Vishwa Chemicals Plot No. 4801/A/13, GIDC Ankleshwar Dist: Bharuch
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1 Annexure-I List of Products & Raw Materials Sr.No Name of Products Existing Product 1 Zinc Sulphate/ Sodium Nitrate (Existing Product As Per GPCB CCA NO: AWH ) Proposed Product Existing prod. cap Existing MT/Month 2 Ammonium Formate proposed Ammonium Acetate MT/Month 4 Ammonium Propionate 5 Methyl 3 Amino Crotonate 6 Sodium 2. Ethyl Hexonate 7 Sodium formate 8 Methanolic ammonia 9 Methanolic MMA 10 Propyl propionate 11 1 Chloromthyl Naphthalene 12 N-Ethyl-2-nitromethylenepyrrolidine 13 Barbituric acid 14 N-methyl-1Naphthalene methaneamine 15 Veratraldehyde 16 Solvent distillation(mdc,methanol,toluene,aceton IPA,ethyl acetate,thf,n-hexane) List of byproduct Proposed Total Quantity prod. cap (MT/Month) MT/Month Sr. No Name of byproducts Existing Proposed Quantity (MT/Month) byproduct byproduct 1 HCL 22% Proposed Note: Our total production= existing + proposed 200 MT/month 1
2 List of Raw Material Sr. No Name of Raw Material Qunatity MT/Month 1 Ammonium Formate Formic Acid 24.3 Ammonia Ammonium acetate Acetic Acid 26.0 Ammonia Ammonium Propionate Propionic Acid 15.9 Ammonia 3.7 Water Methyl 3 Amino Crotonate Methyl Acetoacetate 33.3 Ammonia Sodium 2 Ethyl Hexanoate 2-Ethyl Hexanoic Acid 26.0 Caustic soda Sodium Formate Formic Acid 21.9 Sodium hydroxide Methanolic Ammonia Methanol 52.9 Ammonia Methanolic MMA Methanol 48.0 Monomethyl amine Propyl propionate Propanoic acid 32.8 Propanol Chloro Methyl Naphthalene in toluene Naphthalene 21.0 Para Formaldehyde 4.9 HCl (34%) 52.5 Toluene
3 Sr. No Name of Raw Material Qunatity MT/Month 11 N-ethyl-2-nitromethylenepyrrolidine 1-ethyl-2-pyrrolidinone 4.5 dimethyl sulfate 5.1 sodium methoxide 7.3 nitromethane 3.3 MDC 18.1 Toluene Barbituric acid Methanol 29.6 sodium 1.2 Diethyl melonate 7.2 urea 2.8 Water 17.2 HCl N-methyl-1Naphthalene methaneamine 1-chloromethyl naphthalene 4.5 N-methyl formamide 2.2 Sodium hydride (50% in parafin) 1.4 N,N-Dimethylformamide 10.5 Toluene 54.5 Water 48.8 Sodium hydroxide 6.6 Hydrochloric acid 32.0 Carbon Veratraldehyde Vanillin 5.3 Water 9.3 Sodium hydroxide 2.8 Dimethyl sulphate 4.4 Sulphuric Acid-50% 0.8 3
4 1. Ammonium Formate Annexure-II Manufacturing process, PFD and Mass Balance In SS reactor, formic acid is charged. Start ammonia gas purging at 30 to 40 0 C under cooling circulation till ph is raised up to 7.0 to 7.5. Keep the reaction mass for 1 hr. cool the reaction mixture at room temperature to crystallize & then filter the reaction mass in centrifuge. Collect the mother liquor as solution of ammonium formate and it is recycled in next batch and pack the wet cake as finished product ammonium formate. H H C H H N H H C Formic Acid Ammonia Ammonium Formate NH 4 MATERIAL BALANCE FOR PRODUCT: Formic Acid Kg Ammonium Formate Kg Ammonia Kg ML (ammonium formate-recycle) Kg Total Kg Total Kg FLOW DIAGRAM: 4
5 2. Ammonium Acetate Vishwa Chemicals In SS reactor, acetic acid is charged. Start ammonia gas purging at 30 to 40 0 C under cooling circulation till ph is raised up to 7.0 to 7.5. Keep the reaction mass for 1 hr. cool the reaction mixture at room temperature to crystallize & then filter the reaction mass in centrifuge. Collect the mother liquor as solution of ammonium acetate and it is recycled in next batch and pack the wet cake as finished product ammonium acetate or dry it & pack it as per requirement. H CH3 C H H N H CH3 C NH 4 60 g/mol 17 g/mol 77 g/mol Acetic Acid Ammonia Ammonium acetate MATERIAL BALANCE FOR PRODUCT: Acetic Acid Kg Ammonium acetate Kg Ammonia Kg ML (ammonium acetate-recycle) Kg Total Kg Total Kg FLOW DIAGRAM: Acetic acid Kg Ammonia gas Kg 1000 Kg Mix under Cool & Crystallize Centrifuge Wet cake 900 KG 100 kg ML (Recycle) Drying 45 Kg Evaporation Unload & Pack 855 Kg 5
6 3. Ammonium Propionate Charge propionic acid & water in reactor. Start addition of ammonia gas till the reaction complies. Unload the liquid finish product Ammonium Propionate in carboys and pack it. CH 3 CH 2 COOH + NH 3 CH 3 CH 2 COONH 4 Propionic Acid Ammonia Ammonium Propionate MATERIAL BALANCE FOR PRODUCT: Propionic Acid Kg Ammonium Propionate Kg Ammonia Kg Water Kg Total Kg Total Kg FLOW DIAGRAM: Propionic Acid Kg Ammonia Kg Water Kg MIX UNDER COOL 1149 Kg PACKING CARBOY Ammonium Propionate 65 % 1149 Kg 6
7 4. METHYL 3 AMINO CROTONATE Charge methyl acetoacetate in reactor at room temp. Start charging of ammonia in reactor at C till reaction over. Cool the reaction mass to crystallize. Centrifuge the mass and dry the wet cake. Pack the dry material in bags as finish product. CH 3 CO - CH 2 - COOCH 3 + NH 3 CH 3 C = CH COOCH 3 + H 2 O NH 2 Methyl Acetoacetate Ammonia Methyl 3 Amino Crotonate Water MATERIAL BALANCE FOR KG PRODUCT: Methyl Acetoacetate Kg Methyl 3 Amino Crotonate Kg Ammonia Kg Mother Liquor (M3AC-Recycle) Kg Evaporation Loss Kg Total Kg Total Kg FLOW DIAGRAM: Methyl Acetoacetate Kg Ammonia Kg 1291 kg Mix heat & Cool Centrifuge 175 Kg Mother Liquor Recycle in Next Batch Wet cake 1116 KG Drying 103 Kg Evaporation Loss Packing 1013 kg 7
8 5. SODIUM-2-ETHYL HEXANOATE Charge 2-Ethyl Hexanoic acid in SS reactor and add caustic soda (Sodium Hydroxide) in it at 30 to 40 C till ph is raised up to 9.0 to 9.5. After completion of the reaction vacuum dry the reaction mass to crystallize. Then multimill the powder and pack it. C 8 H 16 O 2 + NaOH C 8 H 15 O 2 Na + H 2 O 2 Ethyl Hexanoic acid Caustic soda Sodium 2 ethyl hexanoate water MATERIAL BALANCE FOR PRODUCT 2-Ethyl Hexanoic Acid Kg Sodium 2 Ethyl Hexanoate Kg Caustic soda 80.0 Kg Evaporation Loss 36.0 Kg Total Kg Total Kg FLOW DIAGRAM: 8
9 6. Sodium Formate In SS reactor, formic acid is charged. Add Sodium hydroxide flakes lot wise at 30 to 40 0 C under cooling circulation till ph is raised up to 7.0 to 7.5. Keep the reaction mass for 1 hr. cool the reaction mixture at room temperature to crystallize & then filter the reaction mass in centrifuge. Collect the mother liquor as solution of sodium formate and it is recycled in next batch. Dry the wet cake and pack the finished product sodium formate. HCOOH + NaOH HCOONa + H2O Formic acid sodium hydroxide sodium formate water MATERIAL BALANCE FOR PRODUCT: Formic Acid Kg Sodium Formate Kg Sodium hydroxide Kg ML (Recycle) 251 Kg water, 79 Kg sodium formate Kg Evaporation loss 35.0 Kg Total Kg Total Kg Flow Diagram Formic acid Kg Sodium hydroxide Kg 1365 Kg Mix under Cool & Crystallize Centrifuge 330 kg ML (Recycle) Wet cake 1035 KG Drying 35 Kg Evaporation 9
10 Vishwa Chemicals Unload & Pack 1000 Kg 7. METHANOLIC AMMONIA In SS reactor, methanol is charged. Start ammonia gas purging at C under chilled water circulation till it complies the percentage. Once the desired percentage achieved unload the mass to pack in carboys or drum. CH 3 OH + NH 3 CH 3 OH NH 3 Methanol Ammonia Methanolic Ammonia MATERIAL BALANCE FOR PRODUCT: Methanol Kg Methanolic Ammonia Kg Ammonia Kg Total Kg Total Kg FLOW DIAGRAM Methanol Kg Ammonia Kg Mix under Cool Unload & Pack 1000 Kg 10
11 8. METHANOLIC MONOMETHYLAMINE In SS reactor, methanol is charged. Start Monomethyl amine gas purging at C under chilled water circulation till it complies the percentage. Once the desired percentage achieved unload the mass to pack in carboys or drum. CH 3 OH + CH 3 NH 2 CH 3 OH CH 3 NH 2 Methanol Monomethylamine Methanolic MMA MATERIAL BALANCE FOR PRODUCT: Methanol Kg Methanolic MMA Kg Monomethyl amine Kg Total Kg Total Kg FLOW DIAGRAM: Methanol Kg MMA Kg Mix under Cool Unload & Pack 1000 Kg 11
12 9. PROPYL PROPIONATE Charge propanoic acid and propanol in a reactor. Heat the mass to reflux till reaction complies. Cool the mass to 25 C. separate out water. Remaining product to pack in carboys or drum. CH 3 CH 2 COOH + CH 3 CH 2 OH CH 3 CH 2 COOCH 2 CH 2 CH 3 + H 2 O Propanoic acid Propanol Propyl propionate Water MATERIAL BALANCE FOR PRODUCT: Propanoic acid Kg Propyl propionate Kg Propanol Kg Water ( Reuse) Kg Evaporation loss 48.0 Kg Total Kg Total Kg FLOW DIAGRAM Propanoic acid Kg Propanol Kg 1903 kg Heat & reflux Cool & water separation 255 Kg Water is reused in process. Distill the material & Pack 1600 Kg 12
13 10. Chloro Methyl Naphthalene in toluene Charge naphthalene, paraformaldehyde and HCl (34%) in reactor. Heat to 80 0 C and maintain till reaction completes. Cool the reaction mass and settle and separate the HCl (22%) layer to other vessel. Charge Toluene to remaining reaction mass to make 1 chloro methyl naphthalene 80% finish product. Pack it to HDPE Drum. CH 2 Cl (CH 2 O) n HCl H 2 O Napthalene p-formaldehyde Hydrochloric Gas 1 Chloro methyl Naphthalene Water MATERIAL BALANCE FOR PRODUCT: Naphthalene Kg 1 Chloro Methyl Naphthalene in toluene Kg Para Formaldehyde Kg HCl (22%) Kg HCl (34%) Kg Toluene Kg Total Kg Total Kg Naphthalene Kg Paraformaldehyde Kg HCl (34%) Kg Reaction mass Mix heat & Cool Separation HCl (22%) Kg Toluene 800 Kg Packing Kg 1 Chloro Methyl Naphthalene sale with toluene 13
14 11. N-Ethyl-2-nitromethylenepyrrolidine Charge NE2P,DMS, Sodium methoxide & Nitro methane in reactor. Mix and maintain the reaction mass at 25 C for 8 hrs. Charge Dichloro methane to the reactor & separate out remaining methanol. Distill out dichloro methane completely. Add toluene to reactor.mix the reaction mass. Centrifuge the mass and dry the wet cake. Pack the dry material in bags as finish product. C 6 H 11 NO + C 6 H 6 O 4 S + 2CH 3 NaO + CH 3 NO 2 C 7 H 12 N 2 O 2 + Na 2 SO 4 + 2CH 3 OH + C 2 H 6 O NE2P DMS sodium nitro NE2NMP sodium methanol DME Methoxide methane sulphate MATERIAL BALANCE FOR KG PRODUCT: 1-ethyl-Z-pyrrolidinone Kg N-ethyl-2-nitromethylenepyrrolidine Kg Methanol dimethyl sulfate Kg 350 kg methanol recovery, 20 kg evaporation loss, 122 kg dimethyl ether Kg sodium methoxide Kg 377 kg sodium sulphate, 73 kg impurity Kg nitromethane Kg MDC 1120 kg recovery, 60 kg evaporation loss Kg MDC Kg Toluene ML 140 kg toluene, 40 kg NE2NMP, 20 kg MDC Kg Toluene Kg Drying loss 45.0 Kg Total Kg Total Kg 14
15 FLOW DIAGRAM: NEAP 300 Kg DMS Kg Sodium methoxide 486 Kg Nitro methane 220 Kg 1342 kg Mix heat & Cool & MeOH recovery MDC 1200 kg 2542 kg seperation & MDC recovery 942 kg Methanol layer 1120 kg MDC Recovery, 60 kg evap. loss Toluene- 150 kg 570 kg Mix Centrifuge 200 kg toluene ML (to be recover & reuse) Wet cake 370 KG Drying 45 kg evaporation loss 325 kg Packing 15
16 12. BARBITURIC ACID Charge methanol to reactor then charge sodium metal to it lot wise while chilling water circulation to jacket.mix the mass. Now charge diethyl melonate & urea to it.heat the reaction mass to C & maintain for 8 hours.distill out methanol completely.now charge water & then HCl to the reaction mass to recrystallize the product. Centrifuge the mass and dry the wet cake. Pack the dry material in bags as finish product. C 7 H 12 O 4 + CH 4 N 2 O + CH 3 ONa + HCl C 4 H 4 N 2 O 3 + 2C 2 H 6 O + CH 3 OH + NaCl Diethyl Urea sodium Hydrochloric Barbituric Ethanol Methanol Sodium malonate Methoxide Acid Acid Chloride MATERIAL BALANCE FOR KG PRODUCT: Methanol Kg Barbituric acid Kg Mix solvent sodium 85.0 Kg 2102 kg methanol,275 kg ethanol, 125 kg evaporation loss Kg Diethyl melonate Kg Mother Liquor 1245 kg water, 359 kg HCl, 194 kg sodium chloride Kg urea Kg Drying Loss 80.0 Kg Water HCl Kg Kg Total Kg Total Kg 16
17 FLOW DIAGRAM: Methanol 2176 Kg sodium - 85 Kg Diethyl melonate 531 Kg Urea 208 Kg 3000 kg Mix heat & Cool & MeOH recovery 2502 kg Methanol+ethanol Recovery water 1260 kg HCl 480 kg 2238 kg Chilling & Recrystelliza tion Centrifuge 1798 kg ML separation by dist. process Wet cake 440 KG Drying 80 kg evaporation loss 360 kg Packing 17
18 13. N-METHYL-1-NAPHTHALENE-METHANEAMINE Step-1: Charge N,N-Dimethylformamide to reactor then charge sodium hydride (50% inparafin oil) to it lot wise while chilling water circulation to jacket.mix the mass. Now charge N-methyl formamide to it. Maintain the reaction mass at C. Now charge 1- chloromethylnaphthalene solution in toluene. Maintain the reaction mass at C.Once the reaction is over quench the mass to water. Add toluene to reaction mass & extract with toluene. Separate organic layer & distill out toluene completely to get N-methyl-N- (1-Naphthylmethyl)-formamide which is directly used in next step. Step-2: To the reactor containing N-methyl-N-(1-naphthylmethyl)-formamide charge 20% aqueous sodium hydroxide and heated at C for a period of 7hr. Cool the reaction mass and extract with toluene. Separate organic layer and extract with Hydrochloric acid. Decolorize the aqueous layer with activated charcoal. Filter the mass & collect the filtrate. Add 20% aqueous sodium hydroxide and toluene to it. Separate the organic layer. Distill out toluene completely to get Methyl-1-naphthalene-methaneamine. Pack to carboys. Step-1 C 11 H 9 Cl + C 2 H 5 NO + NaH C 13 H 13 NO + NaCl + H 2 1-chloromethyl N-methyl Sodium N-methyl-N-(1-naphthyl Sodium Hydrogen naphthalene formamide hydride methyl)-formamide chloride MATERIAL BALANCE FOR KG PRODUCT: 1-chloromethyl naphthalene Kg N-methyl-N-(1-Naphthylmethyl)-formamide Kg Aqueous layer N-methyl formamide 50.0 Kg 500 kg water, 236 kg DMF, 16 kg paraffin oil, 33 kg sodium chloride Kg Sodium hydride (50% in 32.0 Kg parafin) Toluene recovery Kg N,N-Dimethylformamide Kg Evaporation Loss 26.0 Kg Toluene Kg Hydrogen gas 1.0 Kg Water Kg Total Kg Total Kg 18
19 FLOW DIAGRAM: DMF 236 Kg Sodium hydride - 32 Kg ( 50% in paraffin oil) N-methyl formamide 50 Kg 1-CMN 100 Kg Toluene 86.5 Kg kg Mix heat & Cool 1 kg Hydrogen gas evolved water 500 kg toluene kg 1436 kg layer separation 785 kg Aq. Layer separation by dist. Process. 651 kg Distillation 519 kg toluene recovery 132 kg Stage Kg N-methyl-N-(1-Naphthylmethyl)-formamide directly used in next stage 19
20 14. VERATRALDEHYDE Vishwa Chemicals Charge water and vanillin to reactor. Add sodium hydroxide and dimethyl sulfate.mix the reaction mass. Add sulphuric acid to the reaction mass.once the reaction completes settle down the mass for one hour. Discard the water layer and crystallize the organic layer. Centrifuge the mass & dry it. Pack the product. C 8 H 8 O 3 + 2NaOH + (CH 3 )2SO 4 C 9 H 10 O 3 + CH 3 OH + Na 2 SO 4 + H 2 O Vanillin Sodium Dimethyl Veratraldehyde Methanol Sodium Water hydroxide sulphate sulphate MATERIAL BALANCE FOR KG PRODUCT: Vanillin Kg 3,4-dimethoxybenzaldehyde Kg Aquous Layer Water Kg 65 kg methanol,304 kg sodium sulphate, 590 kg water, 50kg sulphuric acid Kg Sodium hydroxide Kg Mother Liquor 10 kg water, 2 kg methanol, 25 kg 3,4- dimethoxybenzaldehyde 37.0 Kg Dimethyl sulphate Kg Drying Loss 42.0 Kg Sulphuric Acid-50% 52.0 Kg Total Kg Total Kg 20
21 FLOW DIAGRAM: Vanillin 325 Kg Water Kg Sodium hydroxide 171 Kg Dimethyl sulphate 269 Kg 1336 kg Mix & heat Sulphuric acid 52 Kg 1388 kg Mix, Settle & Seperate Aq layer-1009 Kg separation by dist. process Centrifuge 3 7 kg ML Wet cake 342 KG Drying 42 kg evaporation loss 300 kg Packing 21
22 15. Solvent distillation (MDC, Methanol, toluene, acetone, IPA, ethyl acetate,thf,n-hexane) Condenser Dist. Solvent Solvent from Process Reactor 22
23 Annexure-III Water Consumption and Waste water generation Details Sr. No Source Water consumption kl/day Waste water generation kl/day 1. Domestic Gardening Industrial Source of water supply : GIDC supply 2. Domestic effluent will be disposed through septic tank/ soak pit system Sr. No Stack attach to Stack Height (Mtr) Fuel Used 1. Boiler 9.0 Natural Gas 2. Process Stack(From reactors and vacuum pump outlet) Annexure-IV Detail of Air Pollution Fuel APCM Pollutants Consumption rate 300 M 3 /day N.A. SPM < 150 mg/nm Dip pipe in to water and then passes through chiller SO 2 < 100 ppm NOx < 50 ppm ---- Annexure-V Hazardous Waste Details Sr. No Type of Waste Category of Waste Quantity Method of Disposal 1 Discarded Containers/ Barrels/ Liners MT/Year Collection, Storage, Transportation and disposal by selling to registered recycler. 2 Used oil Lit/Hr Collection, Storage, Sale to registered recycler / reuse for machine lubricants. 3. Distillation Residue MT/month Collection, storage, reuse, disposal by CHWIF 23
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