Associated Dyestuff Pvt. Ltd. (Unit-IV) 1
Annexure-I
List of Products
Sr.
No.
Product Capacity
(MT/month)
1 K Acid 100
2 Gamma Acid 50
3 Dyes Intermediates like 500
H Acid
FC Acid
MUA
Sulfo Tobias Acid
Sulfo J Acid
4 VS and Its derivatives 1000
Vinyl Sulphone (PBVS)
OAVS
PCVS
DMAVS
Sulpho VS
Sulpho OAVS
MPDSA
DASA
5 PCVS 50
6 DMAVS 25
Total 1725
Associated Dyestuff Pvt. Ltd. (Unit-IV) 2
List of Raw Materials
Sr.
No.
Name of Raw Materials Mt/Mt
K Acid
1 β Napthol 1.330
2 24% Ammonia 6.830
3 Oleum (65%) 5.675
4 Sodium Bicarbonate 0.920
5 Sodium sulphate-98% 4.500
6 Sulphuric acid (98%) 3.435
Gamma Acid
1 Beta Naphthol 1.665
2 Caustic flakes 1.670
3 Liq. Ammonia (25%) 0.500
4 Oleum (23%) 3.000
5 Sodium bisulphite 0.350
6 Sulphuric acid (98%) 5.585
H acid
1 Acetic acid 0.050
2 Caustic Flakes 1.800
3 CI Powder 0.940
4 Glauber Salt 3.500
5 LSP 5.000
6 Methanol 0.575
7 Naphthalene 1.010
8 Nitric Acid 0.980
9 Oleum 2.860
10 Soda Ash 0.410
11 Spent acid 8.930
12 Sulphuric acid 3.030
FC acid
1 PNCBOSA 1.385
2 PPD 0.620
3 Soda Ash 0.930
4 C.I. Powder 1.140
5 HCl 2.900
MUA
1 MPD 0.800
2 HCl (30%) 2.000
Associated Dyestuff Pvt. Ltd. (Unit-IV) 3
Sr.
No.
Name of Raw Materials Mt/Mt
3 NaOCN 0.580
Sulfo Tobias Acid
1 Tobias Acid 0.835
2 Oleum Acid (65%) 2.045
3 Sulphuric Acid 0.345
4 KCl 0.420
Sulfo J Acid
1 J-Acid 1.500
2 Oleum (65%) 6.450
3 Sulphuric Acid 1.075
4 Salt 4.250
Vinyl Sulphone(PBVS)
1 Acetanilide 0.555
2 Caustic Lye 0.665
3 Chloro Sulphonic acid 1.475
4 Ethylene Oxide 0.285
5 NaOH 0.055
6 SBS 0.125
7 SBS Slurry 0.345
8 Spent acid 0.775
9 Thionyl Chloride 0.480
OAVS
1 Acetyl Ortho Ansidine 0.715
2 Caustic lye 1.191
3 Chloro sulphonic acid 3.033
4 Ethylene Oxide 0.585
5 Sodium bisulphite 0.650
6 Sulphuric acid 1.386
Sulpho VS
1 p-base vinyl Sulphone 0.875
2 Oleum (65%) 0.850
3 Sulphuric Acid 1.100
4 Salt 0.500
Sulpho OAVS-15 MT/month
1 OAVS 0.876
2 Oleum Acid (65%) 0.850
3 Sulphuric Acid 1.100
4 KCl 0.500
Associated Dyestuff Pvt. Ltd. (Unit-IV) 4
Sr.
No.
Name of Raw Materials Mt/Mt
MPDSA
1 2 4 DCNB 1.725
2 CI Powder 1.900
3 HCl (30%) 0.140
4 MgO 0.380
5 NaCl 3.400
6 Soda ash 0.150
7 Sodium Trisulphite 1.135
DASA
1 Acetanilide 1.330
2 Caustic Flakes 0.830
3 Chloro Sulphonic Acid 3.200
4 HCl (35%) 1.330
5 PPD 0.935
6 Soda Ash 0.335
PCVS
1 Acetanilide 0.555
2 Caustic Lye 0.665
3 Chloro Sulphonic acid 1.475
4 Ethylene Oxide 0.285
5 NaOH 0.055
6 SBS 0.125
7 SBS Slurry 0.345
8 Spent acid 0.775
9 Sulphuric acid 0.345
10 Thionyl Chloride 0.480
DMAVS
1 2:5 DMA 0.700
2 Acetic Anhydride 0.840
3 Caustic Lye 1.150
4 Chloro sulphonic acid 4.500
5 Dil Sulphuric acid 0.600
6 Ethyleane Oxide 0.400
7 SBS 0.550
8 Sulphuric acid 0.357
Associated Dyestuff Pvt. Ltd. (Unit-IV) 5
Annexure -II
Manufacturing Process
1. K Acid
Manufacturing Process:
B-Naphthol is sulphonated by 98% Sulphuric acid and 65% Oleum. Then sulpho
mass dump in ice & water. Then salted out with Sodium Sulphate. Then filter it
and get cake then amidation by 24% Ammonia & Sodium bisulphite. Then isolate
the material with 98% Sulfuric acid. Filter it and centrifuge it & the final product is
known as K-acid.
Chemical Reaction:
Mass Balance:
Input KG Output KG
β Napthol 1330 SO2 555
Sulphuric acid (98%) 2270
Oleum(65%) 5675
Ice 21670
Water 1000
Sodium sulphate-98% 4500
Wash water 2500 Spent acid-reuse/sale 32990
Spent acid-reuse/sale 2750
24% Ammonia 6830 NH3 445
Sodium Bicarbonate 920
Sulphuric acid (98%) 1165 SO2 1650
Wash water 840 ML to MEE 7685
ML to MEE 950
Drying loss 675
K-ACID 1000
Total 48700 48700
Centrifuge
Final product
Mass balance of K-ACID
Isolation
Filtration & nutch
Drownings
Isolation
Filtration
Sulphonation
Nutch
Centrifuge
Amidation
Associated Dyestuff Pvt. Ltd. (Unit-IV) 6
2. Gamma Acid
Manufacturing Process:
β-Naphthol is sulphonated by 98% Sulphuric Acid and 23% Oleum. Then
sulfomass dump in Ice & Water then salted out with Potassium Chloride.
Then take fusion with Caustic and isolate with dilute Sulphuric Acid. Final
product is known as Gamma Acid.
Chemical Reaction:
Mass Balance:
Input KG Output KG
Beta Naphthol 1665 SO2 620
Sulphuric acid(98%) 2000
Oleum(23%) 3000
Ice 25000
Wash water 835 ML to MEE 27115
ML to MEE 2850
Liq. Ammonia(25%) 500
Sodium bisulphite 350
Caustic flakes 1670
Sulphuric acid(98%) 3585 SO2 1085
Water 10000
Wash water 835 ML to MEE 14500
ML to MEE 1600
Drying loss 670
Gamma acid 1000
Total 49440 49440
Isolation
Filtration
Centrifuge
Final product
Autoclave II
Centrifuge
Autoclave I
Mass balance of Gamma Acid
Sulphonation
Drawing
Filtration
Associated Dyestuff Pvt. Ltd. (Unit-IV) 7
3. H Acid
Manufacturing Process:
Sulphonation: Naphthalene is charged in the Cast Iron sulphonator and
Sulphuric acid with Oleum is charged at low temperature to have reaction
with monohydrate. The reaction mass is then heated to 1700C and 65%
Oleum is charged. The temperature is maintained for about 3 hours. On
completion of the reaction it is taken for nitration.
Nitration: Nitration is carried out in CI vessels. The sulphonated mass is
reacted with Nitric acid at controlled temperature. The mass is taken to
neutralizer.
Neutralization: This reaction is carried out in a MSRL brick lined vessel.
The excess acid is reacted with limestone to get gypsum.
Filtration: The gypsum is then precipitated out and separated in horizontal
vacuum filter and is thoroughly washed with water.
Reduction: The nitro mass thus obtained is reduced to amino compound
by iron powder and HCl in hot condition. After completion of the reduction
the mass is filtered to remove iron oxide sludge.
Concentration: The amino solution is concentrated in the multiple effect
evaporators to a desired level for hydrolysis.
Autoclaving: The concentrated mass is hydrolyzed under pressure of 6-7
kg/cm2 with caustic soda at a temperature of 1700C.
Isolation: The hydrolyzed product obtained from the autoclave is reacted
with Sulphuric acid or HCl for an acidic pH of about 2. H acid is there by
precipitated and filtered through vacuum filters and washed to obtain wet
cake of H-acid. The wet cake is finally dried to get the product.
Associated Dyestuff Pvt. Ltd. (Unit-IV) 9
Mass Balance:
INPUT KG OUTPUT KG
Naphthalene 1010
Sulphuric acid 2030
Water 220
Oleum 2860
8620
Nitric Acid 980 NOx
(Scrubbuing 350
9525
LSP 5000
Glauber Salt 3500 CO2 1400
Water 8500
31045
Water 750 Gypsum(73%) 9600
(Sludge)
22597 Nitro sollution
Steam 5420
CI Powder 940 Effluent 3920
Acetic acid 50
Soda Ash 410
25996
Iron Sludge(70%) 1950
Water 5710 (Sludge)
31269 Amino Sol.
Rec.Water 8345
Caustic Flakes 1800 Methenol(Rec) 510
Methanol 575
21759 Fusion Mass
Spent acid 8930
Sulphuric acid 1000 SO2 710
Water 4750
42827
Mother liquor 25100
Mother liquor 900
drying loss 650
H acid 1000
Mass Balance 54435 54435
Mass Balance of H - Acid
Sulphonation
Nitration
Neutralizer
Filtration
Reduction
Filtration
Evaporator
Fusion
Isolation
Filtration
Centrifuge
H - Acid
Associated Dyestuff Pvt. Ltd. (Unit-IV) 10
4. FC Acid
Manufacturing Process:
PNCBOSA is condensing by PPD. Then filter it and condense mass is reduce
by C.I. powder and HCl. Then bring pH 9.0 by soda ash. Filter it. Then
isolated it by HCl. Again filter it and finally get product FC acid.
Chemical Reaction:
Mass Balance:
Input KG KG Output
PPD 620
PNCBOSA 1385
Soda Ash 410
Water 8275
Water 1030 4170 ML to MEE
C.I. Powder 1140 340 CO2 to air
HCl 1450
Soda Ash 520
Water 1040 2555 Iron Sludge (70%)
HCl (30-35%) 1450
Wash water 1050 9170 ML to MEE
455 ML to MEE
680 Drying loss
1000 F.C. acidFinal Product
Isolation
Nutch
Centrifuge
Mass balance of FC acid
Condensation
Filter
Filter
Reduction
Associated Dyestuff Pvt. Ltd. (Unit-IV) 11
5. MUA
Manufacturing Process
Dissolve MPD in 30% HCl. During the process temperature will reach up to
60c due to exothermic reaction. After the completion of reaction cools
down the mass up to 10c & charge 580 kg sodium cynate. Stir it for 5 to 6
hours. Then filter and remove effluent. Centrifuge the product and pack in
HDPE bags.
Chemical Reaction
Mass Balance
INPUT KG OUTPUT KG
800
HCL (30%) 2000 HCL
580 Vent Out
1000
1000 3000
Washing ML 1000
380
MUA 1000
5380 5380
ICE
Wash Water
Mass Balance of MUA
CondansationNaOCN
Filteration
MPDCommon
HCL
Scrubber
Centrifuge Dil. Sulphuric Acid
Final Product
Dil. Sulphuric Acid
Associated Dyestuff Pvt. Ltd. (Unit-IV) 12
6. Sulpho Tobias Acid
Process Description:
Oleum & Tobias Acid is charged in Sulphonator vessel. After 12 hrs the
reaction completes & the reaction mass is dumped into drowning vessel
where ice & salt are added. After drowning, reaction mass is filtered
through Nutch filter. The product remains at the top of Nutch filter & the
filtrate as wastewater goes to the effluent treatment plant. The product
from the Nutch filter is taken into the centrifuge for drying. After drying,
the product is packed & dispatched.
Chemical Reaction
Mass Balance:
INPUT Kgs Kgs OUTPUT
Oleum (23%) 3000
Tobias Acid 1000
Ice 9000
Salt 2500
12075 Effluent
1500 Effluent
1925 Final Product(65%)
1250 Kg Real Basis
Total 15500 15500
Products Wet
cake
Mass balance of Sulpho Tobias Acid
Centrifuge
Nutch Filter
Sulphonation
Drowning
Associated Dyestuff Pvt. Ltd. (Unit-IV) 13
7. Sulpho J- Acid
Process Description:
Oleum and J-Acid is charged in Sulphonator vessel and heated to maintain
required temperature. Add sulphuric acid and After 12 hrs the reaction is
complete and the reaction mass is dumped in to drowning vessel where ice,
water, high flow and carbon are charged. The batch is filtered through Nutch
filter/ filter press. The filtrate is taken for second stage of isolation. The filtrate is
taken in to vessel where salt are charged. The batch is filtered through Nutch
filter/filter press. The wet cake of product is centrifuged and dried which is
packed and dispatched. The filtrate is passed through ETP.
Chemical reaction:
Mass Balance:
INPUT Kgs Kgs OUTPUT
J-Acid 1500
Oleum(65%) 6450
Sulphuric Acid 1075
Water 15000
Ice 8250
Salt 4250
27950 Effluent
6575 Effluent
2000 Final Product(50%)
1000 Kg Real Basis
Total 36525 36525
Centrifuge
Products Wet
cake
Drowning
Isolation
Mass balance of Sulpho -J- Acid
Reflux
Clarification
Nutch Filter
Associated Dyestuff Pvt. Ltd. (Unit-IV) 14
8. MPDSA
Manufacturing Process:
Step-1: Sulphonation - Dechlorination
3, 4 DNCB is converted in 2,4dinitro phenyl sulphonic acid with the help
of sodium sulfite (prepared by sod. Sulphate + caustic lye) isolated and
filtered.
Step 2: Reduction
Nitro mass converted in amino mass by reduction with HCl + iron powder.
Di-nitro phenylene is converted in to Meta. Phenylene diamino sulfonic
acid by reduction with iron + HCl. Filter to remove iron sludge. Filtrate is
isolated with HCl. Product is filtered, centrifuge dried for packing. Mother
liquor is send to ETP.
Chemical Reaction:
NO2
NO2
Cl
+ 2 Na2SO3
MGO
Catalyst
NO2
NO2
SO3H
+ NaCl + Na2SO4
Sodium Slufite3,4 DNCB 3,4 dinitro sulphonic acid
Sulpho dichlorination
Drawning
NO2
NO2
Cl
3,4 DNCB
+ H2O
NO2
NO2
SO3H
+
3,4 dinitro sulphonic acid
H2O
Reduction
NO2
NO2
SO3H
+
3,4 dinitro sulphonic acid
Fe + HCl
Iron Powder
NH2
NH2
SO3H
+
Meta phynylene diamine 4-sulphonic acid
FeCl2 + H2O
Associated Dyestuff Pvt. Ltd. (Unit-IV) 15
Mass Balance:
INPUT KG OUTPUT KG
1725
1135
380
2200
1200
2000
Wash Water 1200 Dilute washing ML 1500
Effluent water 4500
1900
140
150
Wash Water 1300
Iron sludge 3800
2200
1000
3000
2300
Water loss 430
MPDSA 1000
16530 16530
Final Product
Sulpho Di
Chlorination
Water
Filteration
Filtration
DrawningNaCL
Water
NaClDrawning
water
CI Powder
ReductionHCL (30%)
Org.Effluent water
Dil washing ML
Centrifuge
Drying
Filtration
Soda ash
Mass Balance of MPDSA
2 4 DCNB
Sodium Trisulphite
MGO
Associated Dyestuff Pvt. Ltd. (Unit-IV) 16
9. DASA
Manufacturing Process:
Acetanilide flakes is sulphonated by Chloro Sulphonic Acid.Then dump in ice and
get Acetyl Sulphone Chloride. Now PPD is condensed with Acetanilide. Sulphanil
Chloride. Then hydrolyze by Caustic Lye .Then filter it and isolated bySulfuric
Acid at 6.5 pH. Then filter it and centrifuge it. The final product ispacked as a
D.A.S.A.
Chemical Reaction:
Associated Dyestuff Pvt. Ltd. (Unit-IV) 17
Mass Balance:
INPUT KG KG
Acetanilide 1330 HCl 360
Chloro Sulphonic Acid 3200
ICE 2670
Wash Water 1200 Spent Acid (25-30%) 6040
PPD 935
Soda Ash 335
Caustic Flakes 830
Water 3800
HCl (30%) 1330
Wash Water 1670 ML to MEE 8090
ML to MEE 1140
Drying loss 670
DASA 1000
Total 17300 17300
Mass Balance of DASA
OUTPUT
Sulphonation
Sulphonation
Filtration
Condensation
Hydrolysis
FiltrationIsolation
Nutch
FiltrationCentrifuge
DMA V.S.Final Product
Dumping
Associated Dyestuff Pvt. Ltd. (Unit-IV) 18
10. Vinyl Sulphone (PBVS)
Manufacturing Process:
Chloro Sulphonation: In a reaction vessel, chlorosulphonic acid is taken
through pipeline from storage tank. The Acetanilide powder is added manually
through funnel. The reaction is exothermic and temperature is maintained at 20-
25oC by chilled water circulation in jacket. HCl gas is evolved during the
reaction, which is injected to a scrubber containing water to scrub the vapors
and HCl is recovered. The reaction mixture is dumped into a SS reactor where
TC being added. After the reaction is over, the material is dumped into ice in a
MS/RL/BL tank.
Drowning: The sulphonated mass is filtered and recovery of 25-30% acid is
made as spent acid and kept in separate HDPE storage tanks.
Reduction: In as SS reaction vessel water and Sodium Bi Sulphite are taken
and caustic lye is added. Caustic lye is pumped into a measuring tank and added
by gravity. The Sulphone Chloride mass is then charged into it.
Condensation: The above mass is transferred into another vessel by pump
through closed pipeline and heated to 50oC. Ethylene Oxide is then passed very
slowly with nitrogen blanket in the vessel. After the reaction is over, the mass is
Filtered through a Nutch and product is centrifuged and dried. Dilute Sulphuric
acid is added to maintain pH at 7.0-7.5 in the process.
Esterification: The above product is taken in an ester vessel and calculated
quality of concentrated sulphuric acid is charged. Sulphuric acid is taken to a
measuring tank from storage tank and fed by gravity. The mass is heated by oil
to 150oC under vacuum. Acetic Acid fumes are evolved which are taken to a
condenser is collected as by-product, which in turn used to manufacture
Acetanilide VS lumps are collected, pulverized, blended and packed for sale.
Associated Dyestuff Pvt. Ltd. (Unit-IV) 19
Chemical Reaction:
NHCOCH3
SO2Na
Condensation
+ + H2SO4
NHCOCH3
+ Na2SO4 + H2O
Esterification
+ H2SO4
NH2
OHO2S
O2SOSO3H
+ CH3COOH
Reduction
NHCOCH3
SO2Cl
+ 3NaOH + NaHSO3
NHCOCH3
SO2Na
+ Na2SO4+ NaCl+ 2H2O
O
H2C CH2
NHCOCH3
OHO2S
Associated Dyestuff Pvt. Ltd. (Unit-IV) 20
Mass Balance:
INPUT KG OUTPUT KG
Water 225
NaOH 55
555
1475 HCl HCl 320
480 SO2 SBS 345
3110 Spent Acid 4390
2225
345
125 Rec.of Salts 315
665
Ethylene Oxide 285
Spent acid 775
Effluent 4430
1665
655
Drying Loss 675
345 Acetic acid 200
PBVS 1000
12330 12330
Mass Balance of PBVS
Acetanilide
SulphonationChloro Sulphonic acid HCl/SOx
ScrubberThionyl Chloride
ICEDrawning
water
SBS Slurry
ReductionSBS
Caustic Lye
Ethoxylation
CondansationWash water
Final Product
Effluent
Drying
EsterificationSulphuric acid
Centrifuge
Associated Dyestuff Pvt. Ltd. (Unit-IV) 21
11. OAVS
Manufacturing Process:
Acetyl orthoanisidine is charged in to chloro sulphonic acid below 300C. After the
addition the temperature is raised to 50-550C and maintained for 4 hours. It is
cooled and drowned over ice and filtered. The Sulpho chloride is charged in to
slurry of sodium bi sulphate and made neutral with caustic and the pH is
maintained at 7 Ethylene oxide is passed in to the solution maintaining pH 7 by
adding H2SO4. When the reaction is complete, it is filtered and dried. It is further
clarified by heating with calculated quantity of H2SO4 and then pulverized.
Chemical Reaction:
Associated Dyestuff Pvt. Ltd. (Unit-IV) 22
Mass Balance:
INPUT KG OUTPUT KG
Acetyl Ortho Ansidine 715 HCl 156
Chloro sulphonic acid 3033
Ice 1950 Spent acid(23-25%) 4270
Sodium bisulphite 650
Caustic lye 1191
Ethylene Oxide 585 Effluent for Glauber 3875
Sulphuric acid 1069 Salt recovery
Sulphuric acid 317 Acetic acid 209
1000
Mass Balance 9510 9510
Mass Balance of OAVS
Sulphonation
Sulphonation Dumping
Reduction
Ethoxylation
Esterification
Pulverization
Pulverization OAVS
12. Sulpho VS
Manufacturing Process:
Vinyl Sulphone Ester is charged in to sulphuric acid below 30oC. Then charge
Oleum 65% in it & dumps this sulpho mass in ice and water & salted out by
potassium chloride. Then filter it and centrifuge it. The final product is packed as
a Sulpho VS.
Chemical Reaction:
NH2
SO2OCH2CH2SO3H
+ H2SO
4 + H2S
2O
7
NH2
SO2OCH2CH2SO3H
SO3H
Mass Balance:
INPUT KG OUTPUT KG
629
629
810
Ice 1396
KCL 461
Spent Acid 2925
Sulfo VS 1000
3925 3925
Nutch & Centrifuge
Final Product
Mass Balance of Sulfo VS
SulphonationOleum Acid (65%)
Sulphuric Acid
Drawning
Vinyl Sulphone
Associated Dyestuff Pvt. Ltd. (Unit-IV) 23
13. Sulpho OAVS
Manufacturing Process:
Sulphonation:
The Sulphonation is carried out in a C.I. Sulphonator; Ortho anicidine Sulfo VS is
heated with Sulfuric Acid and Oleum (65%) at a temperature of 50oC,
Sulphonation takes place and Sulpho orthoanicidinevinyl sulphone is formed.
Check acidity of S/mass and the sulphonated mass is blown in to the drawning
vessel.
Drawning:
The drowning is carried out in MSRLTL vessel. Take water and ice in drowning
vessel and charge s/mass dumping in at 5 C temperatures the ice and water
then charge KCL in it and precipitate the SOAVS and then filtrate it in MSRLTL
nutch.
Chemical Reaction:
OCH3
SO2OCH2CH2SO3H
NH2
OAVS
Sulphonation
Drawning
+ H2S2O7 + H2SO4
OCH3
SO2OCH2CH2SO3H
NH2
+SO3H
H2SO4 + H2O
SOAVS
OCH3
SO2OCH2CH2SO3H
NH2
+SO3H
H2SO4 + H2O
SOAVS
OCH3
SO2OCH2CH2SO3H
NH2
+SO3H
H2SO4 + H2O
SOAVS
Aniline-(2-methoxyphynyl 3- Ethyl sulfonyl
sulphate-2-Sulfonic Acid
Mass Balance:
INPUT KG OUTPUT KG
OAVS 1000
Oleum Acid (65%) 1770
Sulphuric Acid 1450
water 1000
Ice 8000
KCL 1300
Wash water 1000 Dil. Sulphuric Acid 14070
Drying loss 450
Sulfo OAVS 1000
15520 15520
Final Product
Filtration &
Centrifuge
Mass Balance of Sulfo OAVS
Sulphonation
Drawning
Associated Dyestuff Pvt. Ltd. (Unit-IV) 24
14. PCVS
Manufacturing Process:
Acetyl paracresidine is charged in to chloro sulphonic acid below 30oC.
After the addition the temperature is raised to 50-55oC and maintained
for 4 hours. It is cooled and drowned over ice and filtered. The Sulpho
chloride is charged in to slurry of sodium bi Sulphate and made neutral
with caustic and the pH is maintained at 7. Ethylene oxide is passed in to
the solution maintaining pH 7 by adding H2SO4. When the reaction is
complete, it is filtered and dried. It is further clarified by heating with
calculated quantity of H2SO4 and then pulverized.
Chemical Reaction:
Associated Dyestuff Pvt. Ltd. (Unit-IV) 25
Mass Balance:
INPUT KG OUTPUT KG
Para Cresidine 500
Acetic anhydride 640
ChloroSulphonic acid 3600 HCl 90
Ice 9500
Spent Acid 2800
Washing 2000 Spent acid 16500
SBS 400
Water 13500
Caustic lye 1200
Sludge 10
Effluent 15150
Dil. H2SO4 600
Ethylene Oxide 400
Wash Water 8000 Effluent 10200
Evapo.loss 310
Sulphuric Acid (98%) 300 Acetic acid 180
Product 1000
Total 43440 43440
Mass Balance of PCVS
Acetylation
Sulphonation
Drowning
Filtration
Esterification
PCVS
Reduction
Filtration
Condensation
Filtration
Drying
Associated Dyestuff Pvt. Ltd. (Unit-IV) 26
15. DMAVS
Manufacturing Process:
Di methoxy Aniline is charged in to chloro sulphonic acid bellow 300C. After the
addition the temperature is raised to 50-550C and maintained for 4 hours it is
cooled and drowned over ice and filtered. The Sulpho chloride is charged in to
slurry of sodium bi sulphate and made natural with caustic and the pH is
maintained at 7 Ethylene oxide is passed in to solution maintaining pH 7 by
adding H2SO4. When the reaction is complete, it is filtered and dried. It is further
clarified by heating with calculated quantity of H2SO4 and then pulverized.
Chemical Reaction:
Associated Dyestuff Pvt. Ltd. (Unit-IV) 27
Mass Balance:
INPUT KG OUTPUT KG
Acetic Anhydride 840
2:5 DMA 700
Chlorosulphonic acid 4500 HCl 127
Ice 11550
Washing 3500 Spent acid 17000
SBS 550
Water 1500
Caustic lye 1150
Sludge 10
Dil. H2SO4 600
Ethylene Oxide 400
Wash Water 1000 Effluent 7700
Evapo.loss 610
Sulphuric acid 357 Acetic acid 200
1000
Total 26647 26647
Mass Balance of DMAVS
Acetylation
Sulphonation
Drowning
Filtration
Reduction
Filtration Filtration
Condensation
Filtration Filtration
Drying Drying
Esterification Esterification
DMA V.S. DMA V.S.
Filtration
Associated Dyestuff Pvt. Ltd. (Unit-IV) 28
Annexure-III
Water Balance
Sr. No.
Source Water Consumption
(KLD)
Wastewater Generation
(KLD)
I Domestic 15 12
II Gardening 50 -
III Industrial
a) Process 1054 950
b) Scrubber 93 5
c) Boiler 200 20
d) Cooling 150 30
e) Lab 5 5
f) Washing 100 100
Total Industrial 1602 1110
Total (I+II+III) 1667 1122
Recycle water 1346 -
Actual fresh water
requirement
321 -
Associated Dyestuff Pvt. Ltd. (Unit-IV) 29
Water Balance Diagram
Total Raw Water consumption = 1667 KLD
(321 fresh KLD + 1346 recycle KLD)
(Fresh + recycle water)
Domestic 15
Washing 100
Lab 5
Process Water 622 Greenbelt
50
Cooling 150 5
100
Scrubber
93
30
Bleed
off
Boiler
200
Total
50
Dyes
Interme
diate
Plant 402
Steam 58
Drying loss 18
H2SO4 196
Effluent 694
Ice 222 Recover
water 166*
VS Plant
220
Water from RM 142
H2SO4
193
Effluent
256
Ice 210
MEE-1 GS
recovery
123
ETP-1
694+256+5+5 = 960
SBS 38
5
HCl 42
Acetic acid 8
RO
Recycle-576*
Reject-384
Soak Pit 12
MEE 2-414 Condensate
389*
Solid waste 15
ETP-2 100 + 50 = 150
G salt 22
20
Blow down
Utilities 350
Water 95*
Loss 6
RO 150
Recycle-120*
Reject-30
Ice Plant 432
10 System loss
Associated Dyestuff Pvt. Ltd. (Unit-IV) 30
Annexure IV
ETP-1
Primary & tertiary treatment, Capacity-1000 KLD
S.
No.
Name of Unit Dimensions (m) No. of
Unit
Capacity in
KL
1. Collection Tank 7.5 x 7.5 x 4, LD: 3.5 2 200 each
2. Neutralization Tank 5 x 5 x 3.5, LD: 3 2 75
3. Lime Dosing Tank 2.0 x 2.0 x 2.0 1 8
4. Alum Dosing Tank 2.0 x 2.0 x 2.0 1 8
5. Poly Flock Dosing Tank HDPE Tank 1 1
6. Primary clarifier 12.0 Ø x 3.0 1 282
7. Holding tank 5.0 x 5.0 x 4.0 1 100
8. Pressure Sand Filter Standard supply 2 25 KL/Hr
9. Filter Press 40” x 40” x 36” plates 2 -
10. Sludge Drying area 12 x 20 x 1.2 2 240 m2
surface area
11. Holding Tank 5 x 5 x 3.5, LD: 3 1 75
12. RO unit - 2 sets 10 m3/hr.
50 m3/hr.
13. Permeate Holding Tank 5.5 x 5.5 x 4, LD: 3.5 1 100
14. Reject Holding Tank 5.5 x 5.5 x 4, LD: 3.5 1 100
15. Multi Effect Evaporator-1 - 1 10 m3/Hr G. Salt
recovery
16. Multi Effect Evaporator-2 - 1 50 m3/Hr
17. MEE Condensate
Collection tank
7.5 x 7.5 x 4, LD: 3.5 1 200
Associated Dyestuff Pvt. Ltd. (Unit-IV) 31
ETP-2
Primary, secondary & tertiary treatment, Capacity-150 KLD
Sr.
No.
Name of Unit Dimension
(Size) (m)
No. of
Unit
Capacity in
KL
1. Collection Tank 5 x 5 x 3.5, LD: 3 1 75
2. Neutralization Tank 5 x 5 x 3.5, LD: 3 1 75
3. Chemical Dosing tanks Standard supply 3 2 each
4. Primary clarifier 7.0 Ø x 3.0 1 96
5. Holding Tank 5 x 5 x 3.5, LD: 3 1 75
6. Pressure Sand Filter Standard supply 1 10 KL/hr.
7. Carbon Filter Standard supply 1 10 KL/hr.
8. Filter Press 40” x 40” x 36” plates 1 -
9. Sludge Drying area 10 x 15 x 1.2 2 150 m2
surface area
Associated Dyestuff Pvt. Ltd. (Unit-IV) 32
Annexure-V
Details of Hazardous/Solid waste
Sr.
No.
Types of
Waste
Sources Category
of Waste
as per
HWM
Rules
2016
Quantity Composition
1 ETP Sludge ETP 35.3 250
MT/month
Collection, storage,
transportation & disposal at
TSDF site approved by GPCB
2 Salt from MEE/
ATFD/SD
MEE 35.3 375
MT/month
Collection, storage,
transportation & disposal at
TSDF site approved by GPCB
3 Iron sludge
(Process waste)
Process 26.1 975
MT/month
Collection, storage,
transportation & disposal at
TSDF site approved by
GPCB/ cement industry
4 Gypsum Sludge Process 26.1 4800
MT/month
Collection, storage,
transportation & disposal at
TSDF site approved by
GPCB/ cement industry
5 Spent Oil Driving
unit &
D.G. set
5.1 1.0
MT/Yr.
Collection, storage,
transportation & use within
premises as a lubricant/ sell
to registered recycler.
6 Discarded
containers /
barrels/liners
Raw
material
33.1 Drums
10000
nos./month
Liners
5
MT/month
Being used for packing of
ETP sludge in case of excess
it will be sold to approved
recycler or traders
7 Spent H2SO4 from
process
26.3 4825
KL/month
Captive use for our other
products manufacturing
8 HCl from
process
26.3 1050
KL/month
Sold to actual users
9 Acetic acid from
process
26.3 200
KL/month
Sold to actual users
10 SBS from
process
26.3 950
KL/month
Captive use for our other
products manufacturing
11 Glauber Salt from
process
26.1 550
MT/month
Sold to actual users
Associated Dyestuff Pvt. Ltd. (Unit-IV) 33
Annexure-VI
Source of Air Emissions
Sr.
No.
Stack attached to Fuel Type Stack
Height
in m
APC measures Probable
emission
Flue Gas Stacks
1 Boiler (8 TPH)-2
nos. One stand by
Coal-30 45 Cyclone & Bag filter SPM <150 mg/Nm3
SO2 <100 ppm
NOx <50 ppm 2 Thermo pack Fluid
heater (25 lacs
Kcal/Hr)
Coal/ Lignite-
17 TPD
35 Cyclone & Bag filter
3 Hot air Generator- 2
nos. (45 lacs
Kcal/Hr each)
Coal/ Lignite-
60 TPD
31 Cyclone & Bag filter
4 D.G. set- 2 Nos.
(500 KVA each)
HSD-
50 lit/hr-each
15 ---
Process Gas Stacks
VS and other intermediates Plant
4 Reaction vessel
(VS Plant)
-- 21 Two stage water
scrubber and Alkali
scrubber
SO2 < 40 mg/Nm3
HCl < 20 mg/Nm3
5 Reaction vessel
(VS Plant)
- 21 Two stage water
scrubber and Alkali
scrubber
HCl < 20 mg/Nm3
H acid Plant
6 Nitration reactor
(H-Acid plant)
- 21 Two stage Alkali
Scrubber
NOx <25 mg/Nm3
7 Isolator of H-Acid
Plant
- 21 Two stage Alkali
Scrubber
SO2 < 40 mg/Nm3
Other Intermediates
8 common ducting
connect with
intermediates plant
- 21 Two stage alkali
scrubber (Soda ash)
SO2 <40 mg/Nm3
9 K acid-Amidation - 21 Two stage water
Scrubber
NH3 <175 mg/Nm3
10 SFD-4 nos. - 15 Inbuilt Cyclone and
bag filter SPM <150 mg/Nm3