Annexure-I List of Productsenvironmentclearance.nic.in/writereaddata/Online/TOR/14...7 PNTOSA (Para...

Parshwanath Intermediates, Kadi 0

Annexure-I

List of Products

Sr. No.

Name of Product (commercial Name)

IUPAC Name CAS No. Production capacity

Bromination:

1 Bromanoine Acid -- 116-81-4 80

2 N-Propyl Bromide (N P Br) -- 106-94-5

3 Iso propyle Bromide (I P Br)

-- 75-26-3

4 Ethyle Bromide -- 74-96-4

5 Calcium Bromide 52%

solution

-- 7789-41-5

6 Cetyl Bromide -- 112-82-3

7 EDBr (Ethyle di Bromide) -- 106-93-4

8 HBr (Hydro Bromic Acid) -- 10035-10-6

9 N- Butyl Bromide -- 109-65-9

Sulphonation

1 Scheaffer Acid (6-hydroxy naphthalene-2-

sulfonic acid)

93-01-6 100

2 G Salt

(1,3-Naphthalene disulfonicacid)

842-18-2

3 Alpha Napthol -- 90-15-3

4 ONTSA (Ortho Nitro Toluene Sulfonic Acid)

--

5 EBAMSA (N-Ethyl-N-Benzyl Aniline m-Sulphonic Acid)

-- 101-11-1

6 Aniline 2:5 DSA (Aniline 2:5 Di Sulfonic Acid)

-- 98-44-2

7 PNTOSA (Para Nitro Toluene Sulfonic Acid)

-- 121-03-9

8 MPDDSA (Meta Phenylene Diamine Disulfonic Acid)

-- 137-50-8

1 PCOSA (Para Cresidine Ortho Sulphonic Acid)

-- 6471-78-9 30

2 Sulpho C Acid

(2-Napthyl Amine, 4-6-8 Tri Sulphonic Acid)

--

Other Product

1 Sodium Naphthionate 130-13-2 80

2 N W Acid -Neville Winther’s Acid

1-Naphthol-4-sulfonic acid

84-87-7

3 4 CAP (4- Chloro 2- Amino Phenol)

-- 95-85-2

4 3,5 DABA (3,5 Di Amino Benzoic Acid)

-- 535-87-5

5 2 Pyridone (Carbamol Pyridone)

-- 1003-56-1

6 PAABSA (Para Amino Azo -- 104-23-4


Benzene Sulphonic Acid)

7 5 NAP (5-Nitro 2 Amino

Phenol)

-- 121-88-0

8 4 Sulpho Anthranilic Acid -- 98-43-1

9 2 :5 DCPNA (2:5 Di Chloro

Para Nitro Aniline)

-- 6627-34-5

10 Metanilic Acid -- 121-47-1

11 4 NAPSA (4 Nitro 2 Amino

Phenol 6 Sulfonic Acid)

-- 96-67-3

12 6 NAPSA (6-Nitro 2 Amino

Phenol 4 Sulfonic Acid)

-- 96-93-5

13 MAP (Meta Amino Phenol) -- 591-27-5

14 4 Sulpho Hydrozone -- 118969-29-2

15 DABA (2,5 Diamino Benzoic Acid)

--

16 Mix Cleave Acid / 1 -6 Cleave Acid/ 1-7 Cleave

Acid

-- 51548-48-2

17 PPA (Phenyl Peri Acid)

(8-Anilino-1-naphthalenesulfonic acid)

-- 82-76-8

18 C Acid 2-

Naphthylamine 4,8 di Sulfonic

acid

131-27-1

19 4 ADAPSA (4 Amino Di

Phenyl Amine Sulphonic Acid)

-- 91-30-5

20 K Acid 4-Amino 5-Hydroxy

Naphthalene 1,7

Di Sulphonic acid

118-03-6

21 3 5 DNBA (3,5 Di Nitro Benzoic Acid)

-- 99-34-3

1 OPSAMIDE (Ortho amino phenol para sulfonamide)

2-Amino Phenol 4- sulfonamide

98-32-8 50

2 Peri Acid / Laurrent Acid 1,8-Naphthylamines

ulfonic acid / 1-Naphthylamine-5-sulfonic acid

82-75-7 / 84-89-9

3 Broner Acid 2-Amino-6-naphthalenesulf

onicacid

93-00-5

4 Cromotropic Acid 1,8 Dihydroxy

3,6 Disulfo Nepthelene

148-25-4

5 PPD (Para Phenylene Di Amine)

Benzene-1,4-diamine

106-50-3

6 Violet Acid 1-Naphthol 3,6 Di Sulfonic Acid

578-85-8


7 Koch Acid 1 Naphthyl amine 3,6,8 tri

Sulphonic Acid

117-42-0

1 1 Napthole 8 Sulphonic

Acid

8-hydroxy

naphthalene-1-sulfonic acid

117-22-6 30

2 DTPTSA (Dehydro Thio p- Toluidine Sulfonic Acid)

-- 130-17-6

3 2R Acid Sulpho gamma Acid / 1-

Naphthol-3,6-disulfonicacid

90-40-4

4 Epsilone Acid 1-Naphthol 3,8 Di Sulfonic Acid

117-43-1

5 MDNB (Meta Di Nitro Benzene)

-- 99-65-0

6 DNSDSA (4,4 Dinitro

Stilbene 2,2 Disulfonic Acid)

-- 128-42-7

7 European K Acid

(1-Amino 8 naphthol 4,6

Disulfonic Acid)

40130-23-4

Total 370


List of Raw Material

Sr.

no.

Product name Raw Material Name Quantity

MT/MT

1 Bromanoine Acid

ODCB 0.125

1 Amino Aantra Quinone 0.800

Chloro Sulphonic Acid 0.500

Liquid Bromine 0.280

NaCl 1.800

2 n-Propyl Bromide

N-Propyl Alcohol 0.580

Hydrobromic Acid 2.200

3 Iso propyl Bromide

Iso Propyl Alcohol 0.550

Hydrobromic Acid (48%) 1.350

4 Ethyle Bromide

Ethyl Alcohol 0.465

Hydrobromic Acid (48%) 2.790

5 Calcium Bromide

Ca(OH)2 0.160

HBr Solution 0.680

6 Cetyl Bromide

Cetyl alcohol 0.850

Hydrobromic Acid 0.950

7 Ethylene Di Bromide

Ethyl Glycol 1.000

Liq. Bromine 3.700

Sulphur 1.500

8 Hydrobromic Acid (HBr)

Br2 0.680

Sulfur 0.050

9 N- butyle Bromide n-Butanol 0.650

Liquid Bromine 0.750

sulfur 0.250

Soda Ash 0.135

10 Schaeffer's Acid H2SO4 1.050

B Naphthol 0.950

Carbon 0.025

Caustic Lye / Soda 0.850

Salt 0.115

11 G Salt H2SO4 (98%) 1.250

B Naphthol 1.050

Oleum (23%) 1.000

KCl Salt 1.200

12 Alpha Naphthol ANA 1.050

Sulfuric acid 0.800

13 ONTSA ONT 1.000

Oleum 30% 2.050

Salt 1.200

14 EBAMSA EBA 0.850

Oleum 0.850

Sulfuric Acid 0.850

15 Aniline 2, 5 DSA Metanilic Acid 1.000

Sulfuric Acid (98%) 1.200


Sr.

no.


MT/MT

Oleum 65% 1.150

Hyflow 0.015

Activated Carbon 0.055

Sodium Sulphate 0.900

16 PNTOSA PNT 1.150

Oleum 30% 1.800

17 MPDDSA MPD 0.650

Sulphuric Acid 1.050

Oleum (65%) 1.200

18 PCOSA Para Cresidine 0.750

H2SO4 0.850

Oleum 23% 1.800

Salt 0.400

19 Sulpho C Acid C-Acid 1.110

Oleum(65%) 1.335

Sulfuric Acid 1.350

Glauber salt 0.875

20 Sodium Naphthionate ODCB 1.270

H2SO4 0.850

Soda ash 0.425

21 N W Acid Sodium Naphthionate 1.400

Sodium Bisulphite 1.800

H2SO4 (38%) 2.000

Caustic Lye 0.850

Hydrochloric Acid 0.950

22 4-Chloro 2-Amino Phenol (4 CAP)

2:5 DCNB 1.200

Caustic 0.500

Iron powder 0.135

HCl 0.125

23 3,5 DABA Benzoic Acid 0.085

Sulphuric Acid 98% 1.500

Nitric Acid 98% 1.000

Iron 1.150

HCl 0.350

Caustic Lye (47-48%) 0.450

HCl (30%) 1.800

24 2 Pyridone Mono Ethyl Amine 0.500

Methyl Cyno Acetate 0.625

Methyl Aceto Acetate Ester 0.750

H2SO4 3.200

25 PAABSA Sodium bisulphite 0.620

37% Formaldehyde 0.550

Aniline oil 0.500

Salt 1.650


Sr.

no.


MT/MT

Sulphonic Acid 0.850

30% HCl 0.620

Sodium nitrite 0.350

Sodium bicarbonate 0.650

98% Sulphonic acid 1.000

26 5 NAP OAP 0.800

Acetic Anhydride 0.750

HNO3 0.750

H2SO4 1.000

Caustic Soda 0.120

27 4 Sulpho Anthranilic

Acid

ONT 1.000

65% Oleum 1.050

98% Sulphuric Acid 0.900

Caustic Soda flakes 1.000


28 2:5 DCPNA(2:5 Di

Chloro Para Nitro Aniline)

2-5 DCA 0.750

Acetic Anhydride 0.650

H2SO4 0.850

HNO3 0.650

29 Metanilic Acid Nitro benzene 0.850

Oleum (25%) 1.500

Calcium hydroxide 1.200

HCl (30%) 0.450

Iron Powder 0.900

Soda Ash 0.500

H2SO4 (98%) 0.800

30 4 NAPSA Lime 0.250

NaSH 0.600

4 Nitro Chloro Benzene 0.800

Oleum 0.850

HNO3 0.320

H2SO4 0.650

31 6 NAPSA OAP 0.520

Oleum (23%) 1.000

HNO3 0.320

H2SO4 0.650

32 MAP (Meta Amino Phenol)

Metanilic Acid 1.600

NaOH 0.800

Catalyst 0.008

33 4 Sulpho hydrazone 4 Sulpho Anthranilic Acid 1.200

HCl (30%) 2.150

Sodium Nitrite 0.350

Sodium bisulphite 0.900

Caustic Soda 0.550


Sr.

no.


MT/MT

Benzaldehyde 0.650

34 DABA (2,5 Diamino Benzoic acid)

Benzoic Acid 1.350

Nitric Acid (98%) 1.250

H2SO4 (98%) 3.770

Cast Iron Powder 2.280

HCl(30-35%) 1.750

Soda Ash 0.270

35 Mix Clave Acid (1,6 Cleves Acid & 1,7

Cleves Acid)

Nepthaline 0.950


Nitric acid (68%) 0.650

Lime stone Powder 1.450

Soda 0.450

HCl 0.185

Acetic Acid 0.085

Sulphuric Acid (40%) 0.800

36 Phenyl Peri Acid (PPA) Peri Acid 0.900

Aniline oil 0.750

Hyflow 0.020

Carbon 0.010

HCl 0.180

37 2- Naphthylamine 4,8 di Sulfonic acid (C

Acid)

Naphthalene 1.250

Sulphuric Acid(98%) 1.200

Oleum 65% 1.450

Nitric Acid 0.325

Mgo 0.350

HCl 0.055

Iron 0.450


38 4-ADAPSA PNCBOSA 1.000

Aniline Oil 0.350

NASH 1.400

NaHSO3 1.200

HCl 1.800

39 K-ACID G-Salt 0.710

Ammonia (25%) 0.700

SBS 0.125


Oleum Acid (65%) 2.200

KCl 0.350

40 3,5 DNBA (3, 5 Di

Nitro Benzoic Acid)

Benzoic Acid 0.550

H2SO4 2.500

2HNO3 0.900

Oleum 1.200

41 Opsamide Chloro Sulphonic Acid 3.000


Sr.

no.


MT/MT

ONBC 1.200

Ammonia/Mono methyl Amine/ Anthranilic Acid

0.450

HCl 30% 0.125

Caustic Lye 1.075

HCl 0.630

NAHS Solution (30%) 0.550

42 Peri Acid & Laurentˈs Acid

Naphthalene 0.850


Nitric Acid 0.450

Lime Stone 1.800

Magnesium oxide 0.450

HCl 0.350

Iron Powder 0.850

43 Broner Acid Beta Napthole 1.500

H2SO4 1.450

Carbon 0.010

Glauber's Salt 1.000

HCl 2.500

Ammonia 28% 2.200

Schaffers acid 1.500

SBS 0.350

44 Chromotropic Acid H- Acid 1.450

NaOH 0.950

Salt 0.025

H2SO4 0.750

45 PPD PNA 1.650

Caustic Flakes 0.350

Sulphur 0.250

NaSH 0.800

46 Violet Acid Naphthalene 0.800


Oleum(65%) 2.000

Lime Stone 2.000

Sodium Sulphate 1.250

Caustic Flaks 1.200

HCl 0.550

47 KOCH ACID Napthalene 0.350


Oleum 0.500

Nitric Acid 0.270

Lime Stone 1.500

Soda Ash 0.170

Iron Powder 0.300

HCl 0.035


Sr.

no.


MT/MT


48 1-Naphthol 8-Sulphonic Acid

Peri Acid 0.450


NaNo2 0.350

Diazo mass 1.500

Caustic lye 0.350

49 DTPTSA Para Toluidine 0.350

Sulphar 0.300

Para Toluene 0.700

Sulphonic Acid 0.250

50 2R Acid K Acid 1.500

NaOH 1.550

H2SO4 1.000

51 Epsilone Acid Oleum 65% 1.000


Napthalene 1.800

Nitric Acid (98%) 0.850

Lime Stone 2.500

Mgo 0.750

Iron Powder 1.800

HCl 0.540


Sodium nitrite 0.325

52 Meta Di Nitro Benzene Nitro Benzene 0.780

Nitric Acid 0.460

Sulphuric acid 0.925

Caustic lye 0.050

53 DNSDSA PNTSA 1.750

Soda Ash 0.130

Caustic Lye 1.200

H2SO4 0.800

54 European K Acid Napthalene 0.750

Oleum (65%) 1.100

Nitric Acid 0.600

Lime Stone 1.350

Soda Ash 0.300

Iron Powder 0.650

HCl 0.075

Caustic lye 0.450



Annexure-II

Manufacturing Process

1. Bromanoine Acid

Manufacturing Process:

Add Sulpho Di Chlorination, Add Water, Add ODCB, Add 1 Amino Anthra

Quinone, Add Chloro Sulphonic Acid, Removal of HCl. Drawning Add

Water, Sent as residue Waste, ODCB recovery. Bromination Add Liquid

Bromine, Add NaCl. Filtration followed by Drying removal as an effluent,

Final Product Bromanoine Acid.

Mass Balance:

INPUT KG OUTPUT KG

ODCB 4200

1 Amino Aantra Quinone 800 HCl/SO2 315

Chloro Sulphonic Acid 500

Water 500

Water 2200 Residue 125

ODCB Recovery 4075

Water 2200

Liquid Bromine 280

NaCl 1800

Waste Water 5840

Drying loss 1125

Bromanoine Acid 1000

Total 12480 12480

Mass Balance of Bromanoine Acid

Sulpho Di

Chlorination

Distillation

Bromination

Filtration

Drying

Drawning


2. N-Propyl Bromide


First we take catalyst, water and NPA in glass lines reactor. Then slowly

Bromine is added in GLR. When Bromine addition is complete, contents are refluxed for 3 to 4 hours. After completion of reflux, distillate is

collected in the receiver and washed with H2SO4 (1% of product) and then acidity is removed by soda ash. Material is then filtered and packed in

drums. SO2 gas is scrubbed in NaOH solution.

Chemical Reaction:

CH3CH2CH2OH + 2Br2 + S CH3CH2CH2Br + Dil. H2SO4

Mass Balance:

INPUT KG OUTPUT KG

N-Propyl Alcohol 580 Recovered HBr (16%) 1545

Hydrobromic Acid 2200

Water 500 Waste water 575

Residue 160

n-Propyl bromide 1000

Total 3280 3280

Mass Balance of n-Propyl Bromide

Washing

Reaction

Vaccum

Distillation


3. Iso Propyl Bromide Manufacturing Process:

Charge Iso Propanol and Hydro bromic acid in reactor under stirring. Then

start slowly addition of Sulfuric acid up to reflux. After completion of

reaction distill it. Wash the product with Soda Ash solution for neutralize.

Then pack in HDPE drum.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Iso Propyl Alcohol 550 Recovered HBr (23%) 870

Hydrobromic Acid (48%) 1350

Water 500 Waste Water 500

Residue 30

Iso propyl Bromide 1000

Total 2400 2400

Reaction

Mass Balance of Iso propyl Bromide

Washing

Vaccum

Distillation


4. Ethyle Bromide


Charge Ethanol and Hydro bromic acid in reactor under stirring. Then

start slowly addition of Sulfuric acid up to reflux. After completion of

reaction distill it. Wash the product with Soda Ash solution for neutralize.

Then pack in HDPE drum.

Chemical Reaction:

CH3–CH2-OH + HBr + H2SO4 CH3–CH2-Br + Dil H2SO4

Mass Balance:

INPUT KG OUTPUT KG

Ethyl Alcohol 465

Hydrobromic Acid (48%) 2790 Recovered HBr(24%) 2110

Water 550

Waste Water 585

Residue 110

Ethyl Bromide 1000

Total 3805 3805

Mass Balance of Ethyle Bromide

Reaction

Wash Water

Vacuum

Distillation


5. Calcium Bromide 52% solution


Charge calcium hydroxide and water in reactor under stirring. Then start

slowly addition of Hydro bromic Acid. After completion of reaction stir the

mass and filter it. Finally pack in HDPE drum.

Chemical Reaction:

Ca(OH)2 + HBr CaBr2 + H2O

Mass Balance:

INPUT KG OUTPUT KG

Ca(OH)2 160

HBr Solution 680

Water 450

Drying loss 290

Calcium Bromide 1000

Total 1290 1290

Mass Balance of Calcium Bromide

Reaction

Filteration

Drying


6. Cetyl Bromide


Cetyl Alcohol is taken in Aqueous Hydrobromic Acid. To this Gaseous HBr

is passed, after passing required amount of HBr acid over a given period

of time the mass is analyzed for completion of reaction on GC.

When unreacted Cetyl Alcohol is less than 1% HBr acid addition is

stopped and taken for Water washing.

The Organic is taken in to the Glass lined reactor and water is added.

This mass was stirred at room temperature for about 30 mins. Organic

layer taken for Purification and Aqueous layer containing HBr is recycled

to next Batch.

Organic Layer is then taken for Fractionation after removal of Low Boiler

Impurities under Vacuum, the Product is fractionated. Pure Cetyl

Bromide thus obtained is packed in 200 lit Drums.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Cetyl alcohol 850

Hydrobromic Acid 950 Recovered HBr 710


Cetyl Bromide 1000

Total 2150 2150

Mass Balance of Cetyl Bromide

Reaction

Water wash

Drying &

Packing


7. EDBr (Ethyle di Bromide)


In reactor vessel take Mono ethylene glycol is di Brominated with liquid

bromine in presence of Sulphur as catalyst, to get the product.

Chemical Reaction:

OH-CH2-CH2-OH + Sulphur + Liq. Br2 Br-CH2-CH2-Br + Dil. H2SO4

Mass Balance:

INPUT KG OUTPUT KG

Ethyl Glycol 1000 Waste water 4700

Liq. Bormine 3700 Drying Loss 500

Sulphur 1500 Ethylene Di Bromide 1000

Total 6200 6200

Mass Balance of Ethylene Di Bromide

Reactor vessel


8. HBr (Hydro Bromic Acid)


Charge water and sulfur in reactor under stirring. Then start slowly

addition of Bromine. After completion of reaction distill it. Finally pack in

HDPE drum.

Chemical Reaction:

4H2O +3Br2 + S 6HBr + H2SO4

Mass Balance:

INPUT KG OUTPUT KG

Water 720

Br2 680

Sulfur 50

Waste water 450

HBr (48%) 1000

Total 1450 1450

Product

Mass Balance of Hydrobromic Acid(HBr)

Reaction

Distillation


9. N- Butyle Bromide


First we take catalyst, water and NBA in glass lines reactor. Then slowly

Bromine is added in GLR. When Bromine addition is complete, contents

are refluxed for 3 to 4 hours. After completion of reflux, distillate is

collected in the receiver and washed with H2SO4 (1% of product) and then

acidity is removed by soda ash. Material is then filtered and packed in

drums. SO2 gas is scrubbed in NaOH solution.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

n-Butanol 650

Liquid Bromine 750 Waste water 525

sulfur 250

Water 500


Soda Ash 135

n-Butyle Bromide 1000

Total 2785 2785

Reaction &

Distillation

Mass Balance of N-Butyle Bromide

Purification

Product


Sulphonation

1. Scheaffer Acid


In sulphonator take Sulphuric acid. Cool it to required temp. Add Beta

Naphthol. Heat it to elevated temp. Maintain for hours. Dump the mass in

water. Add activated carbon. Filter it.

Collect filtrate add soda ash or caustic lye and make neutral. Cool it and

filter it. Collect wet cake as finished product.

Mass Balance:

INPUT KG OUTPUT KG

H2SO4 1050

B Naphthol 950

Water 2250

Carbon 25

Waste Carbon 25

Water 1200

Caustic Lye / Soda 850

Salt 115

Wastewater 3370

Wastewater 1565

Drying loss 480

Scheffer Acid 1000

Total 6440 6440

Nutch Filter

Centrifuge

Wet Cake

Drying

Mass Balance of Scheffer Acid

Sulphonation

Dumping

Clarifier

Isolation


2. G Salt


In sulphonator take Sulphuric acid. Cool it to required temp. Add Beta

Naphthol and stir slowly add Oleum 23% with controlling of temp. Heat it

to elevated temp. Maintain for Hrs. Dump the mass in ice water. Add KCl

salt and heat to boil. Cool it. Filter it. Collect wet cake as finished product

and filtrate for recovery of G-salt.

Chemical Reaction:

Mass Balance:

Input KG Output KG

H2SO4 (98%) 1250

B Naphthol 1050

Oleum (23%) 1000

KCl Salt 1200

Water 2500

Spent Acid (40-45%) 5465

Drying Loss 535

G Salt 1000

Total 7000 7000

Mass Balance of G Salt

Sulphonation

Dumping

Filteration &

Centrifugation

Drying


3. Alpha Napthanol


Take ANA in GLR or Lead line vessel melt it. Add Sulphuric Acid and slowly

add water, heat it at elevated temperature. Maintain temp for several

hours. Cool it and Filter it in nutch as finished Crude alpha Naphthol.

Make vaccum distillation to get pure Alpha Naphthol.

Chemical Reaction:

Mass Balance:

Input KG Output KG

ANA 1050

Sulphuric acid 800

Water 2000

Spent Acid (40-45%) 2900

Water 1200

Waste Water 1150

Alpha Naphthol 1000

Total 5050 5050

Product

Mass balance of Alpha Naphthol

GLR or Lead Line

Filter

Crude Alpha

Naphthol

SS Reactor

Filter


4. ONTSA


In sulphonation reactor O.N.T. and Oleum is taken, under no pressure

after stirring of these materials. Then salt and water is added to isolate

the reaction mass. Then it is taken in notch for filtration of the above

materials.

Mass Balance:

Input KG Output KG

ONT 1000

Oleum 30% 2050

Salt 1200

Water 2200

Spent Sulphuric Acid (45-50%) 4350


Drying loss 350

ONTSA 1000

Total 6450 6450

Mass balance of ONTSA

Dryibng

+Packing

Sulphonation

Isolation

Nutch Filltration

Centrifuge


5. EBAMSA


Sulphonation of sulphuric acid is carried out in presence of EBA and

Oleum and drawning of sulpho mass is carried out with water, Filtration,

Centrifuge and drying process will gives EBAMSA.

Chemical Reaction:

Mass Balance:

Input KG Output KG

EBA 850 SO2 gas 25

Oleum 850

Sulphuric Acid 850

Water 2500

Spent Sulphuric Acid

(40-45%)3545

Drying loss 480

EBAMSA 1000

Total 5050 5050

Drying

Mass balance of EBAMSA

Sulphonation

Drowning

Filtration

Centrifuge


6. Aniline 2:5 DSA


Metalinic acid is sulphonated with sulphuric acid & Oleum(65%). Then

mass is dump in water give tri sulphonic acid is hydrolyzed to get aniline

2:5 DSA. It is isolated with salt & filter & wash & C.F.

Chemical Reaction:

+

+

H2SO4

H2S2O7

+ H2O + SO3

+H2O+ H2SO4

Metanil ic AcidAniline 2, 4, 5-Trisulphonic Acid

Water Sulphur Trioxide

Aniline 2, 4, 5-Trisulphonic Acid

Aniline 2, 5-Disulphonic Acid

Sulphuric Acid

NH2

HO3S

SO3H

SO3H

NH2

HO3S

SO3H

SO3H

NH2

HO3S

SO3H

NH2

HO3S

Mass Balance:

Input KG Output KG

Metanilic Acid 1000

Sulfuric Acid (98%) 1200 SO2 Gas 65

Oleum 65% 1150

Hyflow 15

Activated Carbon 55 Spent Acid (40-45 %) 4245

Steam 750

Water 1800

Water 1400 Solid waste 280

Sodium Sulphate 900

Steam 650

Waste Water 2650

1680

Total 8920 8920

Wet Cake of

Aniline 2:5 DSA

Aniline 2:5 DSA (As is

real basis 1000 Kg)

Mass balance of Aniline 2, 5 DSA

Sulphonation

Hydrolysis

Clarification

Isolation

Filtration &

Centrifuge


7. PNTOSA


Sulphonation

In closed vessel P.N.T. and Oleum 23% with water is taken, under no

pressure after stirring of these materials, it is transferred in open vessel

called dumping. Then it is taken in notch for filtration of the above

materials. The material now called P.N.T.O.S.A. output of spent acid

comes out during this process.

Chemical Reaction:

Mass Balance:

Input KG Output KG

PNT 1150

Oleum 30% 1800

Wash Water 1200

Spent Acid (50-55 %) 2630

Drying loss 520

PNTOSA 1000

Total 4150 4150

Mass balance of PNTOSA

Sulphonation of

PNT

Drowing of

sulphonated

Filltration

Drying


8. MPDDSA


Sulphonation: Take sulphuric acid in M.S. vessel & charge MPD (meta

phenylene Diamine) within 6 hours below 900C temperature, then charge

oleum 65% within 4 hours below 1000C Then raise temperature to 1300C

& maintain up to Sulphonation completion approximately 8 hours.

Isolation: Charge water in brick wise vessel & charge sulpho mass within

2 hours & maintain temperature upto 700C and then reduce to room

temperature, stir for 8 hours then filter it in filter-press then centrifuge.

Spray Drying: The final product will be transferred to the spray drying

holding tank and spray dried.

Chemical Reaction:

+

NH

Oleum

NH

SO3HNH NH

SO3H

M.W : 268 g/molM.W : 118 g/mol

MPDDSA

H2SO4

MPD

Mass Balance:

INPUT KG OUTPUT KG

MPD 650

Sulphuric Acid 1050

Oleum (65%) 1200

Water 4200

Spent Acid (30-35 %) 4705

Spent Acid (30-35 %) 870

Drying loss 525

MPDDSA 1000

Total 7100 7100

Dyring

Mass Balance of MPDDSA

Sulphonation

Isolation

Filtration

Centrifuge


1. PCOSA


In a sulphonator charge sulphuric acid and add PCD. Cool the mass and

solely charge Oleum 23 % at elevated temp. Stir for a hr. and heat to

required temp. Dump the mass in ice water. Free Stir and filter the mass.

Collect wet cake as finished product.

Chemical Reaction:

Mass Balance:

Input KG Output KG

Para Cresidine 750

H2SO4 850

Oleum 23% 1800

Salt 400

Ice 1000

Water 1200



Drying loss 540

PCOSA 1000

Total 6000 6000

Drying

Mass balance of PCOSA

Sulphonation

Drowning

Nutch Filtration

Centrifuge


2. Sulpho C Acid


C Acid is reacted with 98% Sulphuric acid and 65% Oleum. Then reacted

mass is filtered in filter press. Inorganic salt is removed out from the filter

press.

Clear liquid is isolated in isolator and add salt. Then again filtered it and

ML goes to dryer for drying purpose and then blended it and get the final

product.

Chemical Reaction:

SO3H

SO3HSO3H

SO3H

SO3H

NH298% H2SO4

NH2

Mass Balance:

INPUT KG OUTPUT KG

C-Acid 1110

Oleum(65%) 1335

Sulphuric Acid 1350

Water 2075

Glober salt 875

Spent Acid (50-55%) 4345

Spent Acid (50-55%) 950

Sulpho C Acid, 1000

Real Basis 1450

Total 6745 6745

Packing

Mass Balance of Sulpho C Acid

Sulphonation

Dumping

Clarification

Filter press

Centriguge


Other Products: 1. Sodium Naphthionate


Alpha naphthyl Amine is Sulphonated with Sulphuric Acid in ODCB at

higher temp convert Naphthionic acid. Distill ODCB with water as

azeotropic mixtures, followed by neutralization with sodium Carbonate

(Soda Ash). Collect 1st cut ODCB from bottom and sent for Acid

treatment(AT). Filter the mass. Collect in isolation vessel and Cool the

mass. Filter it in Nutch and CF it gives cold water wash to get Sodium

Naphthionate. Collect filtrate take in Naphthionate isolation vessel add

dil. Sulphuric acid. Filter the mass and collect W/C as NA. Charge

collected NA in a vessel.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

ODCB 2500 ODCB + Water 1440

H2SO4 850

ODCB 1230

Soda ash 425

water 2200


Drying Loss 465

Sodium Naphthionate 1000

Total 6475 6475

Drying loss

Mass Balance of Sodium Naphthionate

Sulphonation

Distillation

Isolation

Filter/CF

Neutralization


2. N W Acid


Sodium Naphthionate is condensed with Sodium Bisulphite at reflux

temp for 48 hrs. Followed by Hydrolysis with Sulphuric acid to remove

SO2. SO2 is scrubbed in soda ash solution and reuse for further batch.

Hydrolyzed mass is neutralize and alkaline with Sodium Hydroxide

(Caustic Lye) boil for removal of Ammonia. Cool it and remove isolated

salt. Than isolate N. W. acid with dil. sulphuric acid/Hydrochloric acid.

Filter it. Collect W/C and then dry the mass as N. W. Acid.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Sodium Naphthionate 1400

Sodium Bisulphite 1800

Water Recycle 1800

H2SO4 (38%) 2000 SO2 gas 480

Sodium

Naphthionate

Reuse

70

Caustic Lye 850 NH3 gas 65

Water Recycle 1000

Condensate Water

reuse2800

Process Sludge 55

Hydrochloric Acid 950

Waste Water 4835

Drying loss 495

N W Acid 1000

Total 9800 9800

Expel of NH3

Mass Balance of N W Acid (Neville Winther’s Acid)-1-Naphthol-4-sulfonic acid

SS vessel

Hydrolysis

Separation SN

Concentration

Filter

Isolation

Filter/CF

Drying


3. 4 CAP


2, 5 Dichloro Nitro Benzene, Caustic soda flakes & Water is charged in

the reactor. Reaction mass is charged along with Soda ash, Iron

powder, HCl, Sodium Bicarbonate & Water in vessel after filtrate the

reaction mass. HCl is added to reduce the pH of mass up to 2.5. Lime

and caustic soda is added for the neutralization the mass. Iron sludge

is separated from slurry during filtration. Isolation, Centrifuging and

Drying steps are carried out to get the product.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

2:5 DCNB 1200

Caustic 500

Water 1800

Iron powder 135

HCl 125 Iron Sludge 345

Waste Water 1900

Drying Loss 515

4 CAP 1000

Total 3760 3760

Drying & Packing

Mass balance of 4-Chloro 2-Amino Phenol (4 CAP)

Hydrolysis

Reduction &

Clarification

Nutch Filter &

Centrifuge


4. 3,5 DABA


Benzoic Acid Nitro mass prepared by the Nitration of it with the help of

Nitric Acid and Sulphuric Acid once the reaction gets over. The Nitro

mass recovered and it will get reduce with cast iron powder when the

reaction is over, material clarified and isolated it with Hydrochloric Acid

to get final product.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Benzoic Acid 85

Sulphuric Acid 98% 1500

Nitric Acid 98% 1000


Ice 1200

Iron 1150

HCl 350 Iron Sludge 1850

Caustic Lye (47-48%) 450

Water 1200

HCl (30%) 1800

Waste Water 3600

Drying Loss 465

3,5 DABA 1000

Total 10235 10235

Drying &

packing

Mass Balance of 3,5 DABA

Nitration

Dumping &

Filteration

Reduction &

Filtration

Isolation

Filteration &

Centrifugation


5. 2 Pyridone


In the reactor mono ethyl amine and Methyl Cyano Acetate is added

for condensation. Then mass is further condensate by Methyl Aceto

Acetate Ester. Mass is sent for hydrolysis where it is hydrolyzed by

Sulphuric acid. Then filter is sent into washing and filtration. Waste

water is sent into ETP. And then product is charged into dryer.

Mass Balance:

INPUT KG OUTPUT KG

Mono Ethyl Amine 500

Methyl Cyno Acetate 625

Methyl Aceto Acetate Ester 750

H2SO4 3200

Spent Acid(60-65%) 3380


Drying Loss 485

2 pyridone 1000

Total 5925 5925

Drying & Packing

Mass balance of 2 Pyridone

Condensation

Condensation

Hydrolysis

Filteration

Centrifuge


6. PAABSA


Sodium bisulphite along with Formaldehyde is charged into reaction

vessel and then salt is added. Then the reaction mass is goes into

filtration and centrifugation, Waste water is sent into ETP. In another

PP Vessel Sulphonic acid and 30% HCl is reacted in presence of sodium

nitrite and maintain temperature 0-50C. Then sodium bicarbonate is

added for coupling. Salt is added for isolation followed by filtration and

centrifugation. Then add sulphonic acid along with water in reaction

mass. After that again filtration and centrifugation is carried out. Then

product is sent into spray dryer.

Mass Balance:

INPUT KG OUTPUT KG

Sodium bisulphite 620

37% Formaldehyde 550

Aniline oil 500

Salt 650

Steam 700

Wastewater 1200

Sulphonic Acid 850

30% HCl 620

Sodium nitrite 350

Ice 800

Sodium bicarbonate 650

Ice 1200

Salt 1000

Wastewater 4150

98% Sulphonic acid 1000

Water 1800

Wastewater 4465

Drying Loss 475

PAABSA 1000

Total 11290 11290

Completion

vessel/Coupling

Mass Balance of PAABSA

Reaction vessel

Filtration &

Centrifugation

P.P. vessel

Isolation

Filtration &

Centrifugation

Reaction vessel

Filtration &

Centrifugation

Drying & Packing


7. 5 NAP


OAP along with water is charged into M.S. jacketed reactor-I and

Heated up to 800C. And Acetic Anhydride is added into vessel. The

nitric acid is added. And further hydrolyzed by hydrogen gas. Then the

wet product is goes into nutch filter and waste water is sent into ETP.

And product is sent into spray dryer.

Mass Balance:

INPUT KG OUTPUT KG

OAP 800

Acetic Anhydride 750

Water 1200

HNO3 750

H2SO4 1000

Caustic Soda 120 Acetic Acid 1250

Waste Water 1880

Drying Loss 490

5 NAP 1000

Total 4620 4620

Drying & Packing

Mass balance of 5 NAP

Acetylation

Nitration

Hydrolysis

Nutch Filter


8. 4 Sulpho Anthranilic Acid


Ortho Nitro Toluene (ONT) is sulphonated using 98% Sulphuric acid and

65% Oleum at 55-60oC. It is hydrolyzed at 105-110oC using catalyst at

pH 12. When hydrolysis is over adjust pH 6.5 - 7 by 70% Sulphuric acid.

Clarify through process. Collect mother liquor with washing. Isolate

product by adjusting pH 1 to 1.5 by 70% Sulphuric acid. Separate out

product by filtration & centrifuging.

Chemical Reaction:

CH3

NO2

+ H2SO4 +H2SO4.SO3

Ortho Nitro Toluene

Hydrolysis

COOH

NH2

SO3H

CH3

NO2

SO3H

4-Sulpho Anthranilic Acid

Sulphonation

-2SO3

-2H2OOleumSulphuric Acid

Mass Balance:

INPUT KG OUTPUT KG

ONT 1000

65% Oleum 1050

98% Sulphuric Acid 900

Water 2200 3850

Caustic Soda flakes 1000

Steam 500

Sulphuric Acid 3850

Wastewater 5160

Drying loss 490

4 Sulpho Anthranilic Acid 1000

Total 10500 10500

Filtration

Drying & Packing

Mass Balance of 4 Sulpho Anthranilic Acid

Sulphonation

Dumping vessel

Hydrolysis

Isolation

Spent Sulphuric Acid

(40-45%)


9. 2:5 Di Chloro Para Nitro Aniline (2:5 DCPNA)


Acetyation reaction take place between 2,5 DCA and Acetic anhydride.

Then nitration reaction take place in presence of H2SO4 and HNO3.

Isolate product by adjusting pH. Separate out product by filtration.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

2-5 DCA 750

Acetic Anhydride 650

H2SO4 850

HNO3 650

Water 1500

Waste Water 3400

2,5 DCPNA 1000

Total 4400 4400

Finish Goods

Mass balance of 2:5 DCPNA(2:5 Di Chloro Para Nitro Aniline)

Acetylation

Nitration

Isolation

Filtration


10. Metanilic Acid


In a reducer MSLR take resist salt solution. Heat to 80oC. Charge iron

powder & slowly charge HCl in lots to control foaming & spot will be

colorless on spot paper. Stir for 2-3 hours at 95-100oC.

Finally adjust pH 7.5 to 8 by using soda ash. Stir for 0.5 hour. Clarify

through press and give hot water wash. Finally adjust pH 1.5 by 98%

Sulphuric Acid. Cool to 25-30oC by cooling filter, suck well, centrifuge &

finally dry the product.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Nitro benzene 850

Oleum (25%) 1500

Calcium hydroxide 1200

Water 2200

Gypsum 2400

HCl (30%) 450

Iron Powder 900

Soda Ash 500

Iron Sludge 1695

H2SO4 (98%) 800

Waste water 2890

Drying loss 415

Metanilic Acid 1000

Total 8400 8400

Filtration &

Centrifuge

Drying

Mass Balance of METANILIC ACID

Reactor 1

Filtration

Reactor 2

Filter Press

Isolation


11. 4 NAPSA


p-Nitro Chlorobenzene is Sulphonated with Oleum (23%) & Sulphuric acid

followed by nitration with Nitric acid to get 2-chloro-3,5-dinitro benzene

sulphonic acid. The above product is hydrolyzed in alkaline medium &

partially reduced by adding NaHS to get 4-NAPSA (Na salt). Filter it and

C/F. Dissolve the 4-NAPSA (Na salt) in Sulphuric Acid and clarify through

filter press & isolated by Sulphuric acid, filter and centrifuge to get pure

4-NAPSA.

Chemical Reaction:

Mass Balance:

Input KG Output KG

Lime 250

NaSH 600

Water 1000

4 Nitro Chloro Benzene 800

Oleum 850

HNO3 320

H2SO4 650

Calcium Thio Sulphide 835

Waste Water 2150

Drying Loss 485

4 NAPSA 1000

Total 4470 4470

Drying & Packing

Mass balance of 4 NAPSA

Calcium

Polysulfide

Sulphonation

Nitration

Reduction &

Clarification

Nutch Filter


12. 6 NAPSA


Sulphonation: Take 98% H2SO4 then charge 23% Oleum and start chilling

get temperature 20 to 30°C check TLC with OAP and OAPSA and check

Acidity (Range 79 to 82). If TLC is not OK then 2 hrs maintain temperature

100 to 105°C. Transfer in nitration vessel.

Nitration: Collect Sulpho mass and start chilling get temperature 15 to

20°C and 6 hrs. Then start WNA 68% with addition between temperatures

15 to 20°C 650 kg in 36 hrs. Maintain with free string 2 hrs then check

AR/BR (0.3% to 0.55% different). If AR/BR different more than 0.55%

charge WNA and again check AR/BR different. Transfer in dumping vessel.

Dumping: Charge Ice approximately 4500 kg in 2 hrs. Then charge Nitro

mass slurry. Slowly addition with temperature 5 to 10°C. Maintain with free

string 2 hrs. Check filter loss (1.5% to 2.5%).After testing start press

filter/nutch filter. Suck the M/L start centrifuge. Start crushing and packing.

Mass Balance:

INPUT KG OUTPUT KG

OAP 520

Oleum (23%) 1000

HNO3 320

H2SO4 650

Ice 1200

Spent Sulphuric

Acid (50-55%) 1800

Spent Sulphuric

Acid (50-55%) 450

Drying Loss 440

6 NAPSA 1000

Total 3690 3690

Drying & Packing

Mass balance of 6 NAPSA

Sulphonation

Nitration

Isolation

Centrifuge

Filtration


13. MAP


Charge in vessel caustic lye/flakes, Metanilic acid Powder/Liquid and heat

up to 2500C to 2600C under string and after complete reaction, charge

water and make slurry of reaction mass and transfer to isolation vessel.

Take slurry in isolation vessel and isolate material with Ice and slowly add

Hydrochloric acid in it to isolate material, after complete isolation do

centrifuge and then transfer for Drying. Take Centrifuge wet cake for

Drying and pack Meta Amino Phenol. Generated waste water from

centrifuge will transfer to ETP for treatment.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Metanilic Acid 1600

NaOH 800

Catalyst 8

Water 3200

Catalyst 8

Waste water 4110

Drying loss 490

Meta amino phenol 1000

Total 5608 5608

Mass Balance of MAP (Meta Amino Phenol)

Fusion Reaction

Clarification

Precicpitation &

Filteration

Drying &

Packing


14. 4 Sulpho Hydrozone


Take water in an MSLR vessel. Charge 4 Sulpho Anthranilic Acid, stir for

half an hour. Charge ice, 98% Sulphuric Acid. Now add Sodium Nitrite

solution in 1 to 2 hrs. Charge Sodium bisulphite powder & Caustic soda

lye to adjust pH 6.5 to 7. Stir for 1 hr. Now receive about diazo solution in

1 hr keeping pH 6.5 to 7 if required, add caustic soda lye. Stir for 3 hrs.

Now produce for benzoylation. Heat to 55oC. Charge Benzaldehyde and

70% Sulphuric acid. Heat to 85oC & stir for 3 hrs. Scrub SO2 gas by

scrubber. Cool to 45oC. Filter to notch suck well & centrifuge.

Chemical Reaction:

COOH

NH2

SO3H

COOH

SO3H

NH-NH2

COOH

SO3H

N=N

+ Benzaldehyde

4-Sulpho Anthranilic Acid 4-Sulpho Hydrozene4-Sulpho Hydregene

++

H2SO4

NaNO2

H

Mass Balance:

Input KG Output KG

4 Sulpho Anthranilic Acid 1200

HCl (30%) 1050

Sodium Nitrite 350

Ice 1200

Sodium bisulphite 900

Caustic Soda 550

Benzaldehyde 650 SO2 Gas 325

HCl (30%) 1100 CO2 Gas 245

Ice 1450

Wash Water 700 Waste Water 7085

Drying Loss 495

4 Sulpho Hydrozene 1000

Total 9150 9150

Drying & Packing

Mass balance of 4 Sulpho hydrazone

Diazotization

Coupling

Benzolation

Filtration &

Centrifuge


15. DABA


Benzoic Acid is mix by 98% Sulphuric Acid. And Nitrated with

Concentrated Nitric Acid (98%) And Dump this sulfo mass in Ice & water.

Then filter it and centrifuge it. Then final product is reducing with Cast

iron powder and Hydrochloric Acid. Then take pH 9.2 by soda. Then filter

it and isolate it. Final product is packing as 2,5 Di amino Benzoic Acid.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Benzoic Acid 1350

Nitric Acid (98%) 1250

H2SO4 (98%) 3500

Ice 1200

Wash Water 1200 Spent acid (40-45%) 4540

Spent acid (40-45%) 750

Cast Iron Powder 2280 Iron Sludge 3450

HCl(30-35%) 1750 CO2 gas 260

Soda Ash 270

H2SO4 (98%) 270

Wash Water 1000 Waste water 2280

Waste water 1280

Drying loss 510

DABA 1000

Total 14070 14070

Isolation

Nutch

Centrifuge

Mass Balance of DABA (2,5 Diamino Benzoic acid)

Nitration

Drownings

Nutch

Centrifuge

Reduction


16. Mix Cleave Acid / 1 -6 Cleave Acid/ 1-7 Cleave Acid


In this process sulphuric acid will be mixed with Naphthalene and added

in to sulphonator.

The sulpho mass will be nitrated with nitric acid. This will be an

exothermic reaction. It is necessary to keep the temperature maintain

using chilling water in to the jacket. At the end of the reaction prepared

Nitro mass will be neutralized.

Reduction of nitro solution will be done using iron powder, HCl and Soda

Ash. Iron powder will be added during the reaction. Gradually nitro

solution will be added into the reduction vessel. During the reaction Iron

sludge will be generate.

Mass isolated with HCL and caustic flask. The final mass is filtered in a

filter nutch and goes to centrifuged after wet cake is dried by centrifuging

to get the product.

Chemical Reaction:

SO3H

NH2

+ H2SO4 + + HNO36Hcl + +4H2O 3Cl2

Mass Balance:

INPUT KG OUTPUT KG

Nepthaline 950

Sulphuric Acid 1150

Nitric acid (68%) 650

Sulphuric Acid 1050

Lime stone Powder 1450 Gypsum sludge 3750

Soda 450

Water 2200

HCl 185

Acetic Acid 85 Iron sludge 1670

Iron Powder 750

Sulphuric Acid (40%) 800

Waste Water 2835

Drying loss 465

Mix clave acid 1000

Total 9720 9720

filter/Nutch

C.F./Drying/

packing

Mass Balance of Mix Clave Acid (1,6 Cleves Acid & 1,7 Cleves Acid)

Sulphonation

Nitration

Neutralizer

Reduction

Isolation


17. Phenyl Peri Acid


Take aniline in reactor and start stir 40 rpm. After charging peri acid in

reactor and start stir 20 to 40 rpm for 3 to 4 hrs and heat it to 1650C

in 4 hrs. After maintain temperature 163 to 1650C keep it under free

stirring for 24 hrs. After cool to 105 to 1060C in 3 to 4 hrs. Mass is

charging to simple distillation.

Simple Distillation:

Mass is under vacuum 25-30 mm and record the consistency of the

mass. So, separate the phenyl peri acid and aniline. Distillation time to

7 to 8 hrs and cool 95-1000C. The aniline is recycle in next batch.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Peri Acid 900

Aniline oil 750

Hyflow 20

Carbon 10

Water 950

Carbon /Hyflow waste 45

HCl 180

Waste Water 1240

Drying Loss 525

Phenyl Peri Acid 1000

Total 2810 2810

Wet cake of

Phenyl Peri Acid:

1525 Kgs

Drying

Mass Balance of Phenyl Peri Acid (PPA)

Condensation

Drawning

filteration

Isolation

Centrifuge


18. C Acid


In this process sulphuric acid will be mixed with Naphthalene and oleum,

then added in to Sulphonation reactor.

The sulpho mass will be nitrated with nitric acid. This will be an

exothermic reaction. It is necessary to keep the temperature maintain

using chilling water in to the jacket. At the end of the reaction prepared

Nitro mass will be neutralized.

Reduction of nitro solution will be done using iron powder, HCl and Water.

Iron powder will be added during the reaction. Gradually nitro solution will

be added into the reduction vessel. During the reaction Iron sludge will be

generate.

Mass isolated with sulphuric acid. The final mass is filtered in a filter nutch

and goes to centrifuged after wet cake is dried by centrifuging to get the

product.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Naphthalene 1250 SO2 gas 45

Sulphuric Acid(98%) 1200

Oleum 65% 1450

Nitric Acid 325 NOx Gas 15

Water 2200

Mgo 350

Spent Acid (50-55%) 4170

Water 2200

HCl 55

Iron 450

Iron Sludge 1750

Sulphuric Acid 250

Waste Water 2750

C Acid (1000 Kg Real) 1000

Total 9730 9730

Centrifuge

Mass Balance of 2- Naphthylamine 4,8 di Sulfonic acid

Sulfonation

Nitration

Drowning

Filter

Reduction

Filtration

Isolation

Filtration

Centrifuge


19. 4 ADAPSA


In auto clave reaction, take water & NaOH. Charge PNCBOSA & mix

properly & raise temp. 100°C. Then charge aniline oil & raise temp.

145°C & maintain for 12 hrs. Cool mixture up to 125°C. Then stir

reaction mass up to 2 hrs & further cool to100°C. Then charge NASH &

stir for 8 hrs. After add S.B.S. at 65°C. & maintain for 3 hrs. Then add

HCl (30%) & filter whole mass in notch filter/centrifuge & dry.

Chemical Reaction:

Mass Balance:

Input KG Output KG

PNCBOSA 1000

ANILINE OIL 350

WATER 2000

NASH 1400

NAHSO3 1200

Waste Water 6260

HCl 1800

Drying Loss 490

4-ADAPSA 1000

Total 7750 7750

Mass balance of 4-ADAPSA

Condensation

Reduction

Isolation,

Filtration &

Centrifuge

Drying & Packing


20. K Acid


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

G-Salt 710

Ammonia (25%) 700 Ammonia 220

SBS 125

Sulphuric Acid (98%) 1000 SO2 Gas 210

Water 1200

Hot Washing Water 1670 Waste water 5040

Drying loss 620


Oleum Acid (65%) 2200

Water 1100

KCl 350


Wash water 800

K-Acid (Real 1000 Kg) 1400

Total 10605 10605

Amidation

Mass Balance of K-ACID

Drawning

Filtration Centrifuge

2-Napthalamine 3,6,8

Trisulphonic Acid

Isolation

Filtration & Centrifuge

Drying

Amido G-Acid

Sulphonation


21. 3:5 DNBA


In reaction vessel, charge benzoic Acid, H2SO4 and Oleum. Then in

presence of nitric acid, nitration reaction take place. At the end of the

reaction prepared Nitro mass will be neutralized. Then the reaction mass

pass under drowning and Spent sulfuric acid is generated and remaining

mass goes to centrifuged after wet cake is dried by centrifuging to get the

product.

Chemical Reaction:

Mass Balance:

Input KG Output KG

Benzoic Acid 550

H2SO4 2500 Nitrous Oxide 45

2HNO3 900

Oleum 1200

Spent sulphuric Acid (60-65%) 3255

Spent sulphuric Acid (60-65%) 850

3,5 DNBA 1000

Total 5150 5150

Mass balance of 3,5 DNBA (3, 5 Di Nitro Benzoic Acid)

Nitration

Drowning

Centrifuge

Finish Products


1. OPSAMIDE


Charge chloro sulfonic acid and ONCB in chloro sulphonation vessel.

Transfer it into dumping vessel & cool it. Then amination reaction takes

place by addition of ammonia solution along with HCl 30%. Then filter

and centrifuge the same and finally dry it.

Mass Balance:

INPUT KG OUTPUT KG

Chloro Sulphonic Acid 3000

ONBC 1200

Ice 1800

Spent Acid (40%) 4550

Ammonia/Mono

methyl Amine/

Anthranilic Acid

450

HCl 30% 125

Steam 1100

Ice 1200

Water 1800

Waste Water 3710

Castic Lye 950

Water 1600

HCl 250

NAHS Sollution(30%) 550

Castic Lye 125

HCl 380 Waste Water 4780

Drying loss 490

Opsamide / Mithyl

Opsamide / Anthranilic

Opsamide

1000

Total 14530 14530

Amination

Mass Balance of Opsamide / Mithyl Opsamide / Anthranilic Opsamide

Chloro

sulphonation

Dumping

Filteration

Filteration &

Centrifugation

Hydrolysis

Reduction

Isolation

Drying &

Packing


2. Peri Acid / Laurent Acid


Sulphonation: Naphthelene is charged in Sulphonation reactor in

presence of sulphuric acid to complete the sulphonaion reaction.

Nitration: This sulphonation mass is to be nitrated with Nitric acid and

then the mass is neutralized with lime stone and magnesium oxide.

Reduction: The filtered mass is further reduced by iron and HCL.

Hence iron sludge is generated after filtration.

Isolation: the reaction mass is then isolated with HCl followed by

filtration and peri acid is generated.

Isolation, filtration and Centrifugation: The remaining mass along

with HCl will isolate, centrifuge, Crushing and Packing done. Hence

Laurent acid will be generated.

Chemical Reaction:

SO3HNH2

+ H2SO4 + + HNO36Hcl + +4H2O 3Cl2


Mass Balance:

INPUT KG OUTPUT KG

Naphthalene 850


Nitric Acid 450

Lime Stone 1800

Magnesium oxide 450

Water 3500

Gypsum Sludge 3560

HCl 80

Iron Powder 850

Iron sludge 2420

HCl 140

Drying loss 345

Peri Acid 700

HCl 130

Waste Water 2450

Drying loss 275

Laurent acid 300

Total 10050 10050

Filtration

Isolation

Filtration

Isolation

Filtration &

Centrifuging

Drying

Reduction

Mass Balance of Peri Acid & Laurentˈs Acid

Sulfonation

Nitration

Neutralization

Filteration


3. Broner Acid


In Sulphonation reaction vessel, charge beta napthole and H2SO4.

Then clarify the reaction mass by adding water and carbon. The mass

is isolated by glauber’s salt followed by filtration by using HCl. Then

amidation take place in presence of ammonia , scheaffers acid and

SBS. Then isolate the mass and final product is recovered after drying.

Mass Balance:

Input KG Output KG

Beta Napthole 1500

H2SO4 1450

Carbon 10

Water 2500

Glauber's Salt 1000


Ammonia 28% 2200

Schaffers acid 1500

SBS 350

Waste Water 5265

Drying loss 485

Broner Acid 1000

Total 13010 13010

Mass balance of Broner Acid

Sulphonation

Clarification

Isolation

CF/Drying &

Packing

Nutch Filteration

Amidation

Isolation &

Filteration


4. 1,8 Dihydroxy 3,6 Disulfo Nepthelene (Cromotropic Acid)


Hydrolysis of H-Acid in presence of NaOH, salt and water. Then isolate

the reaction mass in presence of H2SO4 followed by filtration, waste

water is generated afire filtration and wet cake is dried and product is

recovered.

Mass Balance:

INPUT KG OUTPUT KG

H- Acid 1450

NaOH 950

Salt 25

Water 2200

H2SO4 750

Waste water 3995

1380

Total 5375 5375

Mass Balance of Chromotropic Acid (1,8 Dihydroxy 3,6 Disulfo Nepthelene)

Hydrolysis

Isolation

Filtration

Finished ProductCromotropic Acid,

1000 Kg Real


5. PPD (Para Phenylene Di Amine)


Reduction of HCl in presence of PNA, Iron and Water, Filtration of

reduction mass and distillation of filtration mass gives Para Phenylene

Di amine.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

PNA 1650

Caustic Flakes 350

Sulphur 250

NaSH 800

Water 1000

Waste Water 2965

Residue 85

PPD 1000

TOTAL 4050 4050

MASS BALANCE OF PPD

Reactor

Filtration &

Centrifugation

Distillation


6. Violet Acid


Sulphonation: Take Sulfuric acid in to a reactor add into it

proportionate quantity of Naphthalene slowly so as to maintain

temperature 30˚C. Oleum is added slowly and temperature is to be

raised to 80˚C slowly maintain for sulphonation to be completed.

Drowning: This sulfonated mass is to be neutralized with lime stone

and filtered.

Fusion: The filtered mass is further concentrated and then fusioned

with Caustic Soda at higher temperature.

Isolation: Dump the mass into water and product will come out on

cooling filter, centrifuge, crushing and packing.

Chemical Reaction:


Mass Balance:

INPUT KG OUTPUT KG

Naphthalene 800 SO2 gas 45


Oleum(65%) 2000

Water 2200

Lime Stone 2000

Sodium Sulphate 1250

Gypsum 4450

Drying loss 2650

Caustic Flaks 1200


HCl 550

Violet Acid 1000

Total 13000 13000

Drowning

Centrifuge

Mass Balance of Violet Acid (1 Naphthol 3,6 di sulfonic Acid)

Sulfonation

Drowning

Filtration

Evaporation

Fusion


7. Koch Acid


Sulphonation of sulphuric acid is carried out in presence of

naphthalene and oleum. Nitration and neautralization process by using

nitro mass in presence of lime stone and soda ash.

Nitro Liquor is reacted in presence of iron powder by using reduction,

then isolation, Filtration and Centrifuge gives KOCH acid.

Mass Balance:

INPUT KG OUTPUT KG

Napthalene 350 SO2 gas 15


Oleum 500

Nitric Acid 270 Nox 10

Lime Stone 1500

Soda Ash 170

Water 1800

Water Wash(Recycled) 1000 Gypsum 3000

Waste water 1000

Iron Powder 300 Iron Sludge 540

HCl 35 Waste water 700

Water Wash(Recycled) 670

Sulphuric Acid 225

Waste Water 925

KOCH Acid 1000

Total 7190 7190

Isolation

Filtration

Centrifuge

Mass Balance of 1 Nyphthyl amine 3,6,8 tri sulfonic Acid

Sulfonation

Nitration

Neutralization

Filtration

Reduction


1. 1 Napthol 8 Sulphonic Acid


Diazolation of sulphuric acid is carried out in presence of peri acid,

NaNO2, Filtration Caustic lye is carried out in presence of diazo mass,

centrifuge and drying will gives 1- Naphthol 8- Sulfonic acid.

Chemical Reaction:

Mass Balance:

Input KG Output KG

Peri Acid 450

Sulphuric Acid 250

NaNo2 350

Water 750

Diazo mass 1500 Waste water 2170

Caustic lye 350

Drying Loss 480

1-Naphthol 8-sulfonic Acid 1000

Total 3650 3650

Mass balance of 1-Naphthol 8-Sulphonic Acid

Diazolation

Filltration

Centrifuge

Drying


2. DTPTSA (Dehydro Thio p- Toluidine Sulfonic Acid)


Para Toluidine, Para Toluidine Sulfonic Acid(PTSA) and Sulphur are

charged into a reactor and heated slowly up to 1100C. The mass is

slowly further heated gradually to 1600C in 8 hours time and

maintained for 20 hours. During this period, vapour- phase (which

contains entrained liquid-mist, and Hydrogen Sulfide Gas) is passed

through cooling condenser to cool the vapour phase and separate

liquid-mist (which is cooled and separated as liquid phase) and

Hydrogen Sulfide Gas (which remain in gaseous phase). The separated

liquid phase is refluxed back in to the reactor in- situ and Hydrogen

Sulfide gas is further taken to a mist separator to remove remaining

entrained liquid phase mist(which is cooled to solid form, and collected

in the separator and subsequently recycled as input in next reaction-

batch) and pure Hydrogen Sulfide is taken to a

collection/Storage vessel which is designed to 10 Kgs/Cm2 pressure.

The whole system is kept a closed system so that no fugitive emissions

are there. The reaction pressure is controlled by intermittent stoppage

of heating oil flow through the jacket and hence thare is no danger of

pressure increases in case of power failure or sudden stoppage of the

system. The mass is then heated further to 1650C slowly till completion

of reaction so that pressure of the reactor gets stabilized to 2 Kgs/Cm2.

This pressure is then very slowly released through an Absorption

Reactor (Containing Caustic Solution) to a two stage caustic scrubber

so that no gaseous emission is there. Small quantity of Air is passed

into reactor vapour phase, Which is subsequently passed through the

absorption system and scrubber system to flush out Hydrogen Sulphide

from the reactor.

The reaction mass is then charged to a distillation kettle and distillation

is carried out to recover the unreacted Para Toluidine and partially

converted intermediate molecules which is recycled as input in to the

next reaction batch.

The crude product mass is slowly added in a quench reactor


containing water, maintaining water temperature at around 800C,

under vigorous stirring. It is then centrifuged and washed with water

to obtain wet cake of the product Dehydro Thio Toluidine Sulfonic

Acid. It is then dried and packed or directly packed in bags as per

requirement.

Chemical Reaction:

Mass Balance:

INPUT KG OUTPUT KG

Para Toluidine 350

Sulphar 300

Para Toluene 700

Sulphonic Acid 250


Drying loss 485

DTPTSA 1000

Total 3800 3800

Drying

Mass Balance of DTPTSA (Dehydro Thio Para Toluidine Sulfonic Acid)

Reactor

Separation

Quenching

Reactor

Centrifuge


3. 2R Acid


In Autoclave take water charge K-Acid. Make uniform slurry. Charge

caustic Lye (Sodium Hydroxide).Heat to required elevated temp and

pressure. Cool the mass and dump in water. Add carbon and hyflow. Filter

it. Collect filtrate and add sulphuric acid for isolation. Cool the mass. Filter

it. Collect wet cake as finished product and dry it.

Chemical Reaction:

Mass Balance:

Input KG Output KG

K Acid 1500

NaOH 1550

Water 1200

H2SO4 1000 SO2 Gas 145

Water 3500

Waste water 5470

Waste water 1650

Drying Loss 485

2R Acid 1000

Total 8750 8750

Drying

Mass balance of 2R Acid

Fusion

Isolation

Filtration

Centrifuge


4. Epsilone Acid


Sulphonation of Sulphuric acid is carried out in presence of Napthalene

and Oleum. Nitric acid is reacted in presence of sulfo mass using

Nitration. Nitro mass is reacted in presence of lime stone and Mgo by

using neutralization, then filtration, reduction, Isolation, Centrifuge and

Diazotization gives EPSILONE acid.

Chemical Reaction:


Mass Balance:

INPUT KG OUTPUT KG

Oleum 65% 1000 SO2 gas 65


Napthalene 1800

Nitric Acid(98%) 850 Nox 15

Lime Stone 2500

Mgo 750

Water 1800

Water Wash 2200 Sludge 1580

Waste Water 3250

Iron Powder 1800 Iron Sludge 2250


Water Wash 1200

Sulphuric Acid 550 Waste Water 2565

Sodium nitrite 325

HCl 315

Waste Water 2940

Epsilone Acid 1000

Total 16515 16515

Reduction

Mass Balance of Epsilone Acid (1 Naphthol 3,8 di sulfonic Acid)

Sulfonation

Nitration

Neutralization

Filtration

Isolation

Centrifuge

Diazotization

Filtration

Centrifuge


5. Meta Di Nitro Benzene


The nitration reaction between nitro benzene and sulphuric acid in

presence of nitric acid. Then separate out the spent acid. The crude of

MDNB will be washed by water and finally neutralization in presence of

caustic lye.

Mass Balance:

Input KG Output KG

Nitro Benzene 780 10

Nitric Acid 460

Sulphuric acid 925

Water 170

Spent Acid(60-65%) 1280

Water 1150 Wash water 575

Caustic lye 50 Waste water 670

MDNB 1000

Total 3535 3535

Mass balance of Meta Di Nitro Benzene

Nitrator

Spent Acid

Seperation

Washing of

Crude MDNB

Neutralization

Traces of Nitrous

fumes


6. 4,4 Dinitro Stilbine 2,2 Disulfonic Acid (DNSDSA)


Oxidation reaction takes place between PNTSA, H2SO4, soda ash and

caustic lye. Then crystallization, filtration and centrifugation will take

place. And final product is dried in spray dryer.

Mass Balance:

INPUT KG OUTPUT KG

PNTSA 1750

Soda Ash 80

Caustic Lye 1200

H2SO4 800

Water 2200

Soda Ash 50

Waste water 4705

Drying Loss 375

DNSDSA 1000

Total 6080 6080

Drying

Mass Balance of DNSDSA (4,4 Dinitro Stilbine 2,2 Disulfonic Acid)

Concentration

Crystalization

Filtration &

Centrifuge

Oxidation


7. European K Acid


Sulphonation is carried out in presence of Napthalene and oleaum

nitric acid is reacted in presence of sulfo mass using nitration. Nitro

mass is reacted in presence of lime stone and MgO by using

neutralization, then filtration, reduction, centrifugation and drowning

gives European k Acid.

Mass Balance:

INPUT KG OUTPUT KG

Napthalene 750 SO2 gas 20

Oleum (65%) 1100

Nitric Acid 600 Nox 15

Lime Stone 1350

Soda Ash 300

Water 1500

Water 1500 Gypsum 3000

Waste water 1450

Iron Powder 650

HCl 75

Water 1100

Iron Sludge 1450

Waste water 1230

Caustic lye 450

Sulphuric Acid 150

Water 550

Waste Water 1910

European K Acid 1000

Total 10075 10075

Reduction

Mass Balance of European K Acid

Sulfonation

Nitration

Neutralization

Filter

Filtration

Fusion

Drowning

Filtration

Centrifuge


Annexure-III

Water Balance Diagram

Total Water Consumption

192 KLD (Fresh Water 62 KLD +Recycle 130 KLD)

Domestic

8.0

Process

74

Washing

20

Utilities

75

Greenbelt 15

Soak pit

6.5 Process

62.0

ETP

102 + 1.0 + 20.0 + 3.0 + 14.0 = 140

3.0

Boiler

25

Cooling

50

45

14 102

13 Ice

20.0

Scrubber

12.0

Total volume 168

Drying Loss

8 Steam

Water from

RM-85

SBS 10.0

1.0

RO 140.0

Reject 40

Permeate water 100.0

Acetic Acid 3.0

MEE

Spent HCl 1.0

6.0

48.0 Sale to actual user

Spent Sulfuric

Acid 54.0

Evaporation loss 8.8

Condensate Water 30.0

1.2 Salt

Spray

Dryer

10


Water Consumption and waste water generation

Sr.

No.

Source Water Consumption

Existing

(KL/day)

Waste Water

generation

(KL/day)

1. Domestic 8.0 6.5

2. Green Belt 15 00

3. Industrial

A Process 62 102

B Scrubber 12 1.0

C Washing 20 20

D Boiler 25 3.0

E Cooling 50 14

Total Industrial 169 140

Total (1 +2 + 3) 192 146.5

Less recycle 130 --

Actual fresh water

consumption

62 --


Annexure IV

Details of Hazardous/Solid waste

Sr.

No.

Type of

Solid Waste

Schedule Quantity Disposal method

1 ETP Sludge

+

Salt from

Spray Dryer

35.3 350

+

35

385

Collection, storage & disposal at

TSDF site approved by GPCB.

2 HCl (20-22%) 26.3 26 MT/Month Collection, Storage, Reuse with in

the process or sold to actual users.

3 Spent

Sulphuric acid

(H2SO4)

26.3 235

KL/month

Collection, Storage, Reuse with in

the process or sold to actual users.

4 Iron sludge 26.1 65

MT/month

Collection, Storage, Transportation,

sell to cement manufacturer or

disposed at TSDF site.

5 Gypsum

Sludge

26.1 500

MT/Month

Collection, Storage, disposal at

TSDF site or send to Cement

industries for co-processing.

6 Calcium Thio

Sulphite

-- 65

MT/month

Collection, Storage, Transportation,

sell to actual users under Haz.

Waste rule.

7 Acetic Acid 26.3 100

KL/month


the process or sold to actual users

under Haz. Waste rule.

8 Sodium

Bisulphite

26.3 260

MT/month


the process or sold to actual users

under Haz. Waste rule.

9 Used

Lubricating

Oil

5.1 0.5 Kl/year Collection, storage & use within

premises as lubricant/sell to

registered recycler.

10 Discarded

containers/

barrels/

liners

33.1 Barrels-

10000

nos./month

Liner-3.0

Mt/month

Collection, storage and reuse for

packing of products or disposal by

selling to approved recycler.


Annexure-V

Source of Air Emissions

Flue gas Stack-Proposed

Sr.

No.

Stack

attached to

Stack

Height

in m

Fuel

Used

Fuel

consumption

rate

APC

measure

Pollutant

1 Steam Boiler

(4 TPH)

30 Bio

Coal/

Coal

16 TPD Cyclone &

Bag Filter

PM

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