Annexure-I List of Products. List of Raw Materials
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1 Sr. o. Annexure-I List of Products Sr. ame of Product o 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 amino 3 nitro anisole difloromethoxy 2 nitro aniline 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 Sodium hydrogen sulphide (30%) Sodium hydroxide Carbon disulphide Methoxy 2 Mercapto 1. 4 methoxy 2 nitro aniline Sodium hydrogen sulphide (30%) Sodium hydroxide Carbon disulphide Methyl 2 Mercapto 1. 4 methyl 2 nitro aniline Sodium hydrogen sulphide (30%) Sodium hydroxide Carbon disulphide Difloromethoxy 2 Mercapto 1. 4 difluoro methoxy 2 nitro aniline Sodium hydrogen sulphide (30%) Sodium hydroxide Carbon disulphide Hydroxy 3 Amino Chlorobenzene 1. 2,4 dichloro nitro benzene Sodium bisulphite Asiatic Pharma Chem 1
2 3. Hydrochloric Acid Sodium hydroxide Sodium hydrogen sulphide Hydroxy 3 Chloro aniline 1. 3,4 dichloro nitro benzene Sodium bisulphite Hydrochloric Acid Sodium hydroxide Sodium hydrogen sulphide Hydroxy 3 Amino benzene sulphonamide 1. 4 chloro 3 nitrobenzene sulphonamide Sodium bisulphite Hydrochloric Acid Sodium hydroxide Sodium hydrogen sulphide Hydroxy 3 amino benzene -methyl sulphonamide 1. 4 chloro 3 nitrobenzene n methyl sulphonamide 2. Sodium bisulphite Hydrochloric Acid Sodium hydroxide Sodium hydrogen sulphide Hydroxy 3 amino benzene 2 carboxy sulpho anilide 1. 4 chloro 3 nitrobenzene 2 carboxy sulpho anilide 2. Sodium bisulphite Hydrochloric Acid Sodium hydroxide Sodium hydrogen sulphide ,5 Dinitro Benzoic Acid 1. Benzoic acid itric acid leum ,2 dichloro ethane Amino 3 itro Anisole 1. Para anisidine Acetic anhydride Acetic acid methoxy acetanilide Concentrated nitric acid Concentrated sulfuric acid Difloromethoxy 2 itro Aniline 1. P-hydroxy acetanilide Sodium hydroxide Difloro methylene chloride Asiatic Pharma Chem 2
3 4. Sulphuric acid itric acid Hydroxy 3 Amino benzene sulpho anilide 1. 4 chloro 3 nitrobenzene sulpho anilide Sodium bisulphite Sr. o. 3. Hydrochloric Acid Sodium hydroxide Sodium hydrogen sulphide ame of Raw material Physical form Maximum storage capacity at a time (MT) 1. rtho nitro aniline Solid methoxy 2 nitro aniline Solid methyl 2 nitro aniline Solid difloromethoxy 2 nitro aniline Solid ,5 dichloro nitro benzene Solid ,4 dichloro nitro benzene Solid chloro 3 nitro benzene sulphonamide Solid chloro 3 nitro benzene n-methyl sulphonamide Solid chloro 3 nitro benzene 2 carboxy Solid 20 sulphonamide 10. Benzoic acid Solid Para anisidine Solid Para hydroxy acetanilide Solid chloro 3 nitro benzene sulphoanilide Solid Sodium hydrogen sulphide Liquid Carbon disulphide Liquid Activated carbon Solid Sodium bisulphite Liquid Sodium hydroxide Solid Hydrochloric acid Liquid itric acid Liquid Sulphuric acid Liquid leum 23% Liquid ,2 dichloro ethane Liquid Acetic anhydride Liquid Acetic acid Liquid 10 Asiatic Pharma Chem 3
4 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 ash+ 1 / 2 2 Sodium Hydrogen Sulphide C 2 ortho phenylenediamine + a 2 S 2 3 H H 2 Stage 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
5 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 ML to MEE 2 mercapto Carbon disulphide 95 Water 630 Sodium hydroxide 40 Water mercapto Centrifuge 1845 ML to MEE Drying 50 Drying loss 150 Product Total Asiatic Pharma Chem 5
6 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 ash + H / C 2 + a 2 S 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 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
7 Mass balance: 5 methoxy 2 mercaptobenzomidazole I PUT Kg Kg UT PUT 4 methoxy 2 nitro anilene Sodium hydrogen sulphide (30% ) S S Reactor 4 methoxy ortho phenylene diamine 450 ML to MEE Sodium hydroxide 45 5 methoxy 2 mercapto Carbon disulphide ML to MEE - commercial Water 630 Sodium hydroxide 40 Water methoxy 2 mercapto - commercial Centrifuge 1848 ML to MEE Drying 45 Drying loss 181 Product Total Asiatic Pharma Chem 7
8 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 ash + H / C 2 + a 2 S 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
9 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 methyl 2 mercapto 8 Spent carbon Centifuge 1848 ML to MEE Drying 50 Drying loss 165 Product Total Asiatic Pharma Chem 9
10 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 ash + H / C 2 + a 2 S 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 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
11 Mass balance: 5 difloromethoxy 2 mercapto I PUT Kg Kg UT PUT 4 difluoro methoxy 2 nitro aniline sulphide (30% ) S S Reactor 4 difluoromethoxy ortho phenylene diamine 450 ML to MEE Sodium hydroxide 45 5 difluoromethoxy ML to MEE mercapto Carbon disulphide 95 Water 630 Sodium hydroxide 40 Water difluoromethoxy 2 mercapto Centrifuge 1848 ML to MEE Drying 65 Drying loss 217 Product Total Asiatic Pharma Chem 11
12 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 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 C + ash + ahs 3 + H + a 2 S H / 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
13 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 hydroxy 3 nitro chloro benzene sodium Sodium hydrogen sulphide 320 Sodium bisulphite hydroxy 3 amino chlorobenzene sodium Hydrochloric Acid hydroxy 3 amino chlorobenzene Filter & Centrifuge 1706 ML to MEE Drying 43 Drying loss 143 Product Total Asiatic Pharma Chem 13
14 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 ah + a + H 2 Stage-2 3,4 dichloro nitrobenzene 4 hydroxy 3 chloro nitrobenzene-sodium + ash + ahs 3 + H / 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
15 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 hydroxy 3 chloro aniline sodium Hydrochloric Acid hydroxy 3 chloro aniline Filter & Centrifuge 1706 ML to MEE Drying 43 Drying loss 143 Product Total Asiatic Pharma Chem 15
16 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 H / 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
17 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 hydroxy 3 aminobenzene sulphonamide sodium Hydrochloric acid hydroxy 3 aminobenzene sulphonamide Filter & Centrifuge 1791 ML to MEE Drying 57 Drying loss 188 Product Total Asiatic Pharma Chem 17
18 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 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
19 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 hydroxy 3 aminobenzene - methyl sulphonamide sodium Hydrochloric acid hydroxy 3 aminobenzene - methayl sulphonamide Filter & Centrifuge 1788 ML to MEE Drying 60 Drying loss 202 Product Total Asiatic Pharma Chem 19
20 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 / 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
21 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 hydroxy 3 aminobenzene 2 carboxy sulpho anilide sodium Hydrochloric acid hydroxy 3 aminobenzene 2 carboxy sulpho anilide Filter & Centrifuge 2096 ML to MEE Drying 92 Drying loss 308 Product Total Asiatic Pharma Chem 21
22 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 Asiatic Pharma Chem 22
23 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
24 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 Asiatic Pharma Chem 24
25 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 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
26 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 Asiatic Pharma Chem 26
27 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 / 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
28 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 hydroxy 3 aminobenzene sulpho anilide-sodium Hydrochloric acid hydroxy 3 aminobenzene sulpho anilide Filter & Centrifuge 1768 ML to MEE Drying 264 Product 80 Drying loss Total Asiatic Pharma Chem 28
29 Sr. o. Annexure-III Water consumption & wastewater generation Source Water Consumption (KLD) Wastewater Generation (KLD) I Domestic II Gardening III Industrial 1 Process Boiler Cooling Washing Water treatment Total Industrial Total (I+II+III) Recycle water 80 - Actual fresh water requirement Asiatic Pharma Chem 29
30 Water Balance Diagram Water Consumption KLD (119.5 Fresh + 80 recycle) Domestic 5.0 Process 97.5 Washing 10.0* Utilities * 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 Salt 1.8 Ton MEE 120 ETP =18.5 System loss 1.5 Condensate 116.7* 36.7 To GIDC drainage = 55.2 Asiatic Pharma Chem 30
31 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 methoxy mercapto 5 methyl mercapto 5 difloromethoxy mercapto 4 hydroxy 3 amino chlorobenzene 4 hydroxy 3 chloro aniline 4 hydroxy 3 amino benzene sulphonamide 4 hydroxy 3 amino benzene methyl sulphonamide 4 hydroxy 3 amino benzene 2 carboxy sulphonamide 3,4 dinitro benzoic acid amino 3 nitro anisole difloromethoxy 2 nitro aniline 4 hydroxy 3 amino benzene sulphoanilide Asiatic Pharma Chem 31
32 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 SCM/day HSD-30 lit/hr Probable emission PM<150 mg/m 3 <100 ppm x <50 ppm Asiatic Pharma Chem 32
33 Annexure-V Details of Hazardous Generation and Disposal Sr. Type of Category Quantity Disposal facility o. Waste of Waste 1. ETP sludge & MEE salt = 50 MT/month Collection, Storage, Transportation & Disposal at TSDF site. 2. Discarded Collection, Storage, Transportation drums/ nos./month and disposal by selling to Liners 0.5 authorized recycler. MT/month 3. Used oil kl/year Collection, Storage, Transportation and disposal by selling to authorized re-refiners. 4. Used activated carbon I MT/month Collection, Storage, Transportation, Disposal at common Haz. waste Incineration facility. Asiatic Pharma Chem 33
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