Product: Isosorbide - environmentclearance.nic.inenvironmentclearance.nic.in/writereaddata/FormB/TOR/ConceptualPlan/28_Apr_2017... · Diluted Isosorbide-5-Mononitrate Blending Equipment

Product: Isosorbide

+ 2 H2O

Sorbitol Isosorbide

Name Empirical Formula Mol. Weight

Sorbitol C6H14O6 182 Liquid

Isosorbide C6H10O4 146 Solid

Water 2H2O 36 Liquid

Product: Isosorbide Flow Diagram

2.5 kg Sorbitol 70% solution 1.08 kg Isosorbide

0.02 kg p-Toluene Sulphonic Acid 1.1 kg water to ETP

0.01 kg Sodium acetate anhydrous 0.35 kg distillation residue to CHWTSDF

5000 L SS, 170-220 C

1.08 kg Isosorbide 1 kg Isosorbide (Product)

0.05 litres Methanol 0.12 kg ML to ETP

48” SS Centrifuge Equipment Washing: 2 litres per kg

dehydration

p-Toluene Sulphonic Acid

Dehydration Distillation

Washing Centrifuging

Production capacity: 5 MT/month

Waste Type Quantity/kg Quantity in KL per month

Quantity in KL per day

Treatment

Effluent Liquid 3.22 kg 16.1 0.536 To ETP

Distillation Residue Solid 0.35 kg 1.75 0.058 To CHWTSDF

Gaseous emissions Water vapour 0.10 kg 0.5 0.017 To atmosphere

Equipment and Utilities:

1. 5000 L SS Distillation Unit 2. Thermopack: 250000 kcal/hr 3. 48” SS Centrifuge

Product: Diluted Isosorbide Dinitrate

+ 2 H2O

Sorbitol Isosorbide

2HNO3

Lactose

+ 2 H2O Diluted Isosorbide Dinitrate Blending

Isosorbide Dinitrate




Nitric Acid HNO3 63 Liquid

Sulphuric Acid H2SO4 98 Liquid

Isosorbide Dinitrate C6H8N2O8 236 Solid

H2SO4

dehydration


Product: Diluted Isosorbide Dinitrate Flow Diagram (Pure

Product- 6 MT/M)




5000 L SS, 170-220 C

1.08 kg Isosorbide 1 kg Isosorbide


48” SS Centrifuge

1 kg Isosorbide 0.1 kg vapor loss to scrubber

2 kg HNO3 70% + 0.25 kg HNO3 98%

4 kg Sulphuric Acid Reaction Mass

800 L SS, 5-15 C

36.05 kg Sulphuric Acid + 30 litres water Unreacted isosorbide and Su Nitric Acid + Water to ETP

2500 L SS, 10-15 C 1.1 kg ISDN Crude

1 kg ISDN pure

0.66 kg Acetone 10.76 kg Effluent to ETP

10 litres water

2500 L SS, Ambient, 50 C

ISDN pure Diluted Isosorbide

Lactose Dinitrate

SS Pulverizer and Mixer

Equipment washings: 10 litres per kg of product



Nitration

Precipitation Washing &

drying

Purification & Drying

Pulverizing Blending

Production capacity: 15 MT/month of Diluted Isosorbide Dinitrate (6 MT/M Pure Product)

Waste Type Quantity/kg Quantity in KL per month

Quantity in KL per day

Treatment

Effluent Liquid 58.03 kg 348.18 11.60 To ETP (15% TDS)


Gaseous emissions Water vapour + reaction vapours

0.10 kg 0.6 0.02 To scrubber

Equipment and Utilities: 1. 5000 L SS Distillation Unit 2. Thermopack: 250000 kcal/hr 3. 48” SS Centrifuge 4. 800 L SS Reactor 5. 10 TR Chiller (Glycol) 6. 2500 L SS Reactor 7. SS Dryer 8. SS Pulverizer 9. SS Mixer 10. Steam boiler: 200 kg/hr 11. Nutch filter

Product: Diluted Isosorbide-5-Mononitrate

+ 2 H2O

Sorbitol Isosorbide

CH3COONa (CH3CO)2O

HNO3 (CH3CO)2O

Isosorbide-2-Acetate-5-Nitrate + CH3COOH Isosorbide-2-Acetate

+ CH3COOH

NaOH CH3ONa

Lactose Diluted Blending Isosorbide-5-Mononitrate Isosorbide-5-Mononitrate + CH3COONa

dehydration





Acetic Anhydride (CH3CO)2O 102 Liquid

Isosorbide-2-Acetate C8H12O5 188 Soid

Acetic Acid CH3COOH 60 Liquid


Isosorbide-2-Acetate-5-Nitrate

C8H11O7N 233 Solid

Sodium Hydroxide NaOH 40 Solid

Sodium Methoxide CH3ONa 54 Solid

Sodium Acetate CH3COONa 82 Solid

Isosorbide-5-Mononitrate

C6H9O6N 191 Solid

Product: Diluted Isosorbide-5-Mononitrate Flow Diagram




2500 L SS, 170-220 C 1.4 kg Isosorbide 1.29 kg Isosorbide

0.05 litres Methanol 0.15 kg ML to ETP 48” SS Centrifuge

1.29 kg Isosorbide 1.29 kg Isosorbide-2-Acetate

0.95 kg Acetic Anhydride 0.26 kg Acetic Acid (by-product) to sale


2500 L SS, 100-170 C



Acetylation Distillation

1.29 kg Isosorbide-2-Acet 1500 L SS, 5-15 C 0.2 kg vapor loss to scrubber

1.43 kg Acetic Anhydride

0.57 kg Nitric Acid 98% 3.09 kg Reaction Mass

8.18 kg Effluent to ETP 0.45 kg Methylene Chloride + 4.9 kg recycled MeCL2 0.04 kg Spent charcoal to CHWTSDF 7.1 litres water + 0.04 kg charcoal 7.36 kg Reaction mass

MeCl2 Extract

4.9 kg MeCl2 (reuse) 40-50 C, 8 hrs

2.01 kg Reaction Mass & 0.45 MeCl2 loss to scrubber

2.23 kg Methanol (reuse for 10 batches ) 2.4 kg Methanol + 0.04 kg Charcoal 0.04 kg Spent Charcoal to CHWTSDF 0.035 kg Sodium Methoxide 1.75 kg Reaction Mass + 0.465 kg to scrubber 12.1 kg Toluene (reuse) + 0.2 kg losses 0.15 kg Reaction 12.3 kg Toluene 70 C , 3 hr Waste

1.6 kg ISMN Crude

2.2 kg Water to ETP

1 kg ISMN 2.4 kg Water 0.8 kg evaporation loss to scrubber SS Crystallizer, SS Centrifuge, SS Dryer, SS Pulverizer, SS Mixer

Lactose Diluted Isosorbide-5-Mononitrate

Blending

Equipment washings: 25 litres per kg of product

Nitration

Extraction 3000 L SS, 10 C

Distillation 2000 L SS

Extraction 2500 L SS

Recrystallization Drying

Distillation 2000 L SS

50-60 C,8Hrs

Production capacity: 13 MT/month of Pure Isosorbide Mononitrate

Waste Type Quantity/kg Quantity in MT per month

Quantity in MT per day

Treatment



Solid Hazardous Waste

Solid 0.15 kg 1.95 MT 0.065 To CHWTSDF

Gaseous emissions Water vapour + Solvents +

reaction vapours

1.315 kg 17 0.569 To scrubber

By products Acetic Acid 0.26 3.38 0.1126 Sale to authorized

dealer

Equipment and Utilities:

1. 5000 L SS Distillation Unit 2. Thermopack: 250000 kcal/hr 3. 48” SS Centrifuge 4. 2500 L SS Distillation Unit 5. 1500 L SS Reactor 6. 10 TR Chilling Unit (Glycol) 7. 3000 L SS Reactor 8. 2000 L SS Distillation Unit 9. 2500 L SS Distillation Unit 10. 1000 L SS Reactor 11. SS Crystallizer 12. 36” SS Centrifuge 13. SS Dryer 14. SS Pulverizer 15. SS Mixer 16. Sparkler filter/Nutch filter 17. Steam boiler: 400 kg/hr

Product: Dimethyl Isosorbide

+ 2 H2O

Sorbitol Isosorbide

2NaOH (CH3)2SO4

Dimethyl Isosorbide

+ Na2SO4 + 2 H2O




Dimethyl Sulphate (CH3)2SO4 126 Liquid

Sodium Hydroxide NaOH 40 Solid

Dimethyl Isosorbide C8H14O4 174 Liquid

Sodium Sulphate Na2SO4 142 Solid

dehydration


Product: Dimethyl Isosorbide Flow Diagram




5000 L SS, 170-220 C

1.08 kg Isosorbide 1 kg Isosorbide


48” SS Centrifuge

1 kg Isosorbide 0.1 kg losses to scrubber 1.26 kg Sodium Hydroxide 3 kg Dimethyl Sulphate 2500 L SS 2.05 kg water 70 C (ETR) Reaction Mixture

12.11 kg ML to ETP 6 kg water 3.6 kg Methylene Chloride 4.7 kg Extract in MeCl2 2500 L SS, 25-30 C 3.3 kg MeCl2 for reuse + 0.3 losses to scrubber 2500 L SS 40-50 C 10 hrs 1.1 kg Crude Dimethyl Isosorbide

1 kg Dimethyl Isosorbide 0.1 kg Distillation Residue 1500 L SS, 120-130 C 6 hrs

Equipment washings: 7 litres per 1 kg of Dimethyl Isosorbide



Methylation

Extraction

Distillation

High Vacuum Distillation

Production capacity: 5 MT/month of Dimethyl Isosorbide



Treatment



Gaseous emissions Water vapour and reaction

vapours

0.4 kg 2 0.06 To scrubber

Equipment and Utilities: 1. 5000 L SS Distillation Unit 2. Thermopack: 250000 kcal/hr 3. 48” SS Centrifuge 4. 2500 L SS Distillation Unit 5. 1500 L Distillation Unit

Diluted Nitroglycerin

Product: Diluted Nitroglycerin (1.5 MT Pure)

+ 3H2O


Glycerin C3H8O3 92 Liquid


Sulphuric Acid H2SO4 98 Liquid

Nitroglycerin C3H5N3O9 227 Liquid

Product: Diluted Nitroglycerin Flow Diagram

0.75 kg Glycerin 1 kg Nitroglycerin

1.31 kg HNO3 70 % + 0.56 kg HNO3 98% 0.05 kg Losses to scrubber

2.8 kg Sulphuric Acid 104.57 kg ML to ETP

100 kg Water Washing

0.2 kg CaCl2

Blending with Lactose

Equipment: 5 L Glass Reactor, 5-10 C

Equipment washings: 2 litres per kg of Nitroglycerin

HNO3 / H2SO4

Glycerin

5 - 10ºC

Nitroglycerin

Nitration

Production capacity: 25 MT/month of Diluted Nitroglycerin



Treatment


Gaseous emissions Reaction vapours

0.05 kg 0.075 0.0025 To scrubber

Equipment and Utilities: 1. 5 L Glass Reactors 2. Chilling Unit: 5 TR (Glycol) 3. SS Mixer

Product: Carbimazole

CH3OH, Soda ash

+ Br2 + CH3COOCH3 + CH3OH Vinyl acetate Bromoacetaldehyde Dimethyl acetal

CH3OH CH3NH2

KOH

+ CH3OH

(Methylamino)acetaldehyde Dimethyl acetal

Acetone NH4SCN

Mercazole (Methimazole)

Pyridine ClCOOC2H5 Acetone

Carbimazole


Vinyl acetate monomer C4H4O2 86 Liquid

Bromine Br2 159.8 Liquid

Methanol CH3OH 32 Liquid

Bromoacetaldehyde Dimethyl Acetal (BAMA)

BrCH2CH(OCH3)2 169 Liquid

Methyl Acetate CH3COOCH3 74 Liquid

Monomethyl Amine CH3NH2 31 Gas

(Methylamino)acetaldehyde Dimethyl Acetal (MAMA)

CH3NHCH2CH(OCH3)2 119 Liquid

Potassium Bromide KBr 89.9 Solid

Ammonium Thiocyanate NH4SCN 76 Solid

Mercazole (Methimazole) C4H6N2S 114 Solid

Ethyl Chloroformate ClCOOC2H5 108.5 Liquid

Carbimazole C7H10N2O2S 186 Solid

Pyridine C5H5N 79.1 Liquid

Acetone CH3COCH3 58 Liquid

Product: Carbimazole Flow Diagram

6.64 kg Vinyl Acetate Monomer 5.64 kg BAMA 12.5 kg Bromine 3 kg Methyl acetate 12.1 kg Methanol 8 kg Methanol recycle 2.14 kg Soda Ash 81.14 kg Aqueous Effluent to ETP

71.4 kg Water 7 kg Sodium Bromide to ETP

5.64 kg BAMA 1.975 kg MAMA 10.78 kg MMA 40% solution 10.23 kg Methanol recycle 6.32 kg Methanol 25.83 kg Effluent to ETP 8.3 kg KOH 3 kg Potassium Bromide to ETP

10 kg water

1.975 kg MAMA 0.98 kg Mercazole 0.93 kg Acetone 1.18 kg Ammonium Thiocyanate Distillate Acetone ML for product

recovery

0.98 kg Mercazole 1.25 kg Carbimazole crude 1.16 kg Ethyl chloroformate 12.71 kg effluent to ETP 0.86 kg Pyridine 3.10 kg Acetone

7.86 kg Water

1.25 kg Carbimazole crude 1 kg Carbimazole 0.18 kg charcoal Spent Charcoal 0.18 kg 7.14 kg Acetone Acetone ML for recovery

Equipment washings: 15 litres per kg of carbimazole

Bromination

Amination

Cyclization

Esterification

Purification

Production capacity: 2.5 MT/month of Carbimazole



Treatment

Effluent Liquid 145 kg 362.5 12 To ETP

Solid Waste Spent Charcoal

0.18 0.45 0.015 To CHWTSDF

Equipment and Utilities: 1. 50 L Glass Distillation Units – 15 Nos. 2. Thermopack: 50000 kcal/hr 3. Chilling unit: 5 TR (Glycol) 4. 24” SS Centrifuge 5. SS Dryer 6. SS Pulverizer 7. SS Mixer

Product: Methimazole

CH3OH, Soda ash

+ Br2 + CH3COOCH3 + CH3OH Vinyl acetate Bromoacetaldehyde Dimethyl acetal

CH3OH CH3NH2

KOH

+ CH3OH

(Methylamino)acetaldehyde Dimethyl acetal

Acetone NH4SCN

Mercazole (Methimazole)

Product: Methimazole Flow Diagram

7.75 kg Vinyl Acetate Monomer 6.58 kg BAMA 14.58 kg Bromine 3.5 kg Methyl acetate 14.2 kg Methanol 9.33 kgMethanol recycle 2.5 kg Soda Ash 94.7 kg Aqueous Effluent to ETP

83 kg Water 7.92 kg Sodium Bromide

6.58 kg BAMA 2.30 kg MAMA 12.58 kg MMA 40% solution 11.93 kg Methanol recycle 7.375 kg Methanol 28.46 kg Water to ETP 9.67 kg KOH 3.51 kg Potassium Bromide

10 kg Water

2.30 kg MAMA 1.15 kg Methimazole crude 1.08 kg Acetone 1.38 kg Ammonium Thiocyanate Distillate Acetone ML for product

recovery

1.15 kg Methimazole crude 1 kg Methimazole 0.21 kg charcoal Spent Charcoal 4.6 kg Acetone Acetone ML for recovery

Equipment washings: 15 litres per kg of methimazole

Bromination

Amination

Cyclization

Purification

Production capacity: 2.5 MT/month of Methimazole



Treatment


Solid Waste Spent Charcoal

0.2 0.5 0.016 To CHWTSDF

Equipment and Utilities: 8. 50 L Glass Distillation Units – 12 Nos. 9. Thermopack: 50000 kcal/hr 10. Chilling unit: 5 TR (Glycol) 11. 24” SS Centrifuge 12. SS Dryer 13. SS Pulverizer 14. SS Mixer

Other utilities:

1. Cooling towers: 100 TR x 1, 150 TR x 1, 50 TR x 1

2. Process Scrubbers – As and where required

3. RO Water Systems: 2 x 2000 litres/hour

4. Air Handling Units (with temperature and humidity control): Section-wise for each production block

5. Generator(s)

6. Backup chilling system: 10 TR (Glycol)

7. Fire fighting system with main pump, booster pumps and diesel powered backup pump

Storage Tanks:

1. Underground Storage tanks for Methanol and Toluene-

2. Water tank for fire fighting system-

3. Process Water tank

4. Domestic Water tank

Documents

Product: Isosorbide - environmentclearance.nic.inenvironmentclearance.nic.in/writereaddata/FormB/TOR/ConceptualPlan/28_Apr_2017... · Diluted Isosorbide-5-Mononitrate Blending Equipment