annexure-i list of · pdf fileannexure-i list of products sr. ... para hydroxy acetanilide...

Asiatic Pharma Chem 1

Annexure-I

List of Products

Sr.

No.

Name of Product Quantity

(MT/Month)

1. 2 mercaptobenzimidazole

150

2. 5 methoxy 2 mercaptobenzimidazole

3. 5 methyl 2 mercaptobenzimidazole

4. 5 difloromethoxy 2 mercaptobenzimidazole

5. 4 hydroxy 3 amino chlorobenzene

6. 4 hydroxy 3 chloro aniline

7. 4 hydroxy 3 amino benzene sulphonamide

8. 4 hydroxy 3 amino benzene methyl sulphonamide

9. 4 hydroxy 3 amino benzene 2 carboxy sulpho anilide

10. 3,5 dinitro benzoic acid

11. 4 amino 3 nitro anisole

12. 4 difloromethoxy 2 nitro aniline

13. 4 hydroxy 3 amino benzene sulpho anilide

Total 150

List of Raw Materials

Sr.

No.

Name of Raw material Quantity

(MT/Month)

Quantity

(MT/MT)

2 Mercaptobenzimidazole

1. Ortho nitro aniline 138 0.92

2. Sodium hydrogen sulphide solution (30%) 420 2.8

3. Sodium hydroxide 85 0.57

4. Carbon disulphide 95 0.63

5 Methoxy 2 Mercaptobenzimidazole

1. 4 methoxy 2 nitro aniline 139 0.93




5 Methyl 2 Mercaptobenzimidazole

1. 4 methyl 2 nitro aniline 138 0.92




5 Difloromethoxy 2 Mercaptobenzimidazole

1. 4 difluoro methoxy 2 nitro aniline 141 0.94




4 Hydroxy 3 Amino Chlorobenzene

1. 2,4 dichloro nitro benzene 201 1.34

2. Sodium bisulphite solution 336 2.24


3. Hydrochloric Acid 315 2.10


5. Sodium hydrogen sulphide solution 336 2.24

4 Hydroxy 3 Chloro aniline

1. 3,4 dichloro nitro benzene 201 1.34





4 Hydroxy 3 Amino benzene sulphonamide

1. 4 chloro 3 nitrobenzene sulphonamide 188 1.26





4 Hydroxy 3 amino benzene N-methyl sulphonamide

1. 4 chloro 3 nitrobenzene n methyl

sulphonamide

186 1.24





4 Hydroxy 3 amino benzene 2 carboxy sulpho anilide

1. 4 chloro 3 nitrobenzene 2 carboxy sulpho

anilide

173 1.16





3,5 Dinitro Benzoic Acid

1. Benzoic acid 86 0.58

2. Nitric acid 112 0.75

3. Oleum 156 1.04

5. 1,2 dichloro ethane 283 1.89

4 Amino 3 Nitro Anisole

1. Para anisidine 110 0.73

2. Acetic anhydride 98 0.65

3. Acetic acid 263 1.76

4. 4 methoxy acetanilide 147 0.98

5. Concentrated nitric acid 45 0.30

6. Concentrated sulfuric acid 131 0.88

4 Difloromethoxy 2 Nitro Aniline

1. P-hydroxy acetanilide 111 0.74


3. Difloro methylene chloride 64 0.43


4. Sulphuric acid 7 0.05

5. Nitric acid 172 1.15

4 Hydroxy 3 Amino benzene sulpho anilide

1. 4 chloro 3 nitrobenzene sulpho anilide 177 1.18





Sr.

No.

Name of Raw material Physical

form

Maximum

storage capacity at a

time (MT)

1. Ortho nitro aniline Solid 20

2. 4 methoxy 2 nitro aniline Solid 20

3. 4 methyl 2 nitro aniline Solid 20

4. 4 difloromethoxy 2 nitro aniline Solid 20

5. 2,5 dichloro nitro benzene Solid 20

6. 3,4 dichloro nitro benzene Solid 20

7. 4 chloro 3 nitro benzene sulphonamide Solid 20

8. 4 chloro 3 nitro benzene n-methyl sulphonamide Solid 20

9. 4 chloro 3 nitro benzene 2 carboxy

sulphonamide

Solid 20

10. Benzoic acid Solid 20

11. Para anisidine Solid 20

12. Para hydroxy acetanilide Solid 20

13. 4 chloro 3 nitro benzene sulphoanilide Solid 20

14. Sodium hydrogen sulphide Liquid 40

15. Carbon disulphide Liquid 15

16. Activated carbon Solid 5

17. Sodium bisulphite Liquid 40

18. Sodium hydroxide Solid 40

19. Hydrochloric acid Liquid 40

20. Nitric acid Liquid 10

21. Sulphuric acid Liquid 20

22. Oleum 23% Liquid 20

23. 1,2 dichloro ethane Liquid 10

24. Acetic anhydride Liquid 10

25. Acetic acid Liquid 10


Annexure-II

Manufacturing Process, chemical reaction & Mass Balance

1) 2 Mercaptobenzimidazole

Manufacturing process:

Mixture of ortho nitro aniline is dissolve in sodium hydrogen sulphide

solution at 100oC to 105oC for 6 to 7 hour after layer separation at 60oC -

70oC.

Mixture of ortho phynylene diamine and sodium hydroxide and carbon

disulphide and H2O is heated in a reactor under reflux for 5 to 6 hours.

After filter wet cake collected.

Mix the wet cake, H2O and activated carbon in sodium hydroxide solution

at 60oC to 65oC for 2-3 hours. After filter solution collected.

Maintain pH 7 of collected solution using HCl. After filter wet cake drying,

we get a commercial product 2 Mercaptobenzimidazole.

Chemical Reaction:

NH2

NO2

+ 2 NaSH100-105 °C

NH2

NH2

+ Na2S

2O

3

Stage-1

Stage-2

NH2

+ NaOH + CS2

100 °CN

NH

SH

Stage-3

Sodium Hydrogen Sulphide

ortho nitro aniline ortho

phenylenediamine

2-mercapto benzimidazole

N

NH

SH + NaOH + Activated Carbon

N

NH

SNa

Stage-4

N

NH

SNa + HCl

Filter

PA - 5N

NH

SH

NH2

+ + H2O

+ H2O

+ NaCl

NaSH



2-mercapto benzimidazole- sodium solution

2-mercapto benzimidazole- sodium solution

ortho phenylenediamine

H2OH

2O+ ++ 1/

2O

2


Mass Balance:

IN PUT Kg Kg OUT PUT

Ortho nitro aniline 138

Sodium hydrogen

sulphide solution

(30% solution)

420

451 ML to MEE

Sodium Hydroxide 45 680 ML to MEE

Carbon disulphide 95

Water 630

Sodium hydroxide 40

Water 1808

1845 ML to MEE

50 Drying loss

150 Product

Total 3176 3176

Centrifuge

Drying

2 mercapto benzimidazole

S S Reactor

Ortho phenylene

diamine

2 mercapto

benzimidazole

2 mercapto

benzimidazole


2) 5 Methoxy 2 mercaptobenzimidazole


Mixture of 4 methoxy 2 nitro aniline is dissolve in sodium hydrogen

sulphide solution at 100oC-105oC for 6-7 hours.

Mixture of 4 methoxy ortho phenyl diamine and sodium hydroxide and

carbon disulphide and H2O is heated in SS reactor under reflux for 5-6

hour. After filter wet cake collected.

Mix the wet cake, H2O and activated carbon in sodium hydroxide solution

at 60oC to 65oC for 2-3 hours. After filter solution collected.


we get commercial product 5 methoxy 2 mercaptoBenzimidazole.

Chemical reaction:

NH2

NO2

+ 2 NaSH100-105 °C

NH2

NH2

Stage-1

Stage-2

+ NaOH + CS2

N

NH

SH

Stage-3

N

NH


N

NH

SNa

Stage-4

N

NH

SNa + HCl

N

NH

SH

OCH3OCH3

NH2

NH2

OCH3

80 - 100 °C H3CO

H3CO H3CO

H3CO H3CO

+ NaSH + H2O

+ H2O

+ NaCl

4 methoxy 2 nitro aniline

4 methoxy ortho phenylene

diamine

4 methoxy ortho phenylene diamine

5 methoxy 2 mercapto benzimidazole


5 methoxy 2 mercapto benzimidazole-sodium solution

5 methoxy 2 mercapto benzimidazole- sodium solution


+ +Na2S

2O

3 H2O+ H

2O + 1/

2 O

2


Mass balance:


4 methoxy 2 nitro

anilene168

Sodium hydrogen

sulphide solution

(30% solution)420

450 ML to MEE

Sodium hydroxide 45

Carbon disulphide 95 682 ML to MEE

Water 630

Sodium hydroxide 40

Water 1808

1848 ML to MEE

45 Drying loss

181 Product

Total 3206 3206

Drying

5 methoxy 2 mercaptobenzomidazole

S S Reactor

4 methoxy ortho phenylene

diamine

5 methoxy 2 mercapto

benzimidazole- commercial

5 methoxy 2 mercapto

benzimidazole- commercial

Centrifuge


3) 5 Methyl 2 Mercaptobenzimidazole


Mixture of 4 methyl 2 nitro aniline is dissolve in sodium hydrogen

sulphide solution at 100oC-105oC for 6-7 hours.

Mixture of 4 methyl ortho phenyl diamine, sodium hydroxide, carbon

disulphide and H2O is heated in SS reactor under reflux for 5-6 hour.

After filter and wet cake collected.

Mix the wet cake, H2O and activated carbon and sodium hydroxide

solution at 60oC-65oC for 2-3 hours. After filter and solution collected.


we get commercial product 5 methyl 2 mercaptoBenzimidazole.

Chemical reaction:

NH2

NO2

+ 2 NaSH100-105 °C

NH2

NH2

Stage-1

Stage-2

+ NaOH + CS2

N

NH

SH

Stage-3

N

NH


N

NH

SNa

Stage-4

N

NH

SNa + HCl

N

NH

SH

CH3CH3

NH2

NH2

CH3

CH3

CH3 CH3

CH3CH3

+ H2O+NaSH

+ H2O

+ NaCl

4 methyl 2 nitroaniline 4 methyl ortho phenylenediamine

5 methyl 2 mercapto benzimidazole


4 methyl ortho phenylenediamine


5 methyl 2 mercapto benzimidazole-sodium

solution

5 methyl 2 mercapto benzimidazole-sodium

solution

+ +Na2S

2O

3 H2O+ H

2O+1/

2 O

2


Mass balance:


4 methyl 2

nitroaniline 152

Sodium hydrogen

sulphide solution

(30% solution)420

450 ML to MEE

Sodium hydroxide 45 669 ML to MEE


Water 630

Sodium hydroxide 40

8 Spent carbon

Water 1808

1848 ML to MEE

50 Drying loss

165 Product

Total 3190 3190

Drying

5 methyl 2 mercapto benzomidazole

SS.316 Reactor

4 methyl ortho

phenylenediamine

5 methyl 2 mercapto

benzimidazole

5 methyl 2 mercapto

benzimidazole

Centifuge


4) 5 Difloromethoxy 2 mercaptobenzimidazole


Mixture of 4 difloromethoxy 2 nitro aniline is dissolve in sodium hydrogen

sulphide solution at 100oC -105oC for 6-7 hours.

Mixture of 4 difloromethoxy ortho phenylene diamine, sodium hydroxide,

carbon disulphide and H2O is heated in SS reactor under reflux for 5-6

hour. After filter and wet cake collected.

Mix the wet cake, H2O and activated carbon and sodium hydroxide

solution at 60oC -65oC for 2-3 hours. After filter and solution collected.


we get pure product 5 difloromethoxy 2 mercaptoBenzimidazole.

Chemical reaction:

NH2

NO2

+ 2 NaSH100-105 °C

NH2

NH2

Stage-1

Stage-2

+ NaOH + CS2

N

NH

SH

Stage-3

N

NH


N

NH

SNa

Stage-4

N

NH

SNa + HCl

N

NH

SH

OCHF2

NH2

NH2

OCHF2

OCHF2

80-100 °C OCHF2

OCHF2OCHF2

OCHF2OCHF2

+ NaSH + H2O

+ H2O

+ NaCl

4 difluoromethoxy 2 nitroaniline

4 difluoromethoxy ortho phenylene diamine

4 difluoromethoxy ortho phenylene diamine

5 difluoromethoxy 2 mercapto benzimidazole



5 difluoromethoxy 2 mercapto benzimidazole-sodium solution

5 difluoromethoxy 2 mercapto benzimidazole-sodium solution

+ +Na2S

2O

3H

2O+ H

2O + 1/

2 O

2


Mass balance:


4 difluoro methoxy 2

nitro aniline204

Sodium hydrogen

sulphide solution

(30% solution)420

450 ML to MEE

Sodium hydroxide 45 662 ML to MEE


Water 630

Sodium hydroxide 40

Water 1808

1848 ML to MEE

65 Drying loss

217 Product

Total 3242 3242

Drying

5 difloromethoxy 2 mercapto benzimidazole

S S Reactor

4 difluoromethoxy

ortho phenylene

diamine

5 difluoromethoxy 2

mercapto

benzimidazole

5 difluoromethoxy 2

mercapto

benzimidazole

Centrifuge


5) 4 Hydroxy 3 Amino Chlorobenzene


Mixture of 2,5 dichloro nitro benzene is dissolve in sodium hydroxide and

H2O at 140oC for 12hours.

In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide

and sodium bisulphite at 100oC-105oC.

Maintain pH 7 of collected filter mass using HCl. After filter, we get pure

commercial product 4 hydroxy 3 amino chlorobenzene.

Chemical reaction:

Cl

+ 2NaOH

Stage-1

Stage-2

+ NaSH + NaHSO3

Stage-3

+

NO2NO2

ONa

Cl Cl

NO2

ONa

Cl

140 °C

100-105 °C

NH2

ONa

Cl

NH2

ONa

ClHCl

RT

NH2

OH

Cl

+ NaCl

+ NaCl

+ Na2S

2O

3.H

2O

2,5 dichloro nitro benzene

4-hydroxy,3-nitro chlorobenzene-sodium solution

4-hydroxy,3-nitro chlorobenzene-sodium

solution

4 hydroxy 3 amino chloro benzene

4 hydroxy 3 amino chloro benzene-sodium

solution

4 hydroxy 3 amino chloro benzene-sodium

solution

+ H2O

+ H2O +

1/2 O

2


Mass balance:


2,4 dichloro nitro

benzene 192

Sodium hydroxide 160

Water 600

Sodium hydrogen

sulphide solution 320Sodium bisulphite

solution 320

Hydrochloric Acid 300

1706 ML to MEE

43 Drying loss

143 Product

Total 1892 1892

4 hydroxy 3 amino chlorobenzene

MS Reactor

Drying

4 hydroxy 3 nitro chloro

benzene sodium solution

4 hydroxy 3 amino

chlorobenzene sodium

solution

4 hydroxy 3 amino

chlorobenzene

Filter & Centrifuge


6) 4 Hydroxy 3 Chloro Aniline


Mixture of 3,4 dichloro nitro benzene is dissolve in sodium hydroxide and

H2O at 140oC for 12 hours.


and sodium bisulphite at 100oC-105oC.


commercial product 4 hydroxy 3 chloro Aniline.

Chemical reaction:

Cl

+ 2 NaOH

Stage-1

Stage-2

+ NaSH +NaHSO3

Stage-3

+ HCl

Cl

NO2

ONa

NO2

Cl

ONa

NO2

Cl

ONa

NH2

Cl

ONa

Cl

OH

Cl

NH2 NH2

+ NaCl

+ NaCl

+ Na2S

2O

3.H

2O

3,4 dichloro nitrobenzene 4 hydroxy 3 chloro nitrobenzene-sodium

solution

4 hydroxy 3 chloro nitrobenzene-sodium

solution

4 hydroxy 3 chloro aniline-sodium solution

4 hydroxy 3 chloro aniline-sodium solution

4 hydroxy 3 chloro aniline

+ H2O

+ H2O + 1/

2O

2


Mass balance:


3,4 dichloro nitro

benzene192


Water 600

Sodium hydrogen

sulphide solution320

Sodium bisulphite

solution 320

Hydrochloric Acid 300

1706 ML to MEE

43 Drying loss

143 Product

Total 1892 1892

Drying

4 hydroxy 3 chloro anilene

MS Reactor

4 hydroxy 3 chloro nitro

benzene sodium solution


sodium solution


Filter & Centrifuge


7) 4 Hydroxy 3 Aminobenzene Sulphonamide


Mixture of 4 chloro 3 nitro benzene sulphonamide is dissolve in sodium

hydroxide and H2O at 100oC -105oC for 12 hours.


and sodium bisulphite at 100oC -105oC.


commercial product 4 hydroxy 3 Amino benzene Sulphonamide.

Chemical reaction:

+ 2 NaOH

Stage-1

Stage-2

+ NaSH + NaHSO3

Stage-3

+ HCl

SO2NH2

NO2

Cl

SO2NH2

NO2

ONa

SO2NH2

NO2

ONa

SO2NH2

NH2

ONa

SO2NH2

NH2

ONa

SO2NH2

NH2

OH

+ NaCl

+ NaCl

+ Na2S

2O

3.H

2O

4 chloro 3 nitrobenzene sulfonamide

4 hydroxy 3 nitrobenzene sulfonamide-sodium solution

4 hydroxy 3 nitrobenzene sulfonamide-sodium solution

4 hydroxy 3 aminobenzene sulfonamide-sodium solution

4 hydroxy 3 aminobenzene sulfonamide-sodium solution

4 hydroxy 3 aminobenzene sulfonamide

+ H2O

+ + 1/2 O

2H2O


Mass balance:


4 chloro 3

nitrobenzene

sulphonamide

236


Water 700

Sodium hydrogen

sulphide 320

Sodium bisulphite 320

Hydrochloric acid 300

1791 ML to MEE

57 Drying loss

188 Product

Total 2036 2036

Drying

4 hydroxy 3 aminobenzene sulphonamide

M.S. Reactor

4 hydroxy 3 aminobenzene

sulphonamide sodium

solution


sulphonamide

Filter & Centrifuge


8) 4 Hydroxy 3 Aminobenzene n Methyl Sulphonamide


Mixture of 4 chloro 3 nitro benzene n methyl sulphonamide is dissolve in

sodium hydroxide and H2O at 100oC -105oC for 12 hours.


and sodium bisulphite at 100oC -105oC.


commercial product 4 hydroxy 3 amino benzene n methyl Sulphonamide.

Chemical Reaction:

+ 2 NaOH

Stage-1

Stage-2

+ NaSH +NaHSO3

Stage-3

+ HCl

SO2NHCH3

NO2

Cl

NO2

ONa

NO2

ONa

NH2

ONa

NH2

ONa

NH2

OH

SO2NHCH3

SO2NHCH3SO2NHCH3

SO2NHCH3 SO2NHCH3

+ NaCl

+ NaCl

+ Na2S

2O

3.H

2O

4-chloro,3-nirobenzene,n-methyl sulfonamide 4-hydroxy,3-nirobenzene,n-

methyl sulfonamide-sodium solution

4-hydroxy,3-nirobenzene,n-methyl sulfonamide-sodium

solution

4-hydroxy,3-aminobenzene,n-methyl sulfonamide-sodium

solution

4-hydroxy,3-aminobenzene,n-methyl sulfonamide-sodium

solution

4-hydroxy,3-aminobenzene,n-methyl sulfonamide

+ H2O

+ H2O + 1/

2 O

2


Mass balance:


4 chloro 3 nitrobenzene N-

methyl sulphonamide250


Water 700

Sodium hydrogen sulphide 320



1788 ML to MEE

60 Drying loss

202 Product

Total 2050 2050

Drying

4 hydroxy 3 aminobenzene n methyl sulphonamide

M.S. Reactor

4 hydroxy 3 aminobenzene N-

methyl sulphonamide sodium

solution

4 hydroxy 3 aminobenzene N-

methayl sulphonamide

Filter & Centrifuge


9) 4 Hydroxy 3 Aminobenzene 2-carboxy Sulpho anilide


Mixture of 4 chloro 3 nitro benzene 2-carboxy sulpho anilide is dissolve in

sodium hydroxide and H2O at 100oC -105oC for 12 hours.


and sodium bisulphide at 100oC -105oC.


commercial product 4 hydroxy 3 amino benzene 2-carboxy Sulpho

anilide.

Chemical Reaction:

+ 3 NaOH

Stage-1

Stage-2

+ NaSH + NaHSO3

Stage-3

+ 2 HCl

SO2NH

NO2

Cl

COOH

SO2NH

NO2

ONa

COONa

SO2NH

NO2

ONa

COONa

SO2NH

NH2

ONa

COONa

SO2NH

NH2

ONa

COONa

SO2NH

NH2

OH

COOH + 2 NaCl

+ NaCl + 2 H2O

+ Na2S

2O

3.H

2O

4-chloro,3-nitrobenzene,2-carboxy sulfo anilide

4-hydroxy,3-nitrobenzene,2-carboxy sulfo anilide-sodium solution

4-hydroxy,3-nitrobenzene,2-carboxy sulfo anilide-sodium

solution

4-hydroxy,3-aminobenzene,2-carboxy sulfo anilide-sodium solution

4-hydroxy,3-aminobenzene,2-carboxy sulfo anilide-sodium solution

4-hydroxy,3-aminobenzene,2-carboxy sulfo anilide

+ H2O +1/

2O

2


Mass balance:


4 chloro 3 nitrobenzene 2

carboxy sulpho anilide356


Water 700

Sodium hydrogen sulphide 320



2096 ML to MEE

92 Drying loss

308 Product

Total 2496 2496

Drying

4 hydroxy 3 aminobenzene 2 carboxy sulpho anilide

M.S. Reactor

4 hydroxy 3 aminobenzene 2

carboxy sulpho anilide sodium

solution

4 hydroxy 3 aminobenzene 2

carboxy sulpho anilide

Filter & Centrifuge


10) 3,5 Dinitro Benzoic Acid


Benzoic acid is diluted in 1,2 dichloro ethane followed by the addition of

99% nitric acid after heating at 50oC. Then add drop wise oleum under

stirring over a period of 3 hours. Then continue this process for 2 hours at

50oC and then further continue the process for another 2 hours at 70oC.

This mixture is dumping in H2O and then recover 1,2 dichloro ethane at

90oC. And then get final product after filtration. And isolated product is

3,5 dinitro benzoic acid.

Chemical reaction:

COOH

+ 2 HNO3 + H

2SO

4.SO

3 + 1,2-Dichloro Ethane

benzoic acid

COOH

NO2NO2

3,5 dinitro benzoic acid

+2 H2SO

4 + 1,2-Dichloro Ethane+ H2O

Mass balance:


Benzoic acid 122

Nitric acid 158

Oleum 220 380Recovered 1,2

dichloro ethane

for reuse

1,2 dichloro ethane 400

Ice (H2O) 1200

1445 ML to MEE

212 Product

63 Drying loss

Total 2100 2100

3,5 dinitro benzoic acid

S.S. Reactor

Filter & Centrifuge

Drying


11) 4 Amino 3 Nitro Anisole


Mixture of paraanisidine is dissolve in glacial acetic acid and acetic

anhydride for 2-3 hours at room temperature. After addition of water we

get filtered wet cake that is product of step-1. Then dry the wet cake.

Dilute the dry cake in concentrated sulphuric acid and then add nitric

acid. This mixture is cooled to 0oC to 5oC and get isolated product. This

isolated product collected as wet cake after filteration.

The wet cake is hydrolyzed with hydrochloric acid for 30 mins at 100oC.

The reacted mixture is cooled at room temperature and then made

Alkaline with NaOH solution (20%). This mixture of water is then

crystallized and we get final product (4- amino 3 nitro anisole) after re-

crystallization.

Chemical Reaction:

+ (CH3CO)

2O/CH

3COOH

Stage-1

Stage-2

+ HNO3 + H

2SO

4

Stage-3

+ NaOH

OCH3

NH2

OCH3

NHCOCH3

OCH3

NHCOCH3

OCH3

NHCOCH3

NO2

OCH3

NHCOCH3

NO2

OCH3

NH2

NO2

+ H2O + H

2SO

4

+ CH3COONa

para anisidineacetic anhydride /

acetic acid

4-amino,3-nitro anisole

4-methoxy acetanilide

4-methoxy acetanilide 2-nitro,4-methoxy acetanilide

2-nitro,4-methoxy acetanilide

CH3COOH/H

2O+


Mass balance:

Input Kg Kg Output

Para anisidine 123

Acetic anhydride 110

Acetic acid 295

Water 370

295 Acetic acid

165

4 methoxy

acetanilide

438 ML to MEE

4 methoxy acetanilide 165

Concentrated nitric acid 50

Concentrated sulfuric acid 147

Water 370

514 ML to MEE

168 Product

50 Drying loss

Total 1630 1630

Wet cake

4 amino 3 nitro anisole

S.S. reactor

Filter & Centrifuge

Reactor

Filter & Centrifuge


12) 4 Difloromethoxy 2 Nitro Aniline


Add slowly difloro methylene chloride gas in mixture of P-hydroxy

acetanilide and sodium hydroxide and water. And then reacted mass is

heated to 50oC-55oC for 3-4 hours and maintain for 70-72 hour. After

reacted mass cooled at room temperature then after filtered the mixture

and wet cake collected. And dry the wet cake.

Sulphuric acid is added in dry wet cake and stirred at 30oC-35oC for 30

minute and then add nitric acid. Mixture is cooled to 20oC-25oC

temperature for 2-3 hours. Then after add water slowly and filter the

mixture.

Add water and soldium hydroxide in wet cake. Take this solution in

reactor and heated at 100oC-105oC. Get isolated mixture and then filter

the isolated mixture and then we get final product.

Chemical Reaction:

OH

NHCOCH3

+ NaOH + ClCHF2

NHCOCH3

OCHF2

NHCOCH3

OCHF2

+ H2SO4 + HNO3

NHCOCH3

OCHF2

NO2

NHCOCH3

OCHF2

NO2

+ NaOH

NH2

OCHF2

NO2

para hydroxy acitanilide 4-difloro methoxy acitanilide

4-difloro methoxy acitanilide

4-difloro methoxy,2-nitro

acitanilide

4-difloro methoxy,2-nitro

acitanilide

4-difloro methoxy,2-nitro aniline

+ NaCl + H2O

+ H2SO4 + H2O

+ CH3COONa


Mass balance:

Input Kg Kg Output

P-hydroxy acetanilide 151

Sodium hydroxide 88

Difloro methylene chloride 87

Water 390

446 ML to MEE

Sulphuric acid 10

Nitric acid 234

Water 600

750 ML to MEE

Sodium hydroxide 45

Water 600

705 ML to MEE

100 Drying loss

204 Product

Total 2205 2205

Drying

4 difloromethoxy 2 niro aniline

Reactor

Reactor

Reactor

Filter & Centrifuge

Filter

Filter


13) 4 Hydroxy 3 Amino Benzene Sulphoanilide


Mixture of 4 chloro 3 nitro benzene sulphoanilide is dissolve in sodium

hydroxide and H2O at 100oC-105oC for 12 hours.


and sodium bisulphite at 100oC-105oC. Then after filter the mixture and

collect the filter mass.

Maintain pH 7 of collected solution by adding HCl. After filter wet cake

drying, we get commercial product 4 hydroxy 3 amino benzene

sulphoanilide.

Chemical Reaction:

+ 2 NaOH

Stage-1

Stage-2

+NaSH + NaHSO3

Stage-3

+ HCl

SO2NH

NO2

Cl

SO2NH

NO2

ONa

SO2NH

NO2

ONa

SO2NH

NH2

ONa

SO2NH

NH2

ONa

SO2NH

NH2

+ NaCl

OH

+ NaCl

+ Na2S

2O

3.H

2O

4-chloro,3-nitrobenzene sulfoanilide

4-hydroxy,3-nitrobenzene sulfoanilide-sodium solution

4-hydroxy,3-nitrobenzene sulfoanilide-sodium solution

4-hydroxy,3-aminobenzene sulfoanilide-sodium solution

4-hydroxy,3-aminobenzene sulfoanilide-sodium solution

4-hydroxy,3-aminobenzene sulfoanilide

+ H2O

+ H2O + 1/

2O

2


Mass Balance:

Input Kg Kg Output

4 chloro 3

nitrobenzene sulpho

anilide312


Water 700

Sodium hydrogen

sulphide320



1768 ML to MEE

264 Product

80 Drying loss

Total 2112 2112

Drying

4 hydroxy 3 amino benzene sulpho anilide

M.S. Reactor


sulpho anilide-sodium

solution


sulpho anilide

Filter & Centrifuge


Annexure-III

Water consumption & wastewater generation

Sr.

No.

Source Water

Consumption

(KLD)

Wastewater

Generation

(KLD)

I Domestic 5.0 4.5

II Gardening 20.0 --

III Industrial

1 Process 97.5 120

2 Boiler 15.0 1.5

3 Cooling 50.0 5.0

4 Washing 10.0 10.0

5 Water treatment 2.0 2.0

Total Industrial 174.5 138.5

Total (I+II+III) 199.5 143

Recycle water 80 -

Actual fresh water

requirement

119.5 -


Water Balance Diagram

Water Consumption 199.5 KLD (119.5 Fresh + 80 recycle)

Domestic

5.0

Process

97.5

Washing

10.0*

Utilities

17.0 + 50*

Green belt

20.0*

Cooling

50.0* Boiler

15.0

MEE

120

Soak pit

4.5

Salt

1.8 Ton

Effluent 120

Blow down 1.5

Bleed off 5.0

To GIDC

drainage

18.5+36.7 =

55.2

ETP

10.0+1.5+2.0+5.0=18.5

System loss 1.5

Drying loss 2.0

From RM 24.5

Condensate 116.7*

2.0

36.7


Reference table for calculation of worst case scenario in terms of

hydraulic and organic load

Product Name W/C

(lit/day)

W/w

(lit/day)

COD

(mg/L)

COD

(kg/day)

TDS

(mg/L)

TDS

(kg/day)

2 mercapto

benzimidazole

97520.00 119040.00 4250 505.92 12183 1450.26

5 methoxy 2

mercaptobenzimidazole

80817.68 98784.53 5320 525.53 14872 1469.12

5 methyl 2


88654.55 107890.91 4891 527.69 13368 1442.29

5 difloromethoxy 2


67410.14 81843.32 5678 464.71 14563 1191.88

4 hydroxy 3 amino

chlorobenzene

25174.83 71580.42 7591 543.37 18784 1344.57

4 hydroxy 3 chloro

aniline

25174.83 71580.42 7591 543.37 18784 1344.57

4 hydroxy 3 amino

benzene sulphonamide

22340.43 57159.57 7952 454.53 15631 893.46

4 hydroxy 3 amino

benzene methyl

sulphonamide

20792.08 53108.91 8245 437.88 14978 795.47

4 hydroxy 3 amino

benzene 2 carboxy

sulphonamide

13636.36 40831.17 8636 352.62 15472 631.74

3,4 dinitro benzoic acid 33962.26 40896.23 3217 131.56 17654 721.98

4 amino 3 nitro anisole 26428.57 34000.00 6578 223.65 16423 558.38

4 difloromethoxy 2 nitro

aniline

46764.71 55911.76 7216 403.46 12789 715.06

4 hydroxy 3 amino

benzene sulphoanilide

15909.09 40181.82 8237 330.98 14562 585.13


Annexure-IV

Details of Air Emissions

Sr.

No.

Stack

attached to

Fuel Type &

rate of

consumption

Stack

Height

(m)

APC

measures

Probable

emission

Flue Gas Stacks

1. Boiler

(2 TPH)

Natural Gas-

4000 SCM/day

21 -- PM<150 mg/NM3

SO2<100 ppm

NOx<50 ppm 2. D.G Set

(125 KVA) –

Stand by

HSD-30 lit/hr. 11 --


Annexure-V

Details of Hazardous Generation and Disposal

Sr.

No.

Type of

Waste

Category

of Waste

Quantity Disposal facility

1. ETP sludge

& MEE salt

34.3 5 + 45 = 50

MT/month

Collection, Storage, Transportation

& Disposal at TSDF site.

2. Discarded

drums/

Liners

33.3 1000

nos./month

0.5

MT/month

Collection, Storage, Transportation

and disposal by selling to

authorized recycler.

3. Used oil 5.1 0.2 kl/year Collection, Storage, Transportation

and disposal by selling to

authorized re-refiners.

4. Used

activated

carbon

I-28.2 0.2

MT/month

Collection, Storage, Transportation,

Disposal at common Haz. waste

Incineration facility.

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