annexure-i list of products product capacity (mt/month) · annexure-i list of products sr. no....

33
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

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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) 8

Chemical Reaction:

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