Sr. o. Annexure-I List of Products Sr. ame of Product o. 1. 2 mercapto 2. 5 methoxy 2 mercapto 3. 5 methyl 2 mercapto 4. 5 difloromethoxy 2 mercapto 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 List of Raw Materials ame of Raw material Quantity (MT/Month) 150 Total 150 Quantity (MT/Month) Quantity (MT/MT) 2 Mercapto 1. rtho nitro aniline 138 0.92 2. Sodium hydrogen sulphide (30%) 420 2.8 3. Sodium hydroxide 85 0.57 4. Carbon disulphide 95 0.63 5 Methoxy 2 Mercapto 1. 4 methoxy 2 nitro aniline 139 0.93 2. Sodium hydrogen sulphide (30%) 348 2.32 3. Sodium hydroxide 70 0.47 4. Carbon disulphide 79 0.52 5 Methyl 2 Mercapto 1. 4 methyl 2 nitro aniline 138 0.92 2. Sodium hydrogen sulphide (30%) 382 2.55 3. Sodium hydroxide 77 0.51 4. Carbon disulphide 86 0.58 5 Difloromethoxy 2 Mercapto 1. 4 difluoro methoxy 2 nitro aniline 141 0.94 2. Sodium hydrogen sulphide (30%) 290 1.94 3. Sodium hydroxide 59 0.39 4. Carbon disulphide 66 0.44 4 Hydroxy 3 Amino Chlorobenzene 1. 2,4 dichloro nitro benzene 201 1.34 2. Sodium bisulphite 336 2.24 Asiatic Pharma Chem 1
3. Hydrochloric Acid 315 2.10 4. Sodium hydroxide 168 1.12 5. Sodium hydrogen sulphide 336 2.24 4 Hydroxy 3 Chloro aniline 1. 3,4 dichloro nitro benzene 201 1.34 2. Sodium bisulphite 336 2.24 3. Hydrochloric Acid 315 2.10 4. Sodium hydroxide 168 1.12 5. Sodium hydrogen sulphide 336 2.24 4 Hydroxy 3 Amino benzene sulphonamide 1. 4 chloro 3 nitrobenzene sulphonamide 188 1.26 2. Sodium bisulphite 255 1.70 3. Hydrochloric Acid 239 1.60 4. Sodium hydroxide 128 0.85 5. Sodium hydrogen sulphide 255 1.70 4 Hydroxy 3 amino benzene -methyl sulphonamide 1. 4 chloro 3 nitrobenzene n methyl 186 1.24 sulphonamide 2. Sodium bisulphite 238 1.58 3. Hydrochloric Acid 223 1.49 4. Sodium hydroxide 119 0.79 5. Sodium hydrogen sulphide 238 1.58 4 Hydroxy 3 amino benzene 2 carboxy sulpho anilide 1. 4 chloro 3 nitrobenzene 2 carboxy sulpho 173 1.16 anilide 2. Sodium bisulphite 156 1.04 3. Hydrochloric Acid 292 1.95 4. Sodium hydroxide 97 0.65 5. Sodium hydrogen sulphide 156 1.04 3,5 Dinitro Benzoic Acid 1. Benzoic acid 86 0.58 2. itric acid 112 0.75 3. leum 156 1.04 5. 1,2 dichloro ethane 283 1.89 4 Amino 3 itro 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 itro Aniline 1. P-hydroxy acetanilide 111 0.74 2. Sodium hydroxide 65 0.43 3. Difloro methylene chloride 64 0.43 Asiatic Pharma Chem 2
4. Sulphuric acid 7 0.05 5. itric acid 172 1.15 4 Hydroxy 3 Amino benzene sulpho anilide 1. 4 chloro 3 nitrobenzene sulpho anilide 177 1.18 2. Sodium bisulphite 182 1.21 Sr. o. 3. Hydrochloric Acid 170 1.14 4. Sodium hydroxide 91 0.61 5. Sodium hydrogen sulphide 182 1.21 ame of Raw material Physical form Maximum storage capacity at a time (MT) 1. rtho 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 Solid 20 sulphonamide 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. itric acid Liquid 10 21. Sulphuric acid Liquid 20 22. leum 23% Liquid 20 23. 1,2 dichloro ethane Liquid 10 24. Acetic anhydride Liquid 10 25. Acetic acid Liquid 10 Asiatic Pharma Chem 3
Annexure-II Manufacturing Process, chemical reaction & Mass Balance 1) 2 Mercapto Manufacturing process: Mixture of ortho nitro aniline is dissolve in sodium hydrogen sulphide at 100 o C to 105 o C for 6 to 7 hour after layer separation at 60 o C - 70 o C. Mixture of ortho phynylene diamine and sodium hydroxide and carbon disulphide and H 2 is heated in a reactor under reflux for 5 to 6 hours. After filter wet cake collected. Mix the wet cake, H 2 and activated carbon in sodium hydroxide at 60 o C to 65 o C for 2-3 hours. After filter collected. Maintain ph 7 of collected using H. After filter wet cake drying, we get a commercial product 2 Mercapto. Chemical Reaction: Stage-1 Stage-2 ortho nitro aniline 2 + 2 ash+ 1 / 2 2 Sodium Hydrogen Sulphide 100-105 C 2 ortho phenylenediamine + a 2 S 2 3 H 2 + + H 2 Stage-3 2 100 C + ah + CS2 SH + + H 2 ortho phenylenediamine 2-mercapto ash 2-mercapto SH + ah + Activated Carbon Filter Sa 2-mercapto sodium + H 2 Stage-4 Sa + H PA - 5 SH + a 2-mercapto sodium 2-mercapto Asiatic Pharma Chem 4
Mass Balance: 2 mercapto rtho nitro aniline 138 Sodium hydrogen sulphide 420 (30% ) I PUT Kg Kg UT PUT S S Reactor rtho phenylene diamine 451 ML to MEE Sodium Hydroxide 45 680 ML to MEE 2 mercapto Carbon disulphide 95 Water 630 Sodium hydroxide 40 Water 1808 2 mercapto Centrifuge 1845 ML to MEE Drying 50 Drying loss 150 Product Total 3176 3176 Asiatic Pharma Chem 5
2) 5 Methoxy 2 mercapto Manufacturing process: Mixture of 4 methoxy 2 nitro aniline is dissolve in sodium hydrogen sulphide at 100 o C-105 o C for 6-7 hours. Mixture of 4 methoxy ortho phenyl diamine and sodium hydroxide and carbon disulphide and H2 is heated in SS reactor under reflux for 5-6 hour. After filter wet cake collected. Mix the wet cake, H 2 and activated carbon in sodium hydroxide at 60 o C to 65 o C for 2-3 hours. After filter collected. Maintain ph 7 of collected using H. After filter wet cake drying, we get commercial product 5 methoxy 2 mercaptobenzimidazole. Chemical reaction: Stage-1 2 + 2 ash + H 2 + 1 / 2 2 100-105 C 2 + a 2 S 2 3 + H 2 Stage-2 CH 3 CH 3 4 methoxy 2 nitro aniline 4 methoxy ortho phenylene diamine 2 CH 3 4 methoxy ortho phenylene diamine + ah + CS 2 80-100 C H 3 C 5 methoxy 2 mercapto SH + ash + H 2 Stage-3 H 3 C 5 methoxy 2 mercapto SH + ah + Activated Carbon H 3 C Sa 5 methoxy 2 mercapto -sodium + H 2 Stage-4 H 3 C 5 methoxy 2 mercapto - sodium H Sa + H 3 C 5 methoxy 2 mercapto SH + a Asiatic Pharma Chem 6
Mass balance: 5 methoxy 2 mercaptobenzomidazole I PUT Kg Kg UT PUT 4 methoxy 2 nitro anilene Sodium hydrogen sulphide (30% ) 168 420 S S Reactor 4 methoxy ortho phenylene diamine 450 ML to MEE Sodium hydroxide 45 5 methoxy 2 mercapto Carbon disulphide 95 682 ML to MEE - commercial Water 630 Sodium hydroxide 40 Water 1808 5 methoxy 2 mercapto - commercial Centrifuge 1848 ML to MEE Drying 45 Drying loss 181 Product Total 3206 3206 Asiatic Pharma Chem 7
3) 5 Methyl 2 Mercapto Manufacturing process: Mixture of 4 methyl 2 nitro aniline is dissolve in sodium hydrogen sulphide at 100 o C-105 o C for 6-7 hours. Mixture of 4 methyl ortho phenyl diamine, sodium hydroxide, carbon disulphide and H 2 is heated in SS reactor under reflux for 5-6 hour. After filter and wet cake collected. Mix the wet cake, H 2 and activated carbon and sodium hydroxide at 60 o C-65 o C for 2-3 hours. After filter and collected. Maintain ph 7 of collected using H. After filter wet cake drying, we get commercial product 5 methyl 2 mercaptobenzimidazole. Chemical reaction: Stage-1 2 + 2 ash + H 2 + 1 / 2 2 100-105 C 2 + a 2 S 2 3 + H 2 Stage-2 CH 3 CH 3 4 methyl 2 nitroaniline 4 methyl ortho phenylenediamine 2 CH 3 4 methyl ortho phenylenediamine + ah + CS 2 CH 3 5 methyl 2 mercapto SH H + ash + 2 Stage-3 CH 3 CH 3 5 methyl 2 mercapto SH + ah + Activated Carbon 5 methyl 2 mercapto -sodium Sa + H 2 Stage-4 CH 3 CH 3 5 methyl 2 mercapto -sodium Sa + H 5 methyl 2 mercapto SH + a Asiatic Pharma Chem 8
Mass balance: 5 methyl 2 mercapto benzomidazole 4 methyl 2 nitroaniline 152 Sodium hydrogen sulphide (30% ) I PUT Kg Kg UT PUT 420 SS.316 Reactor 4 methyl ortho phenylenediamine 450 ML to MEE Sodium hydroxide 45 5 methyl 2 mercapto 669 ML to MEE Carbon disulphide 95 Water 630 Sodium hydroxide 40 Water 1808 5 methyl 2 mercapto 8 Spent carbon Centifuge 1848 ML to MEE Drying 50 Drying loss 165 Product Total 3190 3190 Asiatic Pharma Chem 9
4) 5 Difloromethoxy 2 mercapto Manufacturing process: Mixture of 4 difloromethoxy 2 nitro aniline is dissolve in sodium hydrogen sulphide at 100 o C -105 o C for 6-7 hours. Mixture of 4 difloromethoxy ortho phenylene diamine, sodium hydroxide, carbon disulphide and H 2 is heated in SS reactor under reflux for 5-6 hour. After filter and wet cake collected. Mix the wet cake, H 2 and activated carbon and sodium hydroxide at 60 o C -65 o C for 2-3 hours. After filter and collected. Maintain ph 7 of collected using H. After filter wet cake drying, we get pure product 5 difloromethoxy 2 mercaptobenzimidazole. Chemical reaction: Stage-1 2 + 2 ash + H 2 + 1 / 2 2 100-105 C 2 + a 2 S 2 3 + H 2 CHF 2 4 difluoromethoxy 2 nitroaniline CHF 2 4 difluoromethoxy ortho phenylene diamine Stage-2 2 CHF 2 4 difluoromethoxy ortho phenylene diamine + ah + CS 2 80-100 C CHF 2 SH 5 difluoromethoxy 2 mercapto + ash + H 2 Stage-3 CHF 2 CHF 2 SH 5 difluoromethoxy 2 mercapto + ah + Activated Carbon Sa 5 difluoromethoxy 2 mercapto -sodium + H 2 Stage-4 CHF 2 CHF 2 5 difluoromethoxy 2 mercapto -sodium Sa + H SH 5 difluoromethoxy 2 mercapto + a Asiatic Pharma Chem 10
Mass balance: 5 difloromethoxy 2 mercapto I PUT Kg Kg UT PUT 4 difluoro methoxy 2 nitro aniline sulphide (30% ) 204 420 S S Reactor 4 difluoromethoxy ortho phenylene diamine 450 ML to MEE Sodium hydroxide 45 5 difluoromethoxy 2 662 ML to MEE mercapto Carbon disulphide 95 Water 630 Sodium hydroxide 40 Water 1808 5 difluoromethoxy 2 mercapto Centrifuge 1848 ML to MEE Drying 65 Drying loss 217 Product Total 3242 3242 Asiatic Pharma Chem 11
5) 4 Hydroxy 3 Amino Chlorobenzene Manufacturing process: Mixture of 2,5 dichloro nitro benzene is dissolve in sodium hydroxide and H 2 at 140 o C for 12hours. In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide and sodium bisulphite at 100 o C-105 o C. Maintain ph 7 of collected filter mass using H. After filter, we get pure commercial product 4 hydroxy 3 amino chlorobenzene. Chemical reaction: Stage-1 140 C 2,5 dichloro nitro benzene + 2aH 4-hydroxy,3-nitro chlorobenzene-sodium + a + H 2 Stage-2 Stage-3 4-hydroxy,3-nitro chlorobenzene-sodium 100-105 C + ash + ahs 3 + H + a 2 S 2. 2 3 H 2 + 1 / 2 2 4 hydroxy 3 amino chloro benzene-sodium 4 hydroxy 3 amino chloro benzene-sodium + H RT H 4 hydroxy 3 amino chloro benzene + a Asiatic Pharma Chem 12
Mass balance: 4 hydroxy 3 amino chlorobenzene I PUT Kg Kg UT PUT 2,4 dichloro nitro benzene 192 MS Reactor Sodium hydroxide 160 Water 600 4 hydroxy 3 nitro chloro benzene sodium Sodium hydrogen sulphide 320 Sodium bisulphite 320 4 hydroxy 3 amino chlorobenzene sodium Hydrochloric Acid 300 4 hydroxy 3 amino chlorobenzene Filter & Centrifuge 1706 ML to MEE Drying 43 Drying loss 143 Product Total 1892 1892 Asiatic Pharma Chem 13
6) 4 Hydroxy 3 Chloro Aniline Manufacturing process: Mixture of 3,4 dichloro nitro benzene is dissolve in sodium hydroxide and H 2 at 140 o C for 12 hours. In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide and sodium bisulphite at 100 o C-105 o C. Maintain ph 7 of collected filter mass using H. After filter, we get pure commercial product 4 hydroxy 3 chloro Aniline. Chemical reaction: Stage-1 + 2 ah + a + H 2 Stage-2 3,4 dichloro nitrobenzene 4 hydroxy 3 chloro nitrobenzene-sodium + ash + ahs 3 + H 2 + 1 / 2 2 + a 2 S 2 3. H 2 4 hydroxy 3 chloro nitrobenzene-sodium Stage-3 + H 4 hydroxy 3 chloro aniline-sodium H + a 4 hydroxy 3 chloro aniline-sodium 4 hydroxy 3 chloro aniline Asiatic Pharma Chem 14
Mass balance: 4 hydroxy 3 chloro anilene I PUT Kg Kg UT PUT 3,4 dichloro nitro benzene 192 Sodium hydroxide 160 Water 600 MS Reactor 4 hydroxy 3 chloro nitro benzene sodium Sodium hydrogen 320 sulphide Sodium bisulphite 320 4 hydroxy 3 chloro aniline sodium Hydrochloric Acid 300 4 hydroxy 3 chloro aniline Filter & Centrifuge 1706 ML to MEE Drying 43 Drying loss 143 Product Total 1892 1892 Asiatic Pharma Chem 15
7) 4 Hydroxy 3 Aminobenzene Sulphonamide Manufacturing process: Mixture of 4 chloro 3 nitro benzene sulphonamide is dissolve in sodium hydroxide and H 2 at 100 o C -105 o C for 12 hours. In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide and sodium bisulphite at 100 o C -105 o C. Maintain ph 7 of collected filter mass using H. After filter, we get pure commercial product 4 hydroxy 3 Amino benzene Sulphonamide. Chemical reaction: Stage-1 4 chloro 3 nitrobenzene sulfonamide + 2 ah 4 hydroxy 3 nitrobenzene sulfonamide-sodium + a + H 2 Stage-2 Stage-3 + ash + ahs 3 + H + a S. 2 2 3 H 2 + 1 2 / 2 2 4 hydroxy 3 nitrobenzene sulfonamide-sodium 4 hydroxy 3 aminobenzene sulfonamide-sodium 4 hydroxy 3 aminobenzene sulfonamide-sodium + H H 4 hydroxy 3 aminobenzene sulfonamide + a Asiatic Pharma Chem 16
Mass balance: 4 hydroxy 3 aminobenzene sulphonamide I PUT Kg Kg UT PUT 4 chloro 3 nitrobenzene sulphonamide 236 Sodium hydroxide 160 Water 700 M.S. Reactor Sodium hydrogen sulphide 320 Sodium bisulphite 320 4 hydroxy 3 aminobenzene sulphonamide sodium Hydrochloric acid 300 4 hydroxy 3 aminobenzene sulphonamide Filter & Centrifuge 1791 ML to MEE Drying 57 Drying loss 188 Product Total 2036 2036 Asiatic Pharma Chem 17
8) 4 Hydroxy 3 Aminobenzene n Methyl Sulphonamide Manufacturing process: Mixture of 4 chloro 3 nitro benzene n methyl sulphonamide is dissolve in sodium hydroxide and H 2 at 100 o C -105 o C for 12 hours. In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide and sodium bisulphite at 100 o C -105 o C. Maintain ph 7 of collected filter mass using H. After filter, we get pure commercial product 4 hydroxy 3 amino benzene n methyl Sulphonamide. Chemical Reaction: Stage-1 CH 3 CH 3 Stage-2 Stage-3 4-chloro,3-nirobenzene,nmethyl sulfonamide + 2 ah CH 3 CH 3 4-hydroxy,3-nirobenzene,nmethyl sulfonamide-sodium 4-hydroxy,3-nirobenzene,nmethyl sulfonamide-sodium + ash + ahs 3 + H 2 + 1 / 2 2 CH 3 CH 3 + a + H 2 4-hydroxy,3-aminobenzene,nmethyl sulfonamide-sodium + a 2 S 2 3.H 2 4-hydroxy,3-aminobenzene,nmethyl sulfonamide-sodium + H H 4-hydroxy,3-aminobenzene,nmethyl sulfonamide + a Asiatic Pharma Chem 18
Mass balance: 4 hydroxy 3 aminobenzene n methyl sulphonamide 4 chloro 3 nitrobenzene - methyl sulphonamide I PUT Kg Kg UT PUT 250 Sodium hydroxide 160 Water 700 M.S. Reactor Sodium hydrogen sulphide 320 Sodium bisulphite 320 4 hydroxy 3 aminobenzene - methyl sulphonamide sodium Hydrochloric acid 300 4 hydroxy 3 aminobenzene - methayl sulphonamide Filter & Centrifuge 1788 ML to MEE Drying 60 Drying loss 202 Product Total 2050 2050 Asiatic Pharma Chem 19
9) 4 Hydroxy 3 Aminobenzene 2-carboxy Sulpho anilide Manufacturing process: Mixture of 4 chloro 3 nitro benzene 2-carboxy sulpho anilide is dissolve in sodium hydroxide and H 2 at 100 o C -105 o C for 12 hours. In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide and sodium bisulphide at 100 o C -105 o C. Maintain ph 7 of collected filter mass using H. After filter, we get pure commercial product 4 hydroxy 3 amino benzene 2-carboxy Sulpho anilide. Chemical Reaction: Stage-1 Stage-2 CH 4-chloro,3-nitrobenzene,2 -carboxy sulfo anilide + 3 ah C 4-hydroxy,3-nitrobenzene,2-carb oxy sulfo anilide-sodium + a + 2 H 2 Stage-3 C 4-hydroxy,3-nitrobenzene,2-ca rboxy sulfo anilide-sodium C + ash + ahs 3 + H 2 + a 2 S 2 3.H 2 + 1 / 2 2 4-hydroxy,3-aminobenzene,2-carbo xy sulfo anilide-sodium C 4-hydroxy,3-aminobenzene,2-carbo xy sulfo anilide-sodium + 2 H H CH + 2 a 4-hydroxy,3-aminobenzene,2-carbo xy sulfo anilide Asiatic Pharma Chem 20
Mass balance: 4 hydroxy 3 aminobenzene 2 carboxy sulpho anilide I PUT Kg Kg UT PUT 4 chloro 3 nitrobenzene 2 carboxy sulpho anilide 356 Sodium hydroxide 200 Water 700 M.S. Reactor Sodium hydrogen sulphide 320 Sodium bisulphite 320 4 hydroxy 3 aminobenzene 2 carboxy sulpho anilide sodium Hydrochloric acid 600 4 hydroxy 3 aminobenzene 2 carboxy sulpho anilide Filter & Centrifuge 2096 ML to MEE Drying 92 Drying loss 308 Product Total 2496 2496 Asiatic Pharma Chem 21
10) 3,5 Dinitro Benzoic Acid Manufacturing process: Benzoic acid is diluted in 1,2 dichloro ethane followed by the addition of 99% nitric acid after heating at 50 o C. Then add drop wise oleum under stirring over a period of 3 hours. Then continue this process for 2 hours at 50 o C and then further continue the process for another 2 hours at 70 o C. This mixture is dumping in H 2 and then recover 1,2 dichloro ethane at 90 o C. And then get final product after filtration. And isolated product is 3,5 dinitro benzoic acid. Chemical reaction: CH + 2 H 3 + H 2 S 4. S 3 + 1,2-Dichloro Ethane benzoic acid CH +2 H 2 S 4 + H + 1,2-Dichloro Ethane 2 3,5 dinitro benzoic acid Mass balance: 3,5 dinitro benzoic acid Benzoic acid 122 itric acid 158 I PUT Kg Kg UT PUT leum 220 S.S. Reactor 380 1,2 dichloro ethane 400 Ice (H2) 1200 Recovered 1,2 dichloro ethane for reuse Filter & Centrifuge 1445 ML to MEE Drying 212 Product 63 Drying loss Total 2100 2100 Asiatic Pharma Chem 22
11) 4 Amino 3 itro Anisole Manufacturing process: 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 0 o C to 5 o C 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 100 o C. The reacted mixture is cooled at room temperature and then made Alkaline with ah (20%). This mixture of water is then crystallized and we get final product (4- amino 3 nitro anisole) after recrystallization. Chemical Reaction: Stage-1 CCH 3 + (CH 3 C) 2 /CH 3 CH + CH 3 CH/H 2 CH 3 para anisidine acetic anhydride / acetic acid CH 3 4-methoxy acetanilide Stage-2 CCH 3 CCH 3 + H 3 + H 2 S 4 + H 2 + H 2 S 4 CH 3 4-methoxy acetanilide CH 3 2-nitro,4-methoxy acetanilide Stage-3 CCH 3 + ah + CH 3 C CH 3 2-nitro,4-methoxy acetanilide CH 3 4-amino,3-nitro anisole Asiatic Pharma Chem 23
Mass balance: 4 amino 3 nitro anisole Input Kg Kg utput Para anisidine 123 Acetic anhydride 110 Acetic acid 295 Water 370 S.S. reactor Filter & Centrifuge 295 Acetic acid 4 methoxy 165 acetanilide 438 ML to MEE 4 methoxy acetanilide 165 Concentrated nitric acid 50 Concentrated sulfuric acid 147 Water 370 Reactor Filter & Centrifuge 514 ML to MEE Wet cake 168 Product 50 Drying loss Total 1630 1630 Asiatic Pharma Chem 24
12) 4 Difloromethoxy 2 itro Aniline Manufacturing process: Add slowly difloro methylene chloride gas in mixture of P-hydroxy acetanilide and sodium hydroxide and water. And then reacted mass is heated to 50 o C-55 o C 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 30 o C-35 o C for 30 minute and then add nitric acid. Mixture is cooled to 20 o C-25 o C temperature for 2-3 hours. Then after add water slowly and filter the mixture. Add water and soldium hydroxide in wet cake. Take this in reactor and heated at 100 o C-105 o C. Get isolated mixture and then filter the isolated mixture and then we get final product. Chemical Reaction: H CHF 2 CCH 3 + ah para hydroxy acitanilide + CHF2 CCH 3 4-difloro methoxy acitanilide + a + H 2 CHF 2 + H2S4 + H3 CHF 2 + H 2 S 4 + H 2 CCH 3 4-difloro methoxy acitanilide CCH 3 4-difloro methoxy,2-nitro acitanilide CHF 2 CHF 2 + ah + CH 3 C CCH 3 4-difloro methoxy,2-nitro acitanilide 4-difloro methoxy,2-nitro aniline Asiatic Pharma Chem 25
Mass balance: 4 difloromethoxy 2 niro aniline Input Kg Kg utput P-hydroxy acetanilide 151 Sodium hydroxide 88 Difloro methylene chloride 87 Water 390 Reactor Filter 446 ML to MEE Sulphuric acid 10 itric acid 234 Water 600 Reactor Filter 750 ML to MEE Sodium hydroxide 45 Water 600 Reactor Filter & Centrifuge 705 ML to MEE Drying 100 Drying loss 204 Product Total 2205 2205 Asiatic Pharma Chem 26
13) 4 Hydroxy 3 Amino Benzene Sulphoanilide Manufacturing process: Mixture of 4 chloro 3 nitro benzene sulphoanilide is dissolve in sodium hydroxide and H 2 at 100 o C-105 o C for 12 hours. In step-2, mother liquor of step-1 is added in sodium hydrogen sulphide and sodium bisulphite at 100 o C-105 o C. Then after filter the mixture and collect the filter mass. Maintain ph 7 of collected by adding H. After filter wet cake drying, we get commercial product 4 hydroxy 3 amino benzene sulphoanilide. Chemical Reaction: Stage-1 Stage-2 4-chloro,3-nitrobenzene sulfoanilide + 2 ah 4-hydroxy,3-nitrobenzene sulfoanilide-sodium + a + H 2 4-hydroxy,3-nitrobenzene sulfoanilide-sodium +ash + ahs 3 + a 2 S 2 3. H 2 + H 2 + 1 / 2 2 4-hydroxy,3-aminobenzene sulfoanilide-sodium Stage-3 4-hydroxy,3-aminobenzene sulfoanilide-sodium + H H 4-hydroxy,3-aminobenzene sulfoanilide + a Asiatic Pharma Chem 27
Mass Balance: 4 hydroxy 3 amino benzene sulpho anilide Input Kg Kg utput 4 chloro 3 nitrobenzene sulpho anilide 312 Sodium hydroxide 160 Water 700 M.S. Reactor Sodium hydrogen sulphide 320 Sodium bisulphite 320 4 hydroxy 3 aminobenzene sulpho anilide-sodium Hydrochloric acid 300 4 hydroxy 3 aminobenzene sulpho anilide Filter & Centrifuge 1768 ML to MEE Drying 264 Product 80 Drying loss Total 2112 2112 Asiatic Pharma Chem 28
Sr. o. Annexure-III Water consumption & wastewater generation 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 - Asiatic Pharma Chem 29
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* Soak pit 4.5 Drying loss 2.0 From RM 24.5 Boiler 15.0 Cooling 50.0* Effluent 120 Blow down 1.5 Bleed off 5.0 2.0 Salt 1.8 Ton MEE 120 ETP 10.0+1.5+2.0+5.0=18.5 System loss 1.5 Condensate 116.7* 36.7 To GIDC drainage 18.5+36.7 = 55.2 Asiatic Pharma Chem 30
Reference table for calculation of worst case scenario in terms of hydraulic and organic load Product ame W/C (lit/day) W/w (lit/day) CD (mg/l) CD (kg/day) TDS (mg/l) TDS (kg/day) 2 mercapto 97520.00 119040.00 4250 505.92 12183 1450.26 5 methoxy 2 80817.68 98784.53 5320 525.53 14872 1469.12 mercapto 5 methyl 2 88654.55 107890.91 4891 527.69 13368 1442.29 mercapto 5 difloromethoxy 2 67410.14 81843.32 5678 464.71 14563 1191.88 mercapto 4 hydroxy 3 amino 25174.83 71580.42 7591 543.37 18784 1344.57 chlorobenzene 4 hydroxy 3 chloro 25174.83 71580.42 7591 543.37 18784 1344.57 aniline 4 hydroxy 3 amino 22340.43 57159.57 7952 454.53 15631 893.46 benzene sulphonamide 4 hydroxy 3 amino 20792.08 53108.91 8245 437.88 14978 795.47 benzene methyl sulphonamide 4 hydroxy 3 amino 13636.36 40831.17 8636 352.62 15472 631.74 benzene 2 carboxy sulphonamide 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 4 hydroxy 3 amino benzene sulphoanilide 46764.71 55911.76 7216 403.46 12789 715.06 15909.09 40181.82 8237 330.98 14562 585.13 Asiatic Pharma Chem 31
Sr. o. Stack attached to Flue Gas Stacks 1. Boiler (2 TPH) 2. D.G Set (125 KVA) Stand by Annexure-IV Details of Air Emissions Fuel Type & rate of consumption Stack Height (m) APC measures atural Gas- 4000 SCM/day HSD-30 lit/hr. 11 -- Probable emission 21 -- PM<150 mg/m 3 <100 ppm x <50 ppm Asiatic Pharma Chem 32
Annexure-V Details of Hazardous Generation and Disposal Sr. Type of Category Quantity Disposal facility o. Waste of Waste 1. ETP sludge & MEE salt 34.3 5 + 45 = 50 MT/month Collection, Storage, Transportation & Disposal at TSDF site. 2. Discarded 33.3 1000 Collection, Storage, Transportation drums/ nos./month and disposal by selling to Liners 0.5 authorized recycler. MT/month 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. Asiatic Pharma Chem 33