the air, generation
of wastewater and solid wastes. The sources and nature of pollution from the
proposed plant and the types of environmental pollution likely to occur are
presented in Table-1.4.

TABLE – 1.4
AIR POLLUTION – SOURCES & MANAGEMENT

Facility/Department Pollutants Type of Pollution

Sulfonation/SO3 scrubber SO2, SO3 & Acid mist Air pollution
Cooling Tower / Boiler / Effluent Water pollution
Alkali scrubber/ DM plant
Sulfonation/ETP Spent catalyst / Sulphur Solid pollution
Residue / Sludge

1.10.1 Air Pollution Control Measures

The principal air pollution control systems proposed for the sulphonation plant
would be Candle filter, Electrostatic Precipitator and Alkali Scrubber.

The SO2 and Acid mist coming from the sulfonation process would be cleaned by
taking the gas through an ESP to remove the acid mist followed by alkali scrubber
to remove the SO2 gas. The clean gas will be discharged into atmosphere through
as stack of 35.0-m height.

Vimta Labs Limited, Hyderabad/Coimbatore C2-8

 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

1.10.2 Water Pollution Control Measures

The main source of effluent in the proposed sulfonation plant is cooling tower
blow down, boiler blow down, alkali scrubber bleed-off, DM plant reject and
domestic usages.

TABLE – 1.5
WATER POLLUTION – SOURCES & TREATMENT

Sr. No Description Quantity in KLD Treatment

1 Sewage 1.25 Septic tank with dispersion trench
2 Trade Effluent 4.6 Effluent Treatment Plant

1.10.3 Solid Waste Management

Major solid wastes generated from the proposed sulfonation plant would include
TABLE – 1.6
SOLID WASTES – SOURCES & MANAGEMENT
Sr.
Solid waste Categ. Quantity Treatment or Disposal
No
1 Sulphur sludge 34.3 0.003 TPA Stored temporarily in HDPE bags and
sent to secured landfill facility,
Gummidipoondi
2 Spent catalyst 35.2 0.3 TPA Stored temporarily in polyethylene
bags and send back to manufacturers
for rebinding the same
3 Sulphur ash 36.2 0.7 TPA Stored temporarily in HDPE bags and
sent to secured landfill facility,
Gummidipoondi
4 Scrubber residue 36.1 4.5 TPA Concentrated and used in detergent
industry

1.10.4 Noise Pollution Control Measures

The major sources of noise generation from the proposed plant are fixed plant
installations and external transport movements. The noise generating
machineries are blowers, centrifugal pumps, compressors and stand by DG set
which will be maintained within the standard limits of 90-dB(A).

Various measures proposed to reduce the noise pollution include reduction of

noise at source, provision of acoustic enclosure like for the equipment like DG set
and suction side silencers, selection of low noise equipment like closed type
Compressor, isolation of noisy equipment from working personnel. Personnel
working in noise generation areas will be provided with ear muffler.

All rotary equipment like fans, blowers, pumps & compressors would be of low
noise design. The grouting of this equipment will be made free from vibrations.
The work zone noise exposure of the operating personnel would be avoided by
remote operation from the control rooms. The adequate noise control measures
will be adopted and work zone noise levels will be controlled to less than 85-
dB(A).

Vimta Labs Limited, Hyderabad/Coimbatore C2-9

 Application for the proposed LABSA Manufacturing plant at PIPDIC’s Industrial
Estate, Sedarapet, Puducherry

BRIEF SUMMARY

1.11 Cost Provision for Environmental Measures

The capital cost of the project is about Rs. 10.0 Crores. It is proposed to invest
about Rs. 2.5-Crores, i.e. 33.3 % of the capital cost on pollution control,
treatment, green belt development, rainwater harvesting, environmental
monitoring systems and others. The break-up of the investment is given in Table
– 1.7.
TABLE – 1.7
COST PROVISION FOR ENVIRONMENTAL MEASURES

Sr. Description of Item Capital Cost Recurring Cost

No. (Rs. in Lakhs) (Rs. in Lakhs)
1 Air pollution control systems 200.0 25.0
2 Water pollution control system 25.0 5.0
3 Environmental Monitoring 5.0 4.0
4 Greenbelt development, rainwater 20.0 6.0
harvesting and others
Total 250.0 40.0

Vimta Labs Limited, Hyderabad/Coimbatore C2-10