c) Summary of mass balance - Gujarat Pollution Control...

Rapid Environmental Impact Assessment Report Page : 51 of 294 Chapter-2 Project Description

c) Summary of mass balance

Summary of mass balance for 4–Piperidone Hydrochloride is given in Table.

Summary of Mass Balance for – 4-Piperidone Hydrochloride

capacity of Finished Product MT/Month : 10.00

batch size kg : 20

Working Days Per Month : 26

Quantity Sr. No. Name of Raw Material

Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Piperidone Monohydrate Hydrochloric Acid

25 0.23 2.27

2 Acetone 15 0.14 1.36 Reactant

3 Toluene (Fresh) 15 0.14 1.36

4 Toluene (Recovered) 185 1.68 16.82 Solvent

Total 240 2.18 21.82

Output

1 4-Piperidone Hydrochloride 20 0.18 1.82 Finished Product

2 Rec Toluene 185 1.68 16.82 Recovered Solvent

3 Waste acetone 10 0.09 0.91

4 Waste Water 10 0.09 0.91 To ETP

5 Touene Loss 15 0.14 1.36 To Atm Total 240 2.18 21.82


(A-13) Piperidone Mono Hydrate HCl

a) Material Balance Diagram:

Reaction Vessel

Liquid – Liquid Extraction

Distillation

N –Hexane (Fresh): 100 N –Hexane

(Recovered): 1400

Distilled mass

Heating followed by Cooling

Continue…….

Heating followed by Cooling Caustic Lye: 150

N-Carbethoxy-4-Piperidone: 200

Tri methyl ortho formate: 150

Methane sulfonic acid: 120 Methanol (Fresh): 300

Methanol (Recovered): 300

Aqueous Layer (Effluent): 1200

N –Hexane Recovered: 1400

Distillation Loss: 100 Distillation Residue: 10 Methanol Recovered:

600

N –Hexane & Methanol Recovery

Methanol (Fresh): 300 Methanol (Recovered):

300 Caustic Lye Solution:

100

Chloroform (Fresh): 100 Chloroform

(Recovered): 1100 Purified Water: 1400

Liquid – Liquid extraction & Layer

separation


CO2: 60


Organic Layer Chloroform Recovery

Chloroform Recovered: 1100

Distillation Loss: 100 Distillation Residue: 10

High vaccum Distillation of

Crude 4-Piperidone

Distillation Loss:

Distillation Residue: 30

Reaction mass IPA: 450 HCl: 300

Cooling, Chilling & Centrifuge M/L as waste: 50

Piperidone Mono Hydrate HCl

(Finished Product)

IPA Recovered: 400


b) Reaction Chemistry

Chemical Formula

Chemical Name

N

O

COOEt

+ NaOH SolutionWater

Chloroform HCl N

H

O

HCl

+ C2H5OH CO2+

N-Carbethoxy 4-PIperidone 4-Piperidone Hydrochloride

Molecular Weight

171 40 135.5 46 44


Summary of mass balance for Piperidone Mono Hydrate HCl is given in Table .

Summary of Mass Balance for – Piperidone Mono Hydrate HCl


batch size kg : 110



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 N-Carbethoxy-4-Piperidone 200 1.82 18.18

2 Tri methyl ortho formate 150 1.36 13.64

3 Methane sulfonic acid 120 1.09 10.91

4 Caustic Lye 250 2.27 22.73

5 Water 1400 12.73 127.27

Reactant

6 Methanol (Fresh) 600 5.45 54.55

7 Methanol (Recovered) 600 5.45 54.55

8 N-Hexane (Fresh) 100 0.91 9.09

9 N-Hexane (Recovered) 1400 12.73 127.27

10 Chloroform (Fresh) 100 0.91 9.09

11 Chloroform (Recovered) 1100 10.00 100.00

12 Hydrochloric Acid 300 2.73 27.27

Solvent



Kg/Batch Kg/Kg

ofProduct

MT/MonthRemarks

Input

13 Iso Propyl Alcohol (Fresh) 50 0.45 4.55

14 Iso Propyl Alcohol (Recovered)

400 3.64 36.36

Total 6770 61.55 615.45

Output

1 4-Piperidone Monohydrtae Hydrochloride

110 1.00 10.00 Finished Product

2 Effluent with ethanol & Methanol

2200 20.00 200.00 To ETP

3 Residue after distillation 50 0.45 4.55 To TSDF

4 Rec Methanol 600 5.45 54.55

5 Rec Iso Propyl Alcohol 400 3.64 36.36

6 Rec Chloroform 1100 10.00 100.00

7 Rec N-Hexane 1400 12.73 127.27

8 Carbon Di oxide 60 0.55 5.45

9 Iso Propyl Alcohol Loss 50 0.45 4.55

10 N-Hexane Loss 100 0.91 9.09

11 Chloroform Loss 100 0.91 9.09

12 Methanol Loss 600 5.45 54.55

Total 6770 61.55 615.45

Recovered Solvent


(A-14) 4-Piperidone ethylene Ketal


Reaction Vessel N-Carbethoxy-4-

Piperidone: 100 Para Toluene Sulphonic

acid: 110 Mono Ethylene Glycol:

200 Methane sulfonic acid: 90

Toluene (Fresh): 70 Toluene (Recovered): 450

Azeotropic Distillation

Organic Layer

Heating


Cooling of Distilled mass & Layer

separation

Water: 200 Aqueous Layer (Effluent): 490

IPA: 240 KOH Soln in IPA: 95

Toluene Recovery: 450

IPA Recovery: 200

Layer separation of Reaction mass

Water: 95 Chloroform (Fresh): 100

Chloroform (Recovered): 500

Organic Layer Chloroform Recovery: 500

High Vaccum Distillation

Distillation Loss: 210


4-Piperidone ethylene Ketal (Finished Product)



Stage –I

Chemical Formula

Chemical Name

+N

OO

COOEtN -Carbethoxy 4-Piperidone N-Carbethoxy4-Piperidone Ethylene K

N

COOEt

O

OH OH

Mono ethylene glycol

+ H2O

Toluene

MSA

Molecular Weight

171 62 215 18

Stage –II

Chemical Formula

Chemical Name N

H

OO

N-Carbethoxy4-Piperidone Ethylene Ketal

+ C2H5OHN

OO

COOEt

IPA+ KOH

+ CO2

4- Piperidone Ethylene ketal

Molecular Weight

215 56 142 46 44

c) Summary of mass balance Summary of mass balance for 4-Piperidone ethylene Ketal is given in Table.

Summary of Mass Balance for – 4- Piperidone ethylene Ketal


batch size kg : 60




Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input


2 Para Toluene sulfonic acid 110 1.83 18.33

3 Methane sulfonic acid 90 1.50 15.00

4 Mono Ethylene glycol 200 3.33 33.33

Caustic Potash 95 1.58 15.83

Water 295 4.92 49.17

Reactant

5 Toluene (Fresh) 70 1.17 11.67

6 Toluene (Recovered) 450 7.50 75.00


9 Iso Propyl Alcohol (Recovered) 200 3.33 33.33



Solvent

Total 2250 37.50 375.00

Output

1 4-Piperidone ethylene ketal 60 1.00 10.00 Finished Product

2 Effluent with ethanol & methanol

790 13.17 131.67 To ETP

3 Rec Toluene 450 7.50 75.00


5 Rec Chloroform 500 8.33 83.33

Recovered Solvent

6 Toluene Loss 70 1.17 11.67


8 Chloroform Loss 100 1.67 16.67 To Atm

9 Residue after diatilation 40 0.67 6.67 To TSDF Total 2250 37.50 375.00


(A-15) N-Carbethoxy-4-Piperidone


Reaction Vessel N-Methyl-4-Piperidone:

500 Ethyl chloroformate: 600

Toluene (Fresh): 100 Toluene (Recovered):

1500

Organic Layer

Layer separation Water: 400 Aqueous Layer (Effluent): 650

Toluene Recovery: 1500


Distillation Loss: 100


550 kg of N Carbethoxy- 4-Piperidone (Finished Product)

Crude N-Carbethoxy- 4-

Piperidone

Chloro methane: 240



Stage –I

ChemicalFormula

ChemicalName

N OCH3 N O

O

C2H5

O+ ClCO2CH2CH3 + CH3Cl

Toluene

Water

N-Methyl 4-Piperidone Ethyl ChloroFormate N-Carbethoxy 4-Piperidone Methyl chlorid

MolecularWeight

113 108.5 171 50.5


c) Summary of mass balance Summary of mass balance for N-Carbethoxy-4-Piperidone is given in Table .

Summary of Mass Balance for – N-Carbethoxy-4- Piperidone


batch size kg : 500



Kg/Batch Kg/Kg

ofProduct

MT/MonthRemarks

Input

1 N-Methyl-4-Piperidone 500 1.00 10.00

2 Ethyl chloroformate 600 1.20 12.00

3 Water 350 0.70 7.00

Reactant

4 Toluene (Fresh) 100 0.20 2.00

5 Toluene (Recovered) 1500 3.00 30.00 Solvent

Total 3050 6.10 61.00

Output

1 N-Carbethoxy-4-Piperidone 500 1.00 10.00 Finished Product

2 Effluent 650 1.30 13.00 To ETP

3 Chloro methane 240 0.48 4.80



6 Toluene Loss 100 0.20 2.00 To Atm Total 3050 6.10 61.00


(A-16) N-BOC- 4 Carbethoxy-4-Piperidone


Reaction Vessel


Aqueous Layer

Chloroform (Fresh): 100 Chloroform

(Recovered): 500

Di BOC: 60

Organic Layer (Chloroform Recovery)

Chloroform Recovered: 500



Reaction mass & Extraction


Methanol Recovered: 40


Continue…….

N-Carbethoxy-4-Piperidone: 100

Caustic Lye: 125 Water: 600



450 Aqueous Layer

(Effluent): 500

Methanol Recovery

Crude N-T-Boc-4-Piperidone

Hexane (Fresh): 50 Hexane (Recovered):

350



Chemical Formula

Chemical Name

+((CH3)3COC(O))2O

N-Boc 4-CarbethoxyPiperidine

+NH

COOEt

N

COOEt

O O CH3

CH3CH3

4 -Carbethoxy piperidine

(CH3)3COC(O)OH

Molecular Weight 157 218 257

ML: 240

90 kg of N-BOC-4-Carbethoxy-4-Piperidone

(Finished Product)

Cooling, chilling, Filtration


c) Summary of mass balance Summary of mass balance for N-Boc-4-Carbethoxy-Piperidone is given in Table.Summary of Mass Balance for – N-Boc-4-Carbethoxy- Piperidone


batch size kg : 90



Kg/Batch Kg/Kg of Product MT/Month

Remarks

Input

1 N-Carbethoxy-4-Piperidone 100 1.11 11.11 Reactant

2 Methanol (fresh) 50 0.56 5.56

3 Methanol(Recovered) 450 5.00 50.00 Solvent

4 DI BOC 60 0.67 6.67

5 Caustic Lye 125 1.39 13.89 Reactant



8 N-Hexane (Fresh) 50 0.56 5.56

9 N-Hexane (Recovered) 350 3.89 38.89

Solvent

10 Water 600 6.67 66.67 --- Total 2385 26.50 265.00

Output

1 N-Carbethoxy BOC Piperidone


2 Rec Methanol 450 5.00 50.00 Recovered Solvent

3 Waste water 740 8.22 82.22 To ETP

4 Rec Chloroform 500 5.56 55.56

5 Rec N-Hexane 350 3.89 38.89 Recovered

Solvent

6 Solid waste after distillation 55 0.61 6.11 To TSDF

7 N-Hexane Loss 50 0.56 5.56


9 Methanol Loss 50 0.56 5.56 To Atm

Total 2385 26.50 265.00


(B-1) N-Methyl-4-Hydroxy Piperidine


14

14



Stage –I

ChemicalFormula

ChemicalName

N OCH3 N OHCH3

N-Methyl 4-Piperidone

+ H2 gasMethanol

N-Methyl 4-HHydroxy Piperidine

MolecularWeight

113 2 115


c) Summary of mass balance Summary of mass balance for N-Methyl-4-Hydroxy Piperidine is given in Table.

Summary of Mass Balance for – N-Methyl-4-Hydroxy Piperidine


batch size kg : 180



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 N-Methyl-4-Pipridone 200 1.11 11.11 Reactant

2 Water 500 2.78 27.78 ----

3 Raney Nickel 2 0.01 0.11 Catalyst

4 Toluene(Fresh) 14 0.08 0.78

5 Toluene(Recovered) 230 1.28 12.78 Solvent

6 Hydrogen Gas 10 0.06 0.56 Reactant Total 956 5.31 53.11

Output

1 N-Methyl-4-Hydroxy Piperidine 180 1.00 10.00 Finished Product

2 Filtered Raney Nickel 2 0.01 0.11

3 Distilled water 442 2.46 24.56 Reuse


5 Toluene Loss 14 0.08 0.78 To Atm


7 Water Vapors 40 0.22 2.22

8 Toluene Vapors 28 0.16 1.56 To Atm

Total 956 5.31 53.11


(B-2) N-Methyl-4-Chloro Piperidine


900

900

3632



Stage –I

Chemical Formula

Chemical Name

N ClCH3N OHCH3 + SOCl2 + SO2 + HCl

N-Methyl 4-Hydroxy ThionylChloridePiperidine

N-Methyl 4-Chloro Piperidine

SulfurDioxide

Hydrochloriacid

MDC

MolecularWeight

115 119 133.5 64 36.5


c) Summary of mass balance Summary of mass balance for N-Methyl-4-Chloro Piperidine is given in Table.

Summary of Mass Balance for – N-Methyl-4-Chloro Piperidine -Processcapacity of Finished Product MT/Month : 10.00

batch size kg : 750


QuantitySr. No. Name of Raw Material

Kg/BatchKg/Kg

ofProduct

MT/Month Remarks

Input

1 N-Methyl-4-Hydroxy Piperidine 900.0 1.2 12.0 Reactant

2 Thionyl Chloride (Fresh) 875.0 1.2 11.7

3 Thionyl chloride (Recovered) 156.3 0.2 2.1

4 Methylene Di Chloride (Fresh) 62.5 0.1 0.8

5 Methylene Di Chloride (Recovered) 187.5 0.3 2.5

Solvent

6 DMF 18.8 0.0 0.3

7 Caustic Lye 900.0 1.2 12.0 Reactant

8 Water 2500.0 3.3 33.3 ----

9 N-Hexane(Fresh) 62.5 0.1 0.8

10 N-Hexane (recovered) 875.0 1.2 11.7 Solvent

Total 6538 8.72 87.17

Output

1 N-Methyl-4-Hydroxy Piperidine 750 1.0 10.0 Finished Product


3 Rec Methylene Di Chloride + Thionyl chloride 344 0.5 4.6 Reuse

4 SO2 gas 438 0.6 5.8

5 Hydrochloric Acid gas 313 0.4 4.2

ToScrubber


7 Methylene Di Chloride Loss 63 0.1 0.8 To Atm

8 Rec N-Hexane 875 1.2 11.7 Recovered Loss

9 N-Hexane Loss 63 0.1 0.8 To Atm Total 6538 8.72 87.18


Summary of Mass Balance N-Methyl-4-Chloro Piperidine - APCM


Kg/Batch Kg/Kg of Product MT/Month Remarks

Water scrubber Input

1 Water 1166.7 44.9 448.7 Scrubbing Media

2 Hydrochloric Acid Gas 312.5 12.0 120.2 To Scrubber Total 1479.2 56.9 568.9

Water scrubber Output

1 Hydrochloric Acid (30 %)

1479.2 56.9 568.9 Sale as By Product

Total 1479.2 56.9 568.9

Alkali scrubber Input

1 Caustic 446.4 17.2 171.7

2 Water 3273.8 125.9 1259.2 Scrubbing

Media

3 SO2 Gas 437.5 16.8 168.3 To Scrubber

Total 4157.7 159.9 1599.1

Alkali scrubber Output

1 Sodium Hypo Sulphite 4157.7 159.9 1599.1 Sale as By Product

Total 4157.7 159.9 1599.1


(B-3) 4-Hydroxy Piperidine



75

20

20

75


Stage –I

Chemical Formula

Chemical Name

N

OH

COOEt

N-Carbethoxy 4-Hydroxy Piperidine

+ NaOHWater

Chloroform NH

OH

4-Hydroxy Piperidine

+ C2H5OH + CO2

Ethanol CarbonDioxide

Sodium Hydroxide

MolecularWeight

173 40 101 46 44

c) Summary of mass balance Summary of mass balance for N-Hydroxy Piperidine is given in Table.

Summary of Mass Balance for – N-Hydroxy Piperidine


batch size kg : 60



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input


2 Water 500 8.33 83.33 Reactant


4 Hydrogen Gas 12 0.20 2.00 Reactant

5 Toluene(Fresh) 30 0.50 5.00 Solvent

6 Caustic Lye 160 2.67 26.67 Neutralizing Agent

7 Chloroform(Fresh) 75 1.25 12.50

8 Acetone(Fresh) 20 0.33 3.33

9 Toluene(Recovered) 220 3.67 36.67

10 Chloroform(Recovered) 825 13.75 137.50

11 Acetone(Recovered) 160 2.67 26.67

Solvent

Total 2204 36.73 367.33

Output

1 4-Hydroxy Piperidine 60 1.00 10.00 Finished


Product

2 Effluent with waste ethanol 677.5 11.29 112.92 To ETP

3 Raney Nickel 1.5 0.03 0.25 Reuse


5 Water Vapors 90 1.50 15.00 To Atm

6 Rec Toluene 220 3.67 36.67

7 Rec Acetone 160 2.67 26.67

8 Rec Chloroform 825 13.75 137.50

Recovered Solvent

9 Toluene Loss 30 0.50 5.00

10 Acetone Loss 20 0.33 3.33


To Atm

12 Carbon Di Oxide 15 0.25 2.50 To Atm Total 2204 36.73 367.33


(B-4) N-Carbethoxy-4-Hydroxy Piperidine


25

25

1

1



Stage –I

ChemicalFormula

ChemicalName

N

O

COOEt

+ H2 gas Water

N

OH

COOEt

N-Carbethoxy 4- Piperidone Hydrogen N-Carbethoxy 4-Hydroxy Piperidin

Molecular Weight

171 2 173

c) Summary of mass balance Summary of mass balance for N-Carbethoxy-4-Hydroxy Piperidine is given in

Table.

Summary of Mass Balance for – N-Carbethoxt-4-Hydroxy Piperidine


batch size kg : 170



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input 1 N-Carbethoxy-4-Piperidone 200 1.18 11.76 Reactant 2 Water 500 2.94 29.41 --- 3 Raney Nickel rec. 2 0.01 0.12 4 Hydrogen Gas 12 0.07 0.71 Catalyst 5 Toluene(Fresh) 25 0.15 1.47 Reactant 6 Toluene(Recovered) 200 1.18 11.76 7 Raney Nickel fresh. 1 0.01 0.06

Solvent

Total 940 5.53 55.29

Output 1 N-Carbethoxy-4-Hydroxy

Piperidine 170 1.00 10.00 Finished Product

2 Rec Water 402 2.36 23.65 Reuse


3 Raney Nickel 2 0.01 0.12 4 Residue after distillation 50 0.29 2.94 To TSDF 5 Water Vapors 90 0.53 5.29 To Atm 6 Rec Toluene 200 1.18 11.76 Recovered

Solvent7 Toluene Loss 25 0.15 1.47 8 Raney Nickel loss 1 0.01 0.06

To Atm

Total 940 5.53 55.29

(B-5) N-Carbethoxy-4-Chloro Piperidine a) Material Balance Diagram:



Stage –I

ChemicalFormula

ChemicalName

N

OH

COOEt

N-Carbethoxy 4-Hydroxy Piperidine

+ SOCl2

N

Cl

COOEt

4-Hydroxy Piperidine

+ ClH + SO2

HydroChloric SuphurDioxide

Thionyl Chloride

MDC

Water

Acid

Molecular Weight

173 119 191.5 36.5 64

c) Summary of mass balance Summary of mass balance for N-Carbethoxy-4-Chloro Piperidine is given in

Table.

Summary of Mass Balance for – N-Carbethoxt-4-Chloro Piperidine


batch size kg : 120



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 N-Methyl-4-Chloro Piperidine 100 0.83 8.33

2 Ethyl chloro formate 110 0.92 9.17 Reactant



5 Water 400 3.33 33.33 --- Total 2610 21.75 217.50

Output

1 N-Carbethoxy-4-Chloro Piperidine



3 Rec Toluene 1900 15.83 158.33 Recovered


Solvent


5 Residue after distillation 60 0.50 5.00 To TSDF Total 2610 21.75 217.50


(B-6) 4-Chloro Piperidine a) Material Balance Diagram:


Reaction Vessel (Hydrogenation)

Decantation

N-Methyl-4-Chloro Piperidine: 100

Ethyl Chloroformate: 110 Process water: 400 Ammonia Gas: 50

HCl : 500 Toluene(Fresh): 100

Toluene(Recovered): 1900

Layer separation

Crude 4-Chloro Piperidine


Toluene Loss: 100



Toluene recovered: 1900

Disti. 4- Chloro Piperidine

MDC (Fresh): 100 MDC (Recovered):

500

Cooling, Chilling & Filtration

Ethanol as waste: 27

Drying

30 kg of 4-Chloro Piperidine (Finished Product)


MDC Loss: 100

MDC Recovered: 500

Carbon dioxide: 22


Stage –I

ChemicalFormula

ChemicalName

N OH

O

O

CH3

N Cl

O

O

CH3

4 - CHLORO PIPERIDINE

NH Cl

Molecular Weight

160.190 178.63 132.61


c) Summary of mass balance Summary of mass balance for 4-Chloro Piperidine is given in Table.

Summary of Mass Balance for – 4-Chloro Piperidine


batch size kg : 30



Kg/BatchKg/Kg

ofProduct

MT/Month Remarks

Input


2 Ethyl chloro formate 110 3.67 36.67 Reactant

3 Toluene(Fresh) 100 3.33 33.33


5 Water 400 13.33 133.33 ----

6 Hydrochloric Acid 500 16.67 166.67 Reactant

7 Methylene Di Chloride(Fresh) 100 3.33 33.33

8 Methylene Di Chloride(Recovered)

500 16.67 166.67 Solvent

9 Ammonia Gas 50 1.67 16.67 Reactant Total 3760 125.33 1253.33

Output

1 4-Chloro Piperidine 30 1.00 10.00 Finished Product

2 Effluent 1056 35.20 352.00 To ETP



5 Rec Methylene Di Chloride 500 16.67 166.67 Recovered Solvent

6 Toluene Loss 100 3.33 33.33

7 Methylene Di Chloride Loss 100 3.33 33.33

8 Carbon di oxide 22 0.73 7.33 To Atm

9 Ethanol as waste 27 0.90 9.00 To ETP Total 3760 125.33 1253.33


(B-7) 4-Amino N-Benzyl-Piperidine




Stage –I

Chemical Formula

Chemical Name

N

O

+ MeOH N

NH2

N-Benzyl 4-Piperidone

NH3+H2 Gas

N-Benzyl 4-Amino Piperidine

+ H2O

MolecularWeight

189 32 17 189 18


c) Summary of mass balance Summary of mass balance for 4-Amino N-Benzyl Piperidine is given in Table .

Summary of Mass Balance for – 4-Amino N-Benzyl Piperidine


batch size kg : 180



Kg/Batch Kg/Kg

of Product

MT/Month Remarks

Input

1 N-Benzyl-4-Piperidone 200 1.11 11.11 Reactant

2 Methanol(Fresh) 40 0.22 2.22



5 Hydrogen Gas 12 0.07 0.67

6 Ammonia Gas 50 0.28 2.78 Reactant

Total 767 4.26 42.61

Output

1 N-Benzyl-4-Amino Piperidine 180 1.00 10.00 Finished Product


3 Raney Nickel 5 0.03 0.28 Reuse


5 Methanol Loss 40 0.22 2.22 To Atm Total 767 4.26 42.61


(B-8) 4-Hydroxy-N-Benzyl Piperidine a) Material Balance Diagram:



Stage –I

ChemicalFormula

ChemicalName

N O N OH+H2 GasMethanol

N-Benzyl 4-Piperidone N-Benzyl 4-HydroxyPiperidine

MolecularWeight

189 2 191


c) Summary of mass balance Summary of mass balance for 4-Hydroxy N-Benzyl Piperidine is given in Table.

Summary of Mass Balance for – 4-Hydroxy N-Benzyl Piperidine


batch size kg : 100



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 N-Benzyl-4-Piperidone 125 1.25 12.50 Reactant



4 Raney Nickel 2.5 0.03 0.25 Catalyst


Output

1 N-Benzyl-4-Hydroxy Piperidine 100 1.00 10.00 Finished Product


3 Raney Nickel 2.5 0.03 0.25 Reuse


5 Methanol Loss 100 1.00 10.00 To Atm Total 633 6.33 63.25


(B-9) 4-Benzamido Piperidine


Step-2

Chilling

Heating & TemperatureMaintaining

Purified Water:350 Reflux & Layer Seperation

Reaction Vessel Toluene:450

Sodium Carbonate:62.5 N-Carbethoxy-4-Amino

Pipridine:100

Benzoyl Chloride:110

Organic Layer

ML as Toluene

Aqueous Layer

Cooling & Centrifuge:

MethanolRecovery

RefluxMethanol(fresh):50

Methanol(Recoverd):350 Caustic Potash:75 Mass from step-1:

Purified Water:400 Cooling

Recovered Methanol:350

Drying

Step-1 Dry

Chloroform (Fresh): 125 Chloroform (Recovred): 500


Step-3

Heating

Filtration

Cooling and Stirring

Iso Propyl Alkohol(fresh):50 Iso Propyl

Alkohol(Recoverd):350 A.Carbon:

Step 2:

Cooling, Centrifuging, IPA recovery, Drying

50 Kg, 4-Benzamido Piperidine Pure

Recovered IPA350 IPA Loss:50

Manthol loss:50 Chloroform Loss): 125

HeatingHCl:

Filteration Activated Carbon:

Hyflow & Activated Carbon:22.5

Cool, Centrifuge, Water Wash

DryingEffluent:800 Ethanol mixed effluent ;625



Stage –I

Chemical Formula

Chemical Name

N

NH2

COOEt

O Cl

+N

NH

COOEt

O

N-Carbethoxy 4-amino PiperidineBenzoyl Chloride N-Carbethoxy 4-Benzamido Piperidine

Toluene+NaHCO3 +NaCl+ CO2+H2O

MolecularWeight

172 140.5 276 58.5 44 18

Stage –II

Chemical Formula

Chemical Name

N-Carbethoxy 4-Benzamido Piperidine

N

NH

COOEt

O

+ KOHIPA

NH

NH

O

4-Benzamido Piperidine

+ C2H5OH+CO2

.

MolecularWeight

276 56 203 46 44

c) Summary of mass balance Summary of mass balance for 4-Benzamido Piperidine is given in Table.

Summary of Mass Balance for – 4-Benzamido Piperidine


batch size kg : 50




Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 N-Carbethoxy-4-Amino Piperidine

100 2.00 20.00

2 Benzoyl chloride 110 2.20 22.00

3 Toluene 450 9.00 90.00

4 Sodium Carbonate 62.5 1.25 12.50

Reactant

5 Methanol fresh 50 1.00 10.00

6 Methanol Rec 350 7.00 70.00 Solvent


8 Chloroform Rec. 500 10.00 100.00 Solvent 9 Water 750 15.00 150.00 -10 Iso Propyl Alcohol fresh 50 1.00 10.00

11 Iso Propyl Alcohol recov 350 7.00 70.00

12 Chloroform Fresh. 125 2.50 25.00 Solvent

Total 2973 59.45 594.50

Output

1 4-Benzamido Piperidine 50 1.00 10.00 Finished Product

2 Carbon Di Oxide 22.5 0.45 4.50 To Atm

3 Ethanol mixed effluent 750 15.00 150.00

4 Effluent 900 18.00 180.00 To ETP


6 Rec Methanol 350 7.00 70.00 Recovered

Solvent

7 Solid waste after centrifuge 50 1.00 10.00 To TSDF

8 Rec Chloroform 500 10.00 100.00 Recovered Solvent

9 Chloroform loss 125 2.50 25.00

10 Methanol loss 50 1.00 10.00

11 IPA Loss 50 1.00 10.00 To Atm

Total 2973 59.45 594.50


(B-10) 4-Amino N-Carbethoxy Piperidine



Chemical Formula

Chemical Name

+ MeOH

N-Carbethoxyl 4-Piperidone

NH3+H2 Gas

N-Carbethoxy 4-Amino Piperidin

+ H2O

N

O

COOEtN

NH2

COOEt

MolecularWeight

171 32 17 171 18



Summary of mass balance for 4-Amino N-Carbethoxy Piperidine is given in

Table.

Summary of Mass Balance for – 4-Amino N-Carbethoxy Piperidine


batch size kg : 180



Kg/BatchKg/Kg

ofProduct

MT/Month Remarks

Input




4 Methanol rec 450 2.50 25.00 Solvent



Output



2 Rec Methanol+ Ammonia 480 2.67 26.67

3 Raney Nickel recyclable 3.5 0.02 0.19 Reuse

4 Residue after distillation 90 0.50 5.00 To TSDF Total 754 4.19 41.86


(B-11) 4-Amino N-Methyl Piperidine


b) Reaction Chemistry ChemicalFormula

ChemicalName

NCH3 OMethanolic ammonia

HydrogenatorNCH3 NH2

MolecularWeight

126.18 127.21

C) Summary of mass balance Summary of mass balance for 4-Amino N-Methyl Piperidine is given in Table .

Summary of Mass Balance for – 4-Amino N-Methyl Piperidine



batch size kg : 75



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 N-Methyl-4-Piperidone 100 1.33 13.33 Reactant

2 Methanol Rec. 450 6.00 60.00 Solvent




6 Methanol Fresh 50 0.67 6.67 Solvent Total 667 8.89 88.93

Output

1 N-Benzyl-4-Amino Piperidine 75 1.00 10.00 Finished Product


3 Raney Nickel 4 0.05 0.53 Reuse


5 Methanol Vapors 100 1.33 13.33 ReuseTotal 667 8.89 88.93


(B-12) 4-T-BOC-Amino Piperidine




Stage –I

Chemical Formula

Chemical Name

N

NH2

COOEt

+ ((CH3)3COCO)2O

N

NH

COOEt

O

O CH3 CH3

CH3

N-Carbethoxy 4-Amino Piperidine Boc anhydride N-Carbethoxy 4-BocAmino Piperidine

MolecularWeight

172 218 272

Stage –II

Chemical Formula

Chemical Name N

H

NH O

O CH3 CH3

CH3

N-Carbethoxy 4-BocAmino Piperidine

N

NH

COOEt

O

O CH3 CH3

CH3

+ NaOH SolutionWater

Chloroform + C2H5OH CO2+

4-Tert Boc Amino Piperidine

MolecularWeight

272 40 200

c) Summary of mass balance Summary of mass balance for 4-T-Boc Amino Piperidine is given in Table.

Summary of Mass Balance for – 4-T-Boc-Amino Piperidine


batch size kg : 65




Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input


100 1.33 13.33 Reactant



4 Di BOC 80 1.07 10.67 Reactant

5 Water 800 10.67 106.67 ---



8 Chloroform(Recovered) 900 12.00 120.00

9 Acetone(Fresh) 100 1.33 13.33

10 Acetone(Recovered) 500 6.67 66.67

11 N-Hexane(Fresh) 100 1.33 13.33

12 N-Hexane(Recovered) 700 9.33 93.33

Solvent

Total 4180 55.73 557.33

Output

1 4-Amino-N-Boc-Piperidine 65 0.87 8.67 Finished Product


3 Effluent with ethanol & methanol 1115 14.87 148.67 To ETP

4 Methanol Loss 100 1.33 13.33

5 Acetone Loss 100 1.33 13.33


7 N-Hexane Loss 100 1.33 13.33

To Atm

8 Rec Acetone 500 6.67 66.67

9 Rec Chloroform 900 12.00 120.00

10 Rec N-Hexane 700 9.33 93.33

Recovered Solvent

Total 4180 55.73 557.33


(B-13) N-Boc-4-Hydroxy Piperidine

a)Material Balance Diagram

Heating

Temperature & Pressure Maintaining

Raney Nickel Decantation

Crude N-Boc 4-Hydroxy Piperidine

50 Kg, N-Boc 4-Hydroxy Piperidine

Distilled N-Boc 4-Hydroxy Piperidine

HVD

Settled Raney Nickel:

Hydrogen Gas:4.2 Raney Nickel:4.2

N Haxane:

Heating, Stirring, Cooling, Centrifuge

Drying

ReactionMethanol:138.9

N-BOC 4, Piperidone:55.6

Methanol Recovered:125


b)Reaction Chemistry

ChemicalFormula

Chemical Name

N

O

COOEt

+O OO

OO

CH3

CH3

CH3

CH3

CH3CH3

N

O

O O

CH3

CH3

CH3

N-Carbethoxy 4-Piperidone Boc anhydride N-Boc 4-Piperidone


Summary of mass balance for N-Boc-4-Hydroxy Piperidine is given in Table.

Summary of Mass Balance for –N-Boc-4-Hydroxy Piperidine


batch size kg : 50



Kg/Batch Kg/Kg

of Product

MT/Month Remarks

Input

1 N-BOC-4-Piperidone 55.6 1.11 11.11 Reactant

2 Methanol(Fresh) 13.9 0.28 2.78

3 Methanol(Recovered) 125.0 2.50 25.00 Solvent

4 Raney Nickel 4.2 0.08 0.83 Catalyst

5 Hydrogen Gas 4.2 0.08 0.83 Reactant Total 203 4.06 40.56

Output


1 N-BOC-4-Hydroxy Piperidine 50 1.00 10.00 Finished Product


3 Methonol Loss 14 0.28 2.78 To Atm

4 Solid waste after distillation 14 0.28 2.78 To TSDF Total 203 4.06 40.56

(B-14) N-Boc-4-Amino Piperidine




Chemical Formula

N

O

O

CH3 O N O

O

OCH3

CH3

CH3

N NH2

O

OCH3

CH3

CH3


Summary of mass balance for N-Boc-4-Amino Piperidine is given in Table.

Summary of Mass Balance for –N-Boc-4-Amino Piperidine


batch size kg : 35



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 N-BOC-4-Piperidone 50 1.43 14.29


3 Methanol 250 7.14 71.43 Solvent



6 Acetone 160 4.57 45.71 Reactant

Total 474 13.54 135.43

Output

1 4-Amino-N-Boc-Piperidine 35 1.00 10.00 Finished Product


3 Raney Nickel 1 0.03 0.29

4 Acetone 120 3.43 34.29 Reuse



6 Acetone Vapors 43 1.23 12.29 To Atm Total 474 13.54 135.43

(B-15) 4-Piperidino Piperidine


Reaction vessel

Filteration

Piperidine:31.25 Toluene (Solvent)

Iso propyl Alcohol: N-Carbethoxy-4-Piperidone:41.67

5% Pd on carbon:4.17

Hysdrogen Gas:

IPA:208.33 Caustic Potash:

Solvent Recovery

Pd on carbon 5%

Hydrolysis IPA recovered

25Kg, Pure 4-Piperidino Piperidine

Cooling followed by Extraction

PurifiedWater:333

Toluene:

Organic LayerToluenerecovery

crude 4-Piperidino Piperidine

HVD


b) Reaction Chemistry Step-1:

Chemical Formula

Chemical Name N

O

COOEt

+NH

+CH3OH

H2gasPd/C( 5%)

3 -4 kg Pressure 35-40 N

N

COOEt

Molecular Weight

171 85 32 240

Step-2: Chemical Formula

Chemical Name N

N

COOEt

+ KOHIPA

90 -95 °C

NH

N

Molecular Weight

240 56 168


c)Summary of mass balance

Summary of mass balance for 4-Piperidino Piperidine is given in Table.

Summary of Mass Balance for –4- Piperidino Piperidine


batch size kg : 25



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 N-Carbethoxy 4-Piperidone 41.67 1.67 16.67

2 Piperidine 31.25 1.25 12.50

3 Sodium Sulphate 8.33 0.33 3.33 4 Potassium Hydroxide 83.33 3.33 33.33

Reactant

5 Pd/C(5%) 4.17 0.17 1.67 Catalyst

6 IPA 208.33 8.33 83.33

7 Toluene 208.33 8.33 83.33

8 Chloroform(Fresh) 83.33 3.33 33.33

9 Chloroform(Recovered) 333.33 13.33 133.33

Solvent

10 Water 333.33 13.33 133.33 --- Total 1335 53.42 534.17

Output

1 4-Piperidino piperidine 25.00 1.00 10.00 Finished

Product 2 Pd/C(5%) 4.17 0.17 1.67 Reuse

3 Chloroform Loss 83.33 3.33 33.33 To Atm

4 Chloroform Recovered 333.33 13.33 133.33 Recovered

Solvent 5 Solid Waste 10.42 0.42 4.17 To TSDF

Total 456 18.25 182.50


(B-16) 4-Chloro Piperidine HCl

a) Reaction Chemistry

Chemical Formula N OH

O

O

CH3

N Cl

O

O

CH3

NH ClNH Cl HC

b) Summary of mass balance

Summary of mass balance for 4-Chloro Piperidine HCl is given in Table.

Summary of Mass Balance for –4- Chloro Piperidine HCl


batch size kg : 40



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input 1 4-Chloro Piperidine 36 0.89 8.93

2 Toluene fresh 25 0.63 6.25 Reactant

3 Toluene rec 261 6.53 65.25

4 Hydrochloric Acid Gas 11 0.27 2.68

5 Acetone 100 2.50 25.00 Solvent

Total 432 10.81 108.11

Output

1 4-Chloro Piperidine Hydrochloric Acid


2 Rec Toluene 261 6.53 65.25

3 Waste Acetone 75 1.88 18.75 Recovered

Solvent

4 Mixed Toluene & Acetone 56 1.40 14.00 To Atm Total 432 10.80 108.00


(B-17) 4-(-4-Chloro Phenyl )-4-Hydroxy Piperidine


N-Carbethoxy-4-Piperidone:300


b) Reaction Chemistry Stage –I

Chemical Formula

Chemical Name

Br

Cl

+ Mg TuringsTHF

MgBr

Cl

P-Bromo Chloro Benzene Grignard Reagent Magnasium Metal

Molecular Weight

191.5 24 215.5

Stage –II

ChemicalFormula

ChemicalName

+

P-Bromo Chloro Benzene

MgBr

ClN

O

COOEt

Toluene

HCl Solution

N

OH

COOEt

Cl

+ MgBr(OH)

N-carbethoxy4-Piperidone

N-carbethoxy 4-Hydroxy4-(p-Chloro phenyl) Piperidine

MolecularWeight

215.5 171 283.5

Stage –III

Chemical Formula

Chemical Name OH

Cl

+ NaOH

Methanol Toluene

HCl l iOH

Cl

+ C2H5OH + CO2

MolecularWeight

283.5 40 211.5 46 44



Summary of mass balance for 4-(-4-Chloro Phenyl )-4-Hydroxy Piperidine is given in

Table.

Summary of Mass Balance for –4-(-4-Chloro Phenyl )-4-Hydroxy Piperidine


batch size kg : 500



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input


2 Hyflo 6 0.03 0.30

3 Hydrochloric Acid Gas 300 1.50 15.00

4 Acetone 150 0.75 7.50

5 Para Bromo chloro benzene 123 0.62 6.17


Reactant

7 Tetra Hydro Furan(fresh) 360 1.80 18.00

8 Tetra Hydro Furan(Recovered) 720 3.60 36.00

9 Activated Carbon 12 0.06 0.60 Catalyst

10 Methanol 400 2.00 20.00

11 Toluene(Fresh) 200 1.00 10.00


13 Iso Propyl Alcohol(Fresh) 160 0.80 8.00

14 Iso Propyl Alcohol(Recovered) 1600 8.00 80.00

Solvent

15 Purified water 3000 15.00 150.00 ----

16 Caustic Potash 400 2.00 20.00

17 Caustic Lye 300 1.50 15.00 Neutralizing

Agent

Total 11525 57.63 576.26

Output 1 4-(-4-Chloro Phenyl )-4-Hydroxy

Piperidine 200 1.00 10.00 Finished

Product 2 Effluent 3436 17.18 171.80 To ETP


3 Toluene loss 200 1.00 10.00 To Atm 4 Rec Iso Propyl Alcohol 1600 8.00 80.00

5 Iso Propyl Alcohol Rec 1600 8.00 80.00

6 Tetra Hydro Furan Rec 720 3.60 36.00

7 Toluene Rec 3000 15.00 150.00

Recovered Solvent

8 Solid Waste 50 0.25 2.50 To TSDF 9 IPA loss 160 0.80 8.00


11 Tetra Hydro Furan loss 360 1.80 18.00 To TSDF Total 11526 57.63 576.30


(B-18) 4-(-4- Bromo Phenyl )-4-Hydroxy Piperidine


280

37

Tetra Hydro Furan rec 200


80714

80



Stage –I

ChemicalFormula

ChemicalName

Br

Br

+ Mg TuringsTHF

MgBr

Br

P-Di bromo Benzene Grignard Reagent Magnasium Metal

MolecularWeight

236 24 260

Stage –II

ChemicalFormula

ChemicalName

+

Gignard reagent

MgBr

BrN

O

COOEt

Toluene

HCl Solution

N

OH

COOEt

Br

+ MgBr(OH)

N-carbethoxy4-Piperidone

N-carbethoxy 4-Hydroxy4-(p-Bromo phenyl) Piperidine

Molecular

Weight

260 171 328

Stage –III

ChemicalFormula

ChemicalName N

OH

COOEt

Br

+ NaOH

Methanol Toluene

HCl solution

NH

OH

Br

+ C2H5OH + CO2

N-Carbethoxy 4-Hydroxy 4-(p-Bromo phenyl ) Piperidine

Sodium Hydroxide 4-Hydroxy 4-(p-Bromo phenyl )

Piperidine Ethanol Carbon

dioxide


MolecularWeight

328 40 256 46 44


Summary of mass balance for 4-(-4-Bromo Phenyl )-4-Hydroxy Piperidine is given in

Table.

Summary of Mass Balance for –4-(-4-Bromo Phenyl )-4-Hydroxy Piperidine


batch size kg : 5



Kg/Batch Kg/Kg

ofProduct

MT/MonthRemarks

Input


2 Mg Turning 14 0.29 2.86

3 Tetra Hydro Furan Fresh 80 1.60 16.00

4 Para Di Bromo Benzene 114 2.29 22.86

5 Iodine 0 0.00 0.03


Reactant

7 Toluene(Fresh) 286 5.71 57.14


9 Caustic Potash 86 1.71 17.14

10 Methanol 143 2.86 28.57

11 Activated Carbon 9 0.17 1.71

Solvent

12 Hyflo 6 0.11 1.14

13 Iso Propyl Alcohol(Fresh) 80 1.60 16.00 Catalyst

14 Iso Propyl Alcohol(Recovered) 714 14.29 142.86 ---

15 Purified water 2143 42.86 428.57

16 Caustic Lye 107 2.14 21.43 Neutralizing

Agent

17 Tetra Hydro Furan Rec 200 4.00 40.00 Solvent Total 5303 106.06 1060.60

Output


1 4-(-4-Bromo Phenyl )-4-Hydroxy Piperidine


2 Effluent 2729 54.57 545.71 To ETP

3 Rec Toluene 1143 22.86 228.57

4 Rec Iso Propyl Alcohol 714 14.29 142.86 Recovered

Solvent

5 Toluene Loss 286 5.71 57.14

6 Iso Propyl Alcohol Loss 80 1.60 16.00 To Atm

7 Solid Waste 64 1.29 12.86

8 Waste Tetra Hydro Furan 37 0.74 7.40

9 Tetra Hydro Furan rec 200 4.00 40.00 To TSDF

Total 5303 106.05 1060.54


(B-19) 4-Phenyl-4-Hydroxy Piperidine




ChemicalFormula

Br MgBr

N

OH

EtOOCNH

OH

N

O

EtOOC


Summary of mass balance for 4-Phenyl-4-Hydroxy Piperidine is given in Table.

Summary of Mass Balance for –4-(-4-Bromo Phenyl )-4-Hydroxy Piperidine


batch size kg : 5



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 N-Carbethoxy-4-Piperidone 8.33 1.67 16.67

2 Mg Turning 1.67 0.33 3.33

3 Bromo Benzene 2.78 0.56 5.56

4 Chloro Benzene 8.33 1.67 16.67

5 Iodine 0.01 0.00 0.01

6 Hydrochloric Acid 8.33 1.67 16.67

7 Hyflo 0.22 0.04 0.44

Reactant


8 Toluene(Fresh) 16.67 3.33 33.33

9 Toluene(Recovered) 122.22 24.44 244.44

10 Methanol 13.33 2.67 26.67

11 Iso Propyl Alcohol(Fresh) 11.11 2.22 22.22

12 Iso Propyl Alcohol(Recovered) 55.56 11.11 111.11

Solvent

13 Tetra Hydro Furan 30.00 6.00 60.00

14 Activated Carbon 0.33 0.07 0.67 Catalyst

15 Purified water 166.67 33.33 333.33 ----

16 Caustic Potash 8.33 1.67 16.67

17 Caustic Lye 13.89 2.78 27.78 Neutralizing

Agent

Total 468 93.56 935.57

Output

1 4- Phenyl-4-Hydroxy Piperidine 5 1.00 10.00 Finished Product

2 Effluent 222.22 44.44 444.44 To ETP

3 Rec Toluene 122.22 24.44 244.44

4 Rec Iso Propyl Alcohol 55.56 11.11 111.11 Recovered

Solvent

5 Toluene loss 16.67 3.33 33.33

6 Iso Propyl Alcohol loss 11.11 2.22 22.22 To Atm

7 Solid Waste 1.67 0.33 3.33

8 Waste Tetra Hydro Furan 33.33 6.67 66.67 To TSDF

Total 468 93.56 935.56


(B-20) 4-Phenyl Piperidine

a) Material Balance Diagram

Cooling

Layer Separation

MDC:

Water Layer

Stirring

Toluene Layer

5 Kg, 4 phenyl pepridine

Azeotrop

Crude Mass: Methanol:

Palladium on Carbon:1.25

Water:25

Aqueous Layer MDC Layer

Pd on Carbon: 1.25 Methanol:

Layer Separation

Heating & Pressure Maintaining

Cooling

Filtration

Cooling & Filtration



Chemical Formula

Chemical Name

NH

OH+ H2SO4

NH

Toluene

110-115 °C

Molecular Weight

177 98 159


Summary of mass balance for 4-Phenyl Piperidine is given in Table.

Summary of Mass Balance -4-Phenyl Piperidine


batch size kg : 5



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 4-Phenyl 4-Hydroxy piperidine 12.5 2.50 25.00 Reactant



4 Sulphuric acid 1.25 0.25 2.50 Reactant

5 Water 25 5.00 50.00 ---

6 Pd/C (5%) 1.25 0.25 2.50 Catalyst

7 Water 100 20.00 200.00 ---

8 Hyflow 1.25 0.25 2.50

9 Sodium sulphate 1.25 0.25 2.50 Reactant

Total 268 53.50 535.00

Output


1 4-Phenyl Piperidine 5 1.00 10.00 Finished Product

2 Pd/C(5%) 1.25 0.25 2.50 Reuse


4 Toluene Recovered 100 20.00 200.00 Recovered Solvent

5 Solid Waste 3.125 0.63 6.25 To TSDF

6 Water 134 26.80 268.00 To ETP

Total 268 53.68 536.75

(B-21) 1-Amino Piperidine


190

30



ChemicalFormula

ChemicalName

N

NH2

COOEt

N-Carbethoxy 4-Amino Piperidine

+ NaOH

NH

NH2

4-Amino Piperidine

+ C2H5OH + CO2

CarbonDioxide

Sodium Hydroxide

Water

Chloroform

Ethanol

MolecularWeight

171 40 99 46 44


Summary of mass balance for 1-Amino Piperidine is given in Table.

Summary of Mass Balance -1-Amino Piperidine


batch size kg : 180


QuantitySr. No. Name of Raw Material Kg/Batc

h

Kg/Kgof

Product MT/Month

Remarks

Input


2 Ammonia Gas 40 0.22 2.22

3 Methanol 500 2.78 27.78

Reactant



6 Caustic Lye 190 1.06 10.56 Reactant


8 Methylene Di Chloride(Recovered)

900 5.00 50.00 Solvent

9 Water 600 3.33 33.33 --- Total 2548 14.16 141.56

Output

1 1-Amino Piperidine 180 1.00 10.00 Finished Product


2 Rec Methanol+ Ammonia 480 2.67 26.67 Recovered Solvent

3 Raney Nickel recyclable 3.5 0.02 0.19 Reuse



6 Methylene Di Chloride Loss 100 0.56 5.56

7 Carbon Di oxide 50 0.28 2.78 To Atm

8 Effluent with ethanol 804 4.47 44.67 To ETP

Total 2548 14.16 141.56 141.53


(B-22) 1-Methyl-4-Piperidinyl Di Phenyl Hydroxy acetate




Stage –I

ChemicalFormula

ChemicalName

OH COOH

+ CH3OHH2SO4

OH COOCH3

Benzilic acid Methanol Benzilic acid methyl Ester

MolecularWeight

228 32 242

Stage –II

ChemicalFormula

ChemicalName

OH COOCH3

Benzilic acid methyl Ester

+N

OH

CH3

N -methyl 4 -Hydroxy Piperidine

O COOCH3

N

CH3

Toluene

Benzene Sodium Methoxide

methyl [(1-methylpiperidin-4-yl)oxy](diphenyl)acetate

MolecularWeight

242 115 339



Summary of mass balance for 1-Methyl-4-Piperidinyl Di Phenyl Hydroxy acetate is

given in Table.

Summary of Mass Balance -1-Methyl-4-Piperidinyl Di Phenyl Hydroxy acetate


batch size kg : 115



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 N-Methyl-4-Hydroxy Piperidine 80 0.70 6.96 Reactant

2 Toluene 560 4.87 48.70

3 Benzene 345 3.00 30.00 Solvent

4 Benzillic acid 200 1.74 17.39

5 Methanol 500 4.35 43.48

6 Water 1000 8.70 86.96

7 Sodium Methoxide 80 0.70 6.96

Reactant

Total 2765 24.04 240.43

Output

1 1-Methyl-4-Piperidinyl Di Phenyl Hydroxy Acetate


2 Mixed Toluene & Benzene 1000 8.70 86.96 To ETP

3 Waste Methanol 450 3.91 39.13 To TSDF

4 Effluent 1200 10.43 104.35 To ETP

Total 2765 24.04 240.43


(B-23) (1-Methyl-4-Piperidinyl)3-[2[(3-Chloro Phenyl)ethyl]-2-

Pyridinyl]Methanone

a) Reaction Chemistry

Stage –I

ChemicalFormula

ChemicalName

N

N

Cl

CH3

O

{3-[2-(3-chlorophenyl)ethyl]-2,3-dihydropyridin-2-yl}(1-methylpiperidin-4-yl)methanone

N

Cl

NC +N

MgCl

CH3

THF

Toluene

3-[2-(3-chlorophenyl)ethyl]pyridine-2-carbonitrile Gignard reagent

MolecularWeight

242.5 158 344.8



Summary of mass balance for (1-Methyl-4-Piperidinyl)3-[2[(3-Chloro Phenyl)ethyl]-2-

Pyridinyl]Methanone is given in Table.

Summary of Mass Balance - (1-Methyl-4-Piperidinyl)3-[2[(3-Chloro Phenyl)ethyl]-2-

Pyridinyl]Methanone


batch size kg : 150



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 3-(2-Chloro Phenyl )ethyl 2-cyano pyridine

125 0.83 8.33


3 Magnesium Turning 30 0.20 2.00

Reactant

4 Tetra Hydro Furane 540 3.60 36.00 Catalyst

5 Iodine 0.1 0.00 0.01

6 Ethylene Bromide 3 0.02 0.20 Reactant

7 Water 1500 10.00 100.00 ----


9 Tetra Hydro Furan 540 3.60 36.00 Reactant

10 Toluene 600 4.00 40.00 SolventTotal 3913 26.09 260.87

Output

1 Lorata-7 150 1.00 10.00 Finished Product

2 Rec Tetra Hydro Furan High M/C 600 4.00 40.00

3 Rec Toluene & Tetra Hydro Furan 800 5.33 53.33 To TSDF

4 Effluent 2313 15.42 154.20 To ETP

5 Solid waste 50 0.33 3.33 To TSDF

Total Total 3913 26.09 260.87


(B-24) 1-Butanon-4-[4-(4-Chloro Phenyl)-4-Hydroxy-1-Piperidinyl-1-(-4-Fluoro Phenyl)

a) Summary of mass balance Summary of mass balance for 1-Butanon-4-[4-(4-Chloro Phenyl)-4-Hydroxy-1-

Piperidinyl-1-(-4-Fluoro Phenyl) is given in Table.

Summary of Mass Balance - 1-Butanon-4-[4-(4-Chloro Phenyl)-4-Hydroxy-1-

Piperidinyl-1-(-4-Fluoro Phenyl)


batch size kg : 50



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 4-Chloro p-Fluoro phenol 62.5 1.25 12.50

2 4-(p-chloro pheny)4-Hydroxy Piperidine

56.25 1.13 11.25 Reactant

3 Acetone(Fresh) 62.5 1.25 12.50

4 Acetone(Recovered) 250 5.00 50.00 Solvent

5 Potassium carbonate 31.25 0.63 6.25 Reactant

6 Water 125 2.50 25.00 ---



9 Charcoal 6.25 0.13 1.25 Catalyst Total 1219 24.38 243.75

Output

1 Haloperidol(tech) 50 1.00 10.00 Finished Product

2 Acetone Loss 62.5 1.25 12.50 To Atm

3 Acetone Recovered 250 5.00 50.00 Re. Solvent


5 Methanol Recovered 500 10.00 100.00 Re. Solvent

6 water 219 4.38 43.80 --


Total Total 1219 24.38 243.80


(C-1) 4-Amino 1,2,4 Triazole


360

120



Stage –I

Chemical Formula

Chemical Name

H COOH + NH2NH2.H2O H

NH NH2

O

+

WaterFormic acid Hydrazine Hydrate Formyl Hydrazide

H2O

MolecularWeight

46 50 60 18

Stage –II

ChemicalFormula

ChemicalName

N N

N

NH2

4-Amino 1,2,4 Triazole

H

NH NH2

O

Formyl Hydrazide

2 + 2H2O

Water

MolecularWeight

120 84 36



Summary of mass balance for 4-Amino 1,2,4 Triazole is given in Table.

Summary of Mass Balance – 4-Amino 1,2,4 Triazole


batch size kg : 1400



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Hydrazine Hydrate 2400 1.71 8.57

2 Formic acid 2100 1.50 7.50 Reactant

3 Iso Propyl Alcohol Rec 360 0.26 1.29 Solvent

4 Activated Carbon 8 0.01 0.03 Catalyst

5 Hyflo 4 0.00 0.01 Catalyst

6 Iso Propyl Alcohol Fresh 40 0.03 0.14 Reactant

Total 4912 3.51 17.54

Output

1 4-Amino 1,2,4 Triazole 1400

1.00 5.00 Finished Product

2 Distilled Water 3000 2.14 10.71 ---

3 Waste Activated Carbon + Hyflo 12 0.01 0.04 To TSDF

4 Iso Propyl Alcohol rec 360 0.26 1.29 Reuse

5 Water Vapors 100 0.07 0.36 To Atm

6 IPA Loss 40 0.03 0.14

Total 4912 3.51 17.54


(C-2) 3-Amino 1,2,4 Triazole



ChemicalFormula

ChemicalName

NH2 NH

NH2

NHH2CO3

+ H COOHIPA N

NNH

NH2

Guanidine carbonate Formic Acid 3-Amino 1,2,4 triazole

MolecularWeight

136 46 84

Condensation

Water Distillation Effluent: 512

Amino Guanidine bi carbonate:769.2

Formic acid :261.5

pH Adjustment

SolidWaste: 173 Filtration

Centrifugation & IPA wash

IPA(Recovered):3600 IPA Loss:92

3-Amino 1,2,4 Triazole (Finished Product):500

Charcoal:153.8

IPA(Recovered):3600 IPA(Fresh):92



Summary of mass balance for 3-Amino 1,2,4 Triazole is given in Table.

Summary of Mass Balance – 3-Amino 1,2,4 Triazole


batch size kg : 500



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 AminoGuanidine bi carbonate 769 1.5 7.7

2 Formic acid 262 0.5 2.6

3 Iso Propyl Alcohol fresh 92 0.2 0.9

Reactant

4 Iso Propyl Alcohol rec 3600 7.2 36.0 solvent

5 Charcoal 154 0.3 1.5 Catalyst Total 4877 9.8 48.8

Output

1 3-Amino 1,2,4 Triazole 500.0 1.0 5.0 Finished Product

2 Iso Propyl Alcohol 3461.5 6.9 34.6

3 Effluent 684.6 1.4 6.8 To ETP

4 SolidWaste 173 0.3 1.7

5 Iso Propyl Alcohol loss 92 0.2 0.9 To TSDF

Total 4876.9 9.8 48.8


(C-3) 1,2,4 Triazole


Material balance Diagram - APCM

Condensation Hydrazine Hydrate: 222

Formic acid: 444 Ammonia: 178

Ethyl acetate (Recovered h): 756

Ethyl acetate (Fresh): 133

Centrifugation & IPA wash Waste Ethyl

Acetate: 133

Ammonia: 44

Drying

400 kg of 1,2,4 Triazole (Finished Product)

Dying loss: 400 EA (Re.) : 756

Water Scrubber NH3: 0.1 Water: 0.9

Byproduct NH3 (10 %): 1.00 (Sale)



Stage -I

Chemical Formula

Chemical Name

H COOH + NH3 H

O

NH2

+ H2O

Formic Acid Ammonia Formamide Water

MolecularWeight

46 17 45 18

Stage -II

Chemical Formula

Chemical Name

H

O

NH2

+ NH2NH2H2O

Formamide Hydrazine Hydrate

N

NN

H

+NH3+ H2O

(1H) 1,2,4 Triazole

MolecularWeight

45 50 69 17 18


c) Summary of mass balance Summary of mass balance for 1,2,4 Triazole is given in Table.Summary of Mass Balance –1,2,4 Triazole


batch size kg : 400



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 Formic Acid 444.4 1.11 5.56

2 Ammonia 177.8 0.44 2.22

3 Hydrazine Hydrate 222.2 0.56 2.78

Reactant

4 Ethyl acetate (Fresh) 755.6 1.89 9.44

5 Ethyl acetate (Recovered) 133.3 0.33 1.67 Solvent

Total 1733.3 4.33 21.67

Output

1 1,2,4 Triazole 400

1.00 5.00 Finished Product

2 Ammonia 44

0.11 0.55 To Scrubber

3 Ethyl acetate Waste 133 0.33 1.66 To TSDF

4 Ethyl acetate (Recovered) 756

1.89 9.45 Recovered Solvent

5 Drying Loss 400 1.00 5.00 To Atm

Total Total 1733 4.33 21.66

Summary of Mass Balance - 1,2,4 Triazole APCMQuantity

Sr. No. Name of Raw Material Kg/Batch Kg/Kg of Product MT/Month Remarks



2 Ammonia Gas 44.44 0.1111 0.5556 To Scrubber Total 444.44 1.1111 5.5556


1 Liq. Ammonia 444.44 1.1111 5.5556 Sale as By Product

Total 444.44 1.1111 5.5556


(C-4) 1[(2,4 Di Fluoro Phenyl)-1-2-(1-H)1,2,4 Triazolyl Ethanone


Material balance Diagram - APCM

Quenching

Layer Separation Effluent (Aqueous

Layer): 2171

Distillation

Cooling & temp maintaining

Recovered IPA: 4500

200 kg of 1[(2,4 Di Fluoro Phenyl)-1-2-(1-H)1,2,4 Triazolyl Ethanone

(Finished Product)

1,3 Di Fluoro Benzene: 125

MDC: 450 Chloro acetyl chloride:

105 Aluminium Chloride: 156

Ice: 800

MDC (Recovered): 400

Distillation loss: 50 Distillation residue:

25

Centrifugation & Drying

Chilling Sod. Nitrite Solution: 180 Hcl: 600

Ammonia Solution: 500


lPA (Fresh): 500 lPA (Recovered): 4500 4 -Amino 1,2,4 Triazole:

165

Effluent (M/L): 4746 IPA Loss : 100

Waste sludge:100 HCL gas:60



Stage -I

Chemical Formula

Chemical Name

F

F

F

F

OCl

+ ClCH2COClMDC

+ HCl

1,3 Difluoro Benzene Chloro acetyl chloride 2-chloro-1-(2,4-difluorophenyl)ethanone

MolecularWeight

95 113 171.5

Stage -II

ChemicalFormula

ChemicalName

2-chloro-1-(2,4-difluorophenyl)ethanone

F

F

OCl

+N

N N

NH2

4-Amino 1,2,4 triazole

F

F

O

NN

N+NH2

HCl

QA salt

MolecularWeight

190.5 84 274.5

Stage -III

ChemicalFormula

ChemicalName

F

F

O

NN

N+NH2

HCl

QA salt

+ NaNO2Water

HCl solutionLiquor ammonia

F

F

O

NN

N

1-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanone

MolecularWeight

274.5 69 223

Water Scrubber HCl: 60 Water: 140

Byproduct HCl (30 %): 200 (Sale)



Summary of mass balance for 1[(2,4 Di Fluoro Phenyl)-1-2-(1-H)1,2,4 Triazolyl

Ethanone is given in Table.

Summary of Mass Balance –1[(2,4 Di Fluoro Phenyl)-1-2-(1-H)1,2,4 Triazolyl Ethanone


batch size kg : 200



Kg/Batch Kg/Kg

of Product

MT/Month Remarks

Input

1 1,3 DiFluoro Benzene 125 0.63 3.13

2 Chloro acetyl chloride 105 0.53 2.63 Reactant


4 Methylene Di Chloride(Recovered) 400

2.00 10.00 Solvent

5 Aluminium chloride 156

0.78 3.90 Reactant

6 Ice 800 4.00 20.00

7 Water 2500 12.50 62.50 ----


9 Iso Propyl Alcohol(Recovered) 4500 22.50 112.50 Solvent

10 4-Amino 1,2,4 Traizole 165 0.83 4.13


12 Sodium Nitrite 180 0.90 4.50

13 Ammonia Solution 500 2.50 12.50

Reactant

Total 10181 50.91 254.53

Output

1 1-(2,4,Di Fluoro )1-H-1,2,4 Triazolyl Acetophenone 200 1.00 5.00 Finished

Product 2 Methylene Di Chloride Loss 50 0.25 1.25 To Atm

3 Rec Methylene Di Chloride 400 2.00 10.00



Recovered Solvent


6 Waste Sludge 100 0.50 2.50 To TSDF

7 Effluent 4746 23.73 118.65 To ETP


9 Hydrochloric Acid Gas 60 0.30 1.50 ToScrubber

Total 10181 50.91 254.53

Summary of Mass Balance -1[(2,4 Di Fluoro Phenyl)-1-2-(1-H)1,2,4 Triazolyl Ethanone

APCM




1 Water 140 0.700 3.50 Scrubbing Media

2 Hydrochloric Acid Gas 60 0.300 1.50 To Scrubber Total 200 1.000 5.00


1 Hydrochloric Acid (30 %) 200 1.000 5.00 Sale as By Product

Total 200 1.000 5.00


(C-5) Epoxy Mesylate


100

100

100

100

1900

100

250

1410


b) Reaction Chemistry Stage -I

ChemicalFormula

ChemicalName

F

F

O

NN

N

+ CH3 S+

CH3

CH3 OI

EDC

NaOH solutionF

F

NN

N

O

1-(2,4-difluorophenyl)-2-(1H-1,2,4-triazol-1-yl)ethanone

1-{[2-(2,4-difluorophenyl)oxiran-2-yl]methyl}-1H-1,2,4-triazole

MolecularWeight

223 220 237

Stage -II

ChemicalFormula

ChemicalName

F

F

NN

N

O

1-{[2-(2,4-difluorophenyl)oxiran-2-yl]methyl}-1H-1,2,4-triazole

F

F

NN

N

O

+

CH3SO3H

AcetoneCH3 SO3H

Epoxy mesylate

MolecularWeight

237 96 333


c) Summary of mass balance Summary of mass balance for Epoxy Mesylate is given in Table.

Summary of Mass Balance –Epoxy Mesylate


batch size kg : 150



Kg/Batch Kg/Kg

of Product

MT/Month Remarks

Input

1 DFTA 150 1.00 5.00 Reactant


3 Methylene Di Chloride(Recovered) 1250 8.33 41.67

Solvent

4 Tri Methyl Silyl Iodide 250 1.67 8.33

5 Caustic Soda Lye 150 1.00 5.00 Reactant

6 Water 1200 8.00 40.00 ---

7 Acetone(Fresh) 100 0.67 3.33

8 Acetone(Recovered) 2000 13.33 66.67 Solvent

9 Methane Sulfonic acid 60 0.40 2.00 Reactant

Total 5260 35.07 175.33

Output

1 Epoxy mesylate 150 1.00 5.00 Finished Product



4 Acetone Loss 100 0.67 3.33 To Atm

5 Rec Acetone 1900 12.67 63.33 Recovered Solvent

6 Acetone vapors in dryer 100 0.67 3.33 To Atm

7 Rec TMSI 250 1.67 8.33 Recovered Solvent

8 Effluent 1410 9.40 47.00 To ETP

Total 5260 35.07 175.33


(D-1) Alfa Alfa Di Methyl Phenyl acetic acid methyl ester




ChemicalFormula

ChemicalName

COOH

CH3CH3

a,a Dimethyl phenyl acetic acid

+

.

Methanol COOMe

CH3CH3

a,a dimethyl Phenyl Acitic acid

+ H2O

.

+ HCl SolutionToluene

NaHCO3

Methyl ester

MolecularWeight

164 32 36.5 178 18



Summary of mass balance for Alfa Alfa Di Methyl Phenyl acetic acid methyl ester is

given in Table.

Summary of Mass Balance – Alfa Alfa Di Methyl Phenyl acetic acid methyl ester


batch size kg : 180



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Alfa Alfa Di methyl phenyl acetic acid 200 1.11 3.33

2 Methanol 600 3.33 10.00


Reactant



6 Purified water 500 2.78 8.33 ----

7 Sodium Carbonate 50 0.28 0.83 Reactant Total 2550 14.17 42.50

Output

1 Alfa Alfa Di methyl phenyl a. acid M Ester 180 1.00 3.00 Finished


3 Residue after toluene rec & prod.distln 80 0.44 1.33 To TSDF



Total 2550 14.17 42.50


(D-2) Alfa Alfa Di Methyl Phenyl acetic acid


165 kg of Alfa Alfa Di Methyl Phenyl acetic acid

(Finished Product)


Alluminum Chloride as by product:2000

Heating

Cooling & Chilling

Unreacted Benzene:600


Process Water: 1200 Activated Carbon: 5

Hyflow: 5 Caustic Lye: 350

Chilling followed by stirring

Benzene: 200 Aluminum Chloride: 500

Methacrylic acid: 150 Process Water: 1600

HCL: 500

HCl: 250

Effluent (M/L): 1685



Stage -I

ChemicalFormula

ChemicalName

CN

Benzyl cyanide

+

.

CN

CH3CH3

a,a dimethyl Benzyl cynide

+ NaCl

.

MEG

KOH(CH3)2SO4

Dimethyl Sulphate

MolecularWeight

117 126 145 58.5

Stage -II

ChemicalFormula

ChemicalName

CN

CH3CH3

á,á Dimethyl Benzyl cyanide

+

.

NaOH LYE MEG

HCl +WaterCOOH

CH3CH3

a,a dimethyl Phenyl Acitic acid

MolecularWeight

145 40 164



Summary of mass balance for Alfa Alfa Di Methyl Phenyl acetic acid is given in

Table.

Summary of Mass Balance – Alfa Alfa Di Methyl Phenyl acetic acid


batch size kg : 165



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Benzyl Cyanide 100 0.61 1.82

2 Di Methyl Sulfate 150 0.91 2.73

3 Di methyl Sulfoxide 500 3.03 9.09

4 Caustic Potash 2600 15.76 47.27

Reactant

5 Purified water 250 1.52 4.55 ---

6 Toluene 250 1.52 4.55


Total 4450 26.97 80.91

Output

1 Alfa Alfa Di methyl phenyl acetic acid 165 1.00 3.00 Finished


3 Aluminium Chloride 2000 12.12 36.36

4 Benzene Rec. 600 3.64 10.91 To TSDF

Total 4450 26.97 80.91 80.91


(D-3) Alfa Alfa Di Methyl Para Bromo Phenyl acetic acid


Heating followed by cooling

Alfa Alfa Di methyl phenyl acetic acid :400

Clo. (Fresh) : 100 Clo. (Recovered) : 600

Iron Powder: 1.0 Liquid Bromine: 600

Sulfuric acid : 200 Water :1500

Layer separation Effluent (Aqueous

Layer): 1600

Cooling followed by centrifuge

Caustic Lye: 300 Effluent (M/L): 2526

Heptane Recovered: 1600

Heptane Loss: 100 Chloroform loss:100

Chloroform Recovered:600

Heptane Loss:100

170 kg of Alfa Alfa Di Methyl Para Bromo Phenyl acetic acid

(Finished Product)

Azeotrpic distillation of

Crude Product Heptane (fresh): 100

Heptane (Recovered): 1600

HBr gas: 305


Mass Balance Diagram-APCM



Chemical Formula

Chemical Name

COOH

CH3CH3

+ Br2CTC

COOH

CH3CH3

Br

a,a DiMethyl Phenyl acetic Acid a,a DiMethyl P-Bromo Phenyl acetic Acid

+ HBr

MolecularWeight

164 160 243 81

Hydrobromic Acid: 981 Water Scrubbing

Water: 676 HBr Gas: 305

Sodium Bromide: 2590 Water Scrubbing

Caustic: 8 Water: 56

HBr Gas: 2526



Summary of mass balance for Alfa Alfa Di Methyl Para Bromo Phenyl acetic acid is

given in Table.

Summary of Mass Balance – Alfa Alfa Di Methyl Para Btomo Phenyl acetic acid


batch size kg : 170



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Alfa Alfa Di methyl phenyl acetic acid 400 2.35 7.06 Reactant

2 Chloroform fresh 100 0.59 1.76

3 Chloroform rec 600 3.53 10.59 Solvent

4 Iron Powder 1.00 0.006 0.018

5 Liq Bromine 600 3.53 10.59

6 Sulfuric acid 200 1.18 3.53

Reactant


8 Water 1500 8.82 26.47 ---

9 Heptane(Fresh) 100 0.59 1.76

10 Heptane(Recovered) 1600 9.41 28.24 Solvent

Total 5401 31.77 95.31

Output

1 Alfa Alfa Di methyl P Bromo phenyl a. acid 170 1.00 3.00 Finished


3 HBr gas 305 1.79 5.38 To Scrubber

4 Rec Heptane 1600 9.41 28.24 Recovered Solvent

5 Heptane Loss 100 0.59 1.76

6 CTC Loss 100 0.59 1.76 To Atm

7 Rec CTC 600 3.53 10.59 Recovered Solvent

Total 5401 31.77 95.31


Summary of Mass Balance - Alfa Alfa Di Methyl Para Bromo Phenyl acetic acid -

APCM




1 Water 676 3.977 11.93 Scrubbing Media

2 HBr Gas 290 1.704 5.11 To Scrubber Total 966 5.681 17.04


1 Hydrobromic Acid (30 %) 966 5.681 17.04 Sale as By

Product Total 966 5.681 17.04

Alkali scrubber Input

1 Caustic 8 0.05 0.14 To Scrubber

2 Water 56 0.33 0.99

3 HBr Gas 15 0.09 0.27 Scrubbing

Media

Total 79 0.47 1.40

Alkali scrubber Output

1 Sodium Bromide 79 0.47 1.40 Sale as By Product

Total 79 0.47 1.40


(D-4) (A) 4-(-4-Chloro 1-Oxobutyl)2,2,di methyl phenyl a. acid


250 Kg Alfa Alfa Di Methyl Phenyl acetic acid(FEX-2)

Chilling followed by Stirring

Benzene: 200 Aluminum Chloride: 500

Methacrylic acid: 150 Process Water: 1600

HCL: 500 Extraction Aluminum Chloride as by product

Heating Unreacted benzene

Cooling & Chilling HCl: 250


Reaction Vessel

Heating & TemperatureMaintenance

Cooling

Methanol: HCl:

Fex-2:

Purified Water:

ExtractionAqueous Layer Toluene

Process Water: 1200 A. Carbon: 5

Hyflow: 5 Caustic Lye: 350

Effluent : 1000


Organic Layer Recovered Toluene


CoolingPurified Water:

HCl:

Extraction

Organic Layer

Aqueous Layer

Recovered Toluene

Chilling1,2 Di Methoxy ethane:

Aluminum Chloride: Sodium Borohudride:

Fex-3:

Toluene

Heating & Cooling


Layer Separation

Organic Layer

Aqueous Layer

Reaction Vessel Fex-4:

Acetic Anhydride:

Sodium Carbonate

Solution

N-Haxane:

Stirring &Layer Separation

Aqueous Layer


4-(-4-Chloro-1-Oxo Butyl)2,2 Di methyl Phenyl acetic

acid (D-4A) FEX-6

Organic Layer N-Haxane Recovered

Stirring & Chilling

Heating & Temperature Maintaining

Fex-5:

Chilling & Dumping of Mass

Stirring, Settling, Layer Separation & wash

aqueous Layer By MDC

Reaction Vessel Metylene Chloride: Aluminum Chloride:

HCl: Purified Water:

4-Cholo Butyryl Chloride:

Combine Organic Layer

MDC recovered

Aqueous Layer

Degassing


Alfa Alfa Di methyl-4-(1-oxo-1-cyclo propyl)phenyl

acetic acid(D-4B) FEX-8

Extraction

Cooling & Temperaturemaintaining

D.N.S: Caustic Soda:

Fex-6: Toluene:

4-Cholo Butyryl Chloride:

Organic Layer Aqueous Layer

Toluene Recovery

Temperature maintaining

Stirring Caustic Lye Solution: Sodium Bi sulfite

Cooling and Stirring

Caustic Lye Solution: Fex-7:

Potassium Permanganate:

Extraction Toluene:

Organic Layer Aqueous Layer

Toluene Recovery


4-(-4-Chloro-1-Oxo Butyl)2,2 Di methyl Phenyl acetic acid M

Ester (D-4C) FEX-9

Heating to reflux

U/VAC Methanol Recovery

Reaction Vessel Methanolic HCl: Fex-8:


Stirring & Layer Separation

Aqueous Layer

Organic Layer

MIBK: Sodium Bi Carbonate:

Purified Water: Sodium chloride solution

Layer Separation

Aqueous Layer

Aqueous Layer

Organic Layer as Fex-9

Azacyclonol: Potassium Bi Carbonate:

Potassium Iodide:

Heat to reflux & Azeotrop to remove

water


4-(-4-HYDROXY DI PHENYL METHYL )1-PIPERIDINYL-1-OXO BUTYL) ALFA ALFA DI

METHYL PHENYL ACETIC ACID METHYL ESTER (D-4D) FEX-10

Cooling & Neutsching salt

washing by MIBK

Filter & washing ML MIBK recovery

Cooling Water RecoveryWater Addition

Denatured Spirit: Purified water:

Stirring, Cooling, Chilling centrifuge

washing

Reaction Methanol: Fex-10:

Stir, Cooling,

Heating, & Temperature Maintaining

Caustic Lye: Sodium Borohydride 2nd

Lot



Cooling

CentrifugeWater wash HCl

Product: Purified Water

Heating, Stirring, Centrifuge, Hot

water wash

Benzene acetic acid, 4-(1-Hydroxy-4-[4-(Hydroxy Di Phenyl Methyl)-1-

Piperidinyl]Butyl]Alfa Alfa Di Methyl (D-4E) FEX-12

Heating, Stirring, Cooling, Centrifuge

DNS Wash

Fex-12

Mother Liqour

Fex-12 Pure

Mother Liqour

DNS Recovery


Chemical Formula

Chemical Name

MolecularWeight

CN COOH

CH3CH3

COOMe

CH3CH3

CH2OH

CH3CH3CH3CH3

O CH3

O

CH3CH3O CH3

O

ClO

CH3CH3OH

ClO

COOH

CH3CH3

ClO

COOMe

CH3CH3

ClO FEX - 9 FEX -8

FEX -7FEX -6

FEX -5 FEX -4

FEX -3FEX -2FEX -1

Molecular Formula = C14H17ClO3

Formula Weight = 268.73598







Molecular Formula = C12H16O2

Formula Weight = 192.25424Molecular Formula = C10H14OFormula Weight = 150.21756

Molecular Formula = C11H14O2

Formula Weight = 178.22766Molecular Formula = C10H12O2

Formula Weight = 164.20108Molecular Formula = C8H7NFormula Weight = 117.14788

1. 14 1. 08

0.84

1.27

1.54

0.85

1.05

1.05

FEX -12


ChemicalFormula

ChemicalName

MolecularWeight

COOMe

C H 3CH 3

C lO

COOMe

C H 3CH 3

O

NO H

COOMe

C H 3CH 3

O H

NO H

FEX -9

FEX -10

FEX -11

Molecular Formula = C33H41NO4






1.82

1.00

COOH

C H 3CH 3

O H

NO H

FEX -12



COOMe

C H 3CH 3

O H

NO H

FEX -11



Summary of mass balance for 4-(-4-Chloro-1-Oxo Butyl) 2,2 Di methyl Phenyl acetic

acid is given in Table.

Summary of Mass Balance – 4-(-4-Chloro-1-Oxo Butyl) 2,2 Di methyl Phenyl acetic

acid


batch size kg : 250



Kg/Batch Kg/Kg

ofProduct

MT/MonthRemarks

Input

1 4-(4-chloro-1-oxo butyl)alfa alfa di methyl phenyl acetic acid 250

1.00 3.00


3 Methanol rec. 250 1.00 3.00

Reactant

4 HCl 300 1.20 3.60

5 Methylene Di Chloride(Fresh) 50 0.20 0.60 Solvent

6 Sodium Bicarbonate 25 0.10 0.30 ---

7 Water 1000 4.00 12.00 Reactant

8 Methylene Di Chloride(Recovered) 500 2.00 6.00 Solvent Total 2725 10.90 32.70

Output

1 4-(-4-Chloro 1-Oxobutyl)2,2,di methyl phenyl a. acid 250 1.00 3.00 Finished


3 Methanol rec. 250 1.00 3.00

4 Rec Methylene Di Chloride 500 2.00 6.00 Recovered

Solvent


Total 2725 10.9 32.7


(D-5) [2-[(2,6, di chloro phenyl)Amino]phenyl acetoxy acetic acid a) Material Balance Diagram:


ChemicalFormula

CH3

CH3

OHCH3 +Cl

Cl

O

CH3

CH3

OCH3

Cl

O

OO

CH3CH

CH3

O

ONH

ClCl

OO

CH3CH3

CH3

O

ONH

ClCl

OOH

O

ONH

ClCl

S-81

2[(2,6 Di Chloro Phenyl) Amino] Phenyl acetoxy acetic acid

Chloro acetyl chloride: 418 Tertiary Butyl alcohol:300 N N Di Methyl aniline:490

Water:5000 Toluene:600

Sodium by Carbonate

Extraction &

HVD

Filtration

Filtration & Drying

Tetra butyl ammonium bromide:10

Diclofenac sodium:600 Methanol:600

Formic Acid:1080 Water:

Effluent Water: Recovered Toluene: Solid Waste after HVD:

Effluent Methanol Water:



Summary of mass balance for [2-[(2,6, di chloro phenyl)Amino]phenyl acetoxy

acetic acid is given in Table.

Summary of Mass Balance – [2-[(2,6, di chloro phenyl)Amino]phenyl acetoxy acetic

acid


batch size kg : 300



Kg/Batch Kg/Kg

of Product

MT/Month Remarks

Input

1

2-Tert butoxy-2-oxo-ethyl (2-2,6 dichlorophenyl)amino)phenyl acetate

455 1.52 4.55

2 Formic acid 682 2.27 6.82

Reactant



5 Water 909 3.03 9.09 --- Total 2409 8.03 24.09

Output

1 2-(2, 6 dichlorophenyl) Amino) phenyl acetoxy acetic acid 300 1.00 3.00 Finished


3 Toluene Recovered 318 1.06 3.18 Recovered Solvent


Total 2409 8.03 24.09


(D-6) 2-Tert Butoxy-2-oxo-ethyl{2-[2,6 di chloro phenyl)amino]phenyl acetate


Heating

Cooling & filtration

Cooling

Effluent: 4.71Filtration

Drying

Water: 4.0

2-Chloroacetic acid t-butyl ester: 1.0

TBAB: 0.03 Diclofenec sodium: 1.50

Methanol (Fresh):1.20 Methanol (Recovered):

0.10

1.82 kg of 2-Tert Butoxy-2-oxo-ethyl{2-[2,6 di chloro

phenyl)amino]phenyl acetate (Finished Product)

Methanol Loss:1.20 Methanol

Recovered: 0.10



Chemical Formula

CH3

CH3

OHCH3 +Cl

Cl

O

CH3

CH3

OCH3

Cl

O

OO

CH3CH3

CH3

O

ONH

ClCl

OO

CH3CH3

CH3

O

ONH

ClCl

OOH

O

ONH

ClCl

S-81



Summary of mass balance for 2-Tert Butoxy-2-oxo-ethyl{2-[2,6 di chloro

phenyl)amino]phenyl acetate is given in Table.

Summary of Mass Balance – 2-Tert Butoxy-2-oxo-ethyl{2-[2,6 di chloro

phenyl)amino]phenyl acetate


batch size kg : 250



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 2-Chloroacetic acid t-butyl ester 137 0.55 1.65

2 Diclofenec sodium 206 0.82 2.47

3 TBAB 3 0.01 0.04

Reactant

4 Methanol (Fresh) 165 0.66 1.98


6 Water 549 2.20 6.59 --- Total 1075 4.30 12.90

Output

1

2-Tert butoxy-2-oxo-ethyl (2-2,6 dichlorophenyl)amino)phenyl acetate



3 Methano Loss 165 0.66 1.98 To Atm

4 Methanol Recovered 14 0.05 0.16 Recovered Solvent

Total 1075 4.24 12.73


(D-7) 2-Chloro acetic acid butyl ester



Chemical Formula

Chemical Name

CH3

CH3

OHCH3 +Cl

Cl

O

CH3

CH3

OCH3

Cl

O

tert - butenol Chloroacetyl chloride tert-butyl chloroacetate

MolecularWeight

74 113 150.5

Layer separation Effluent: 4.47 Solid waste:0.40

High vaccum Distillation

N,N Di Methyl Aniline Losss: 0.13

Water: 3.0 Caustic Lye: 0.50

HCl: 0.10

Cooling Tert-Butyl alcohol: 1.0

Chloro Acetyl chloride: 1.40

N,N Di Methyl Aniline:1.63 Sodium Sulphate: 0.20

1.33 kg of 2-Chloro acetic acid butyl ester

(Finished Product)

Recovered N,N Di Methyl Aniline: 1.50



Summary of mass balance for 2-Chloro acetic acid butyl ester is given in Table .

Summary of Mass Balance – 2-Chloro acetic acid butyl ester


batch size kg : 100



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Tert-Butyl alcohol 75.19 0.30 0.90

2 Chloro Acetyl chloride 105.26 0.42 1.26 Reactant

3 N,N Di Methyl Aniline 122.56 0.49 1.47 Solvent

4 Conc-Hydrochloric acid 7.52 0.03 0.09

5 Sodium sulphate 15.04 0.06 0.18 Reactant

6 Water 225.56 0.90 2.71 ---

7 Caustic lye 37.59 0.15 0.45 Neutralizing Agent

Total 588.72 2.35 7.06

Output

1 2-Chloroacetic acid t-butyl ester 100.00 0.40 1.20 Finished

Product

2 N,N Di Methyl Aniline (Recovered) 112.78 0.45 1.35 Recovered

Solvent 3 Effluent 336.09 1.34 4.03 To ETP


5 N,N Di Methyl Aniline Loss 9.77 0.04 0.12 To Atm

Total 588.72 2.35 7.06


(D-8) Di Benzo suberone


100 kg of Di Benzo suberone (Finished Product)

Reaction vessel

Cooling & filtration

Autoclave


Layer separation

Water: 4.0 Sodium Hydroxide: 0.20

Raney Ni: 25 Water:667

Phenyl acetic acid: 167 Pthalic anhydride: 167

Sodium acetate: 5 HCl: 33


283

Raney Ni (Recovered): 23

Methanol (Recovered): 283 Heating

Reaction vessel Phosphorus pentoxide:

70Phosphoric acid: 58

Xylene (Fresh): 33 Xylene (Recovered):

267

Cooling & Layer separation



Xylene(Recovered): 23

Methanol Loss: 50 Xylene Loss: 2


b) Reaction Chemistry Stage -I

ChemicalFormula

ChemicalName

COOH

+ O

O

O

O

O

Phenyl acetic acid Phthalic anhydride (3Z)-3-benzylidene-2-benzofuran-1(3H)-one

MolecularWeight

136 148 222

Stage -II

ChemicalFormula

ChemicalName

(3Z)-3-benzylidene-2-benzofuran-1(3H)-one

O

O

OH

O

2-(2-phenylethyl)benzoic acid

+Raney NiNaOH solution

HCl solution

MolecularWeight

222 226

Stage -III

ChemicalFormula

ChemicalName


OH

O

+ P2O5 + H3PO4

Xylene

O

Dibenzo suberone

MolecularWeight

226 142 208

c) Summary of mass balance Summary of mass balance for Di benzo Suberone is given in Table.


Summary of Mass Balance – Di benzo Suberonecapacity of Finished Product MT/Month : 3.00

batch size kg : 100




Remarks

Input

1 Phenyl acetic acid 167 1.67 5.00

2 Pthalic anhydride 167 1.67 5.00

3 Sodium acetate 5 0.05 0.15

Reactant

4 Methanol (fresh) 50 0.50 1.50

5 Methanol (Recovered) 283 2.83 8.50 Solvent

6 Raney Ni 23 0.23 0.69 Catalyst

7 Sodium Hydroxide 33 0.33 1.00

8 Hydrochloric acid 33 0.33 1.00

9 Phosphorus pentoxide 70 0.70 2.10

10 Phosphoric acid 58 0.58 1.75

Reactant

11 Xylene (fresh) 33 0.33 1.00

12 Xylene (Recovered) 267 2.67 8.00 Solvent

13 Water 667 6.67 20.00 --

14 Raney Ni (fresh) 2 0.02 0.06 Solvent Total 1858 18.58 55.75

Output

1 Dibenzo suberone 100 1.00 3.00 Finished Product

2 Effluent 1100 11.00 33.00 To ETP

3 Raney Ni 23 0.23 0.69 Reuse

4 Methanol (Recovered) 283 2.83 8.50 Recovered Solvent


6 Rec. Xylene 267 2.67 8.00 Recovered Solvent

7 Xylene Loss 33 0.33 1.00 To Atm

8 Raney Ni (loss) 2 0.02 0.06

Total 1858 18.58 55.75


(D-9) Di Benzo Suberenone a) Material Balance Diagram:

Reaction vessel

Cooling & filtration Effluent: 1.0

Autoclave

Layer separation

Water: 285.71 Sodium Hydroxide:

28.57

Phenyl acetic acid: 142.86

Pthalic anhydride: 142.86 Sodium acetate: 4.29

HCl: 28.57

Methanol (Fresh):42.86 Methanol (Recovered):

314.29

Heating

Reaction vessel Phosphorus pentoxide:

71.43 Phosphoric acid: 57.14

Xylene (Fresh): 28.57 Xylene (Recovered):400

Cooling & Layer separation

Aqueous Layer (Effluent): 661.43


Xylene (Recovered): 400

100 kg of Di Benzo suberenone

(Finished Product)

Methanol Loss: 42.86 Xylene Loss:

28.57



Stage -I

Chemical Formula

Chemical Name

COOH

+ O

O

O

O

O

Phenyl acetic acid Phthalic anhydride (3Z)-3-benzylidene-2-benzofuran-1(3H)-one

MolecularWeight

136 148 222

Stage -II

Chemical Formula

Chemical Name

(3Z)-3-benzylidene-2-benzofuran-1(3H)-one

O

O

OH

O

NaOH solution

HCl solution

2-[(E)-2-phenylethenyl]benzoic acid

MolecularWeight

222 224

Stage -III

Chemical Formula

Chemical Name


OH

O

+ P2O5 + H3PO4

Xylene

O

Dibenzo suberenone

MolecularWeight

224 206



Summary of mass balance for Di benzo Subererone is given in Table.

Summary of Mass Balance – Di benzo Subererone


batch size kg : 100



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Phenyl acetic acid 142.86 1.43 4.29

2 Pthalic anhydride 142.86 1.43 4.29

3 Sodium acetate 4.29 0.04 0.13

Reactant

4 Sodium Hydroxide 28.57 0.29 0.86 Solvent

5 Hydrochloric acid 28.57 0.29 0.86

6 Phosphorus pentoxide 71.43 0.71 2.14

7 Phosphoric acid 57.14 0.57 1.71

Reactant

8 Xylene (fresh) 28.57 0.29 0.86

9 Xylene (Recovered) 400.00 4.00 12.00 Solvent

10 Water 285.71 2.86 8.57 ---

11 Methanol (fresh) 42.86 0.43 1.29

12 Methanol (Recovered) 314.29 3.14 9.43 Solvent

Total 1547.14 15.47 46.41

Output

1 Dibenzo suberenone 100.00 1.00 3.00 Finished Product

2 Effluent 661.43 6.61 19.84 To ETP

3 Methanol (Recovered) 314.29 3.14 9.43 Recovered Solvent

4 Methanol Loss 42.86 0.43 1.29 To Atm

5 Rec. Xylene 400.00 4.00 12.00 Recovered Solvent

6 Xylene Loss 28.57 0.29 0.86 To Atm

Total 1547.14 15.47 46.41


(D-10) Fex-10




Stage -I

ChemicalFormula

ChemicalName

COOMe

CH3CH3

ClO

NHOH

+COOMe

CH3CH3

O

NOH

MIBK

DNS

methyl 2-[4-(4-chlorobutanoyl)phenyl]-2-methylpropanoate

Azacyclon

FEX -10

Molecular Weight

282.5 267 514


Summary of mass balance for Fex-10 is given in Table.

Summary of Mass Balance – Fex-10


batch size kg : 200



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 4-(-4-Chloro 1-Oxobutyl)2,2, di methyl phenyl a. acid 180 1.00 10.00


3 Methanol 640 3.56 35.56

4 Sodium Carbonate 15 0.08 0.83

Reactant

5 MIBK 1600 8.89 88.89 Solvent

6 Potassium Bi Carbonate 120 0.67 6.67

7 Potassium Iodide 1 0.01 0.06 Reactant

8 Retarter Solvent 1200 6.67 66.67 Solvent

9 Purified water 300 1.67 16.67 ----

10 Azacyclonol 160 0.89 8.89 Reactant Total 5016 27.87 278.67


Output

1 Fex-10 200 1.11 11.11 Finished Product


3 Rec MIBK 1400 7.78 77.78 Recovered Solvent

4 Rec Retarter 1100 6.11 61.11 Reused

5 Solid waste 600 3.33 33.33 To TSDF

6 Ethanol as waste 300 1.67 16.67

7 Waste Hydrochloric Acid 600 3.33 33.33 To ETP

Total 5016 27.87 278.67

(E-1) 2-Amino Pyridine

a)Mass balance Diagram:

Reaction Vessel


Cooling & Layer Separation

Toluene:1500 Pyridine:200

Sodium amide:60

Organic Layer

HVD

Toluene Layer:1400 Toluene Loss:100

190 kg of Pure 2 Amino Pyridine

Aq. Layer:20 Effluent:400

Water:400



Chemical Formula

Chemical Name

N

+NaNH2

Toluene

N NH2

Pyridine sodamide 2-Amino pyridine

Molecular Weight

79 39 94

c) Summary of mass balance Summary of mass balance for 2-Amino Pyridine is given in Table.

Summary of Mass Balance – 2-Amino Pyridine


batch size kg : 190



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Pyridine 200 1.05 2.11

2 Sodamide 60 0.32 0.63 Reactant



5 Water 400 2.11 4.21 --- Total 2160 11.37 22.74

Output

1 2-Amino Pyridine 190 1.00 2.00 Finished Product




5 Solid waste after high vacuum distillation 50 0.26 0.53 To TSDF

Total 2160 11.37 22.74


(E-2) 2-Bromo Pyridine

a) Material Balance Diagram


Step-1:

Chemical Formula

Chemical Name

N NH2

+NaNO2

N Br

HBrCuBr

2-Amino pyridine 2-Bromo Pyridine

Molecular Weight

94 158

Quenching

Stirring

Aqueous Layer

180 kg of 2-Bromo Pyridine

Recovered Chloroform:700

Chloroform Loss:100

Stirring2-Amino Pyridine:125 Acetic Acid:250

Liquid Bromine:200

Sodium carbonate:25

Chloroform:800 Water: 500

Extraction

Organic Layer

HVD

Efluent:880


Step-2:

Chemical Formula

Chemical Name N

HNH

ToluenePd/C ( 5%)

40 -45 °C4-5 kg pressure

Molecular Weight

159 161


Summary of mass balance for 2-Bromo Pyridine is given in Table.

Summary of Mass Balance – 2-Bromo Pyridine


batch size kg : 150



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 2-Amino Pyrdine 200 1.11 2.22

2 Liq Bromine 250 1.39 2.78

3 Acetic acid 500 2.78 5.56

Reactant

4 water 100 0.56 1.11 ---


6 Chloroform(Recovered) 25 0.14 0.28 Solvent

7 Sodium Nitrate 200 1.11 2.22 Reactant

Total 1900 10.56 21.11

Output

1 2-Bromo Pyridine 180 1.00 2.00 Finished Product


3 Rec Chloroform 700 3.89 7.78 Recovered Solvent


4 Chloroform Loss 100 0.56 1.11 To Atm

5 residue after distillation 40 0.22 0.44 To TSDF

Total 1900 10.56 21.11

(E-3) 3[2(3-Chloro Phenyl) Ethyl]-2-Cyano Pyridine


Chilling

Heat to reflux

Methanol (Recovered): 450

Methanol Loss: 150

Cooling Water: 1000

Sulfuric Acid: 900 Ice: 800

Methanol (Fresh):150 Methanol (Recovered): 450

Sodium Methoxide: 30 Methyl Nicotinate: 155

Meta chloro Benzyl cyanide: 150

Heating followed by cooling & Centrifuge

Effluent: 500

Ammonia solution: 450 Effluent (Aqueous Layer): 800

Ammonification & Layer separation

Reaction mass MEG (Fresh): 100 MEG (Recovered): 700 Hydrazine Hydrate: 60

Caustic Lye: 250

Toluene (Fresh): 100 Toluene (Recovered): 1100

Effluent (Aqueous Layer): 1000

Ammonification & Layer separation

Toluene (Recovered): 1100 Toluene Loss: 100


High vaccum Distillation

120 kg of 3[2(3-Chloro Phenyl) Ethyl]-2-Cyano Pyridine (Finished Product)

MEG(Recovered):700 MEG Loss: 700

Heating Acetic Acid: 135

Hydrogen Peroxide: 156 Water: 1500

Cooling & Chilling Di Methyl Carbonyl

chloride: 130 Sodium Cyanide: 65


High vaccum distillation

Distillation residue:40

Chloroform (Fresh): 200 Chloroform (Recovered):

800

Liquid – Liquid extraction


Chloroform Loss: 200

Heating

Aqueous Layer (Effluent):1000

Acetonitrile: 100

Liquid – Liquid extraction

High M/C Acetonitrile: 80


Water: 2000 IPA (Fresh): 70

IPA (Recovered): 480 Heating followed

by cooling & centrifuge

IPA (Fresh): 50

IPA (Recovered): 480 IPA Loss: 120

Centrifuge



Stage -I

Chemical Formula

Chemical Name

CNCl

+N

MeOOC

CH3ONa

Methanol

N

CN OCl

m-Chloro benzyl Cyanide Methyl nicotinate 2-(3-chlorophenyl)-3-oxo-3-(pyridin-3-yl)propanenitrile

MolecularWeight

151.5 137 256.5

Stage -II

Chemical Formula

Chemical Name

N

CN OCl

+ H2SO4

N

OCl

2-(3-chlorophenyl)-3-oxo-3-(pyridin-3-yl)propanenitrile 2-(3-chlorophenyl)-1-(pyridin-3-yl)ethanone

MolecularWeight

256.5 98 231.5

Stage -III

Chemical Formula

Chemical Name

N

Cl

N

OCl

+ NH2NH2H2ONaOH Solution

2-(3-chlorophenyl)-1-(pyridin-3-yl)ethanone 3-[2-(3-chlorophenyl)ethyl]pyridine

MolecularWeight

231.5 50 217.5

Stage -IV

Chemical Formula

Chemical Name

N

Cl

3-[2-(3-chlorophenyl)ethyl]pyridine

N

Cl

3-[2-(3-chlorophenyl)ethyl]pyridine

Acetic acid

+ H2O2

O

N -Oxide

MolecularWeight

217.5 34 233.5

Stage -V


Chemical Formula

Chemical Name

N

Cl

O

N

Cl

NCDMCC

NaCN+

3-[2-(3-chlorophenyl)ethyl]pyridineN -Oxide

3-(2-(3-Chlorophenyl)etyl )2-Cyano pyridine

MolecularWeight

233.5 49 258.5


Summary of mass balance for 3[2(3-Chloro Phenyl) Ethyl]-2-Cyano Pyridine is given

in Table.

Summary of Mass Balance – 3[2(3-Chloro Phenyl) Ethyl]-2-Cyano Pyridine


batch size kg : 120



Kg/BatchKg/Kg

ofProduct

MT/MonthRemarks

Input

1 Meta chloro Benzyl cyanide 150 1.25 2.50

2 Methyl Nicotinate 155 1.29 2.58 Reactant

3 Methanol (Fresh) 150 1.25 2.50

4 Methanol (Recovered) 450 3.75 7.50 Solvent

5 Sodium Methoxide 30 0.25 0.50 Reactant

6 Ice 800 6.67 13.33

7 Water 4500 37.50 75.00 ---


9 Ammonia Solution 450 3.75 7.50 Reactant

10 Mono Ethyl Glycol (Fresh) 100 0.83 1.67

11 Mono Ethyl Glycol (Recovered) 700 5.83 11.67 Solvent


13 Hydrazien Hydrate 60 0.50 1.00 Reactant

14 Toluene (Fresh) 100 0.83 1.67 Solvent


15 Toluene (Recovered) 1100 9.17 18.33

16 Hydrogen Peroxide 156 1.30 2.60

17 Acetic acid 135 1.13 2.25 Reactant


19 Chloroform (Recovered) 1300 10.83 21.67 Solvent

20 Acetonitrile 100 0.83 1.67

21 Di Methyl Carbonyl chloride 130 1.08 2.17

22 Sodium Cyanide 65 0.54 1.08

Reactant


24 Iso Propyl Alcohol (Recovered) 480 4.00 8.00 Solvent

Total 12581 104.84 209.68

Output

1 3[2(3-Chloro Phenyl )Ethyl]-2-Cyano Pyridine 120 1.00 2.00 Finished



4 Residue after solvent recovery 40 0.33 0.67 To TSDF



Solvent

7 High M/C Acetonitrile 80 0.67 1.33 Reused

8 Rec Mono Ethyl Glycol 700 5.83 11.67

9 Rec Chloroform 1300 10.83 21.67 Recovered

Solvent

10 Mono Ethyl Glycol Loss 700 5.83 11.67

11 Toluene Loss 100 0.83 1.67



14 Methanol Loss 150 1.25 2.50

To Atm

Total 12581 104.84 209.69


(E-4) 3[2(3-Chloro Phenyl )Ethyl]- Pyridine 2-Carboxylic acid



ChemicalFormula

ChemicalName

N

Cl

NC N

Cl

HOOC

+ H2SO4

3-[2-(3-chlorophenyl)ethyl]pyridine-2-carbonitrile 3-[2-(3-chlorophenyl)ethyl]pyridine-2-carboxylic acid

MolecularWeight

242.5 98 261.5



Summary of mass balance for 3[2(3-Chloro Phenyl )Ethyl]- Pyridine 2-Carboxylic acid

is given in Table.

Summary of Mass Balance – 3[2(3-Chloro Phenyl )Ethyl]- Pyridine 2-Carboxylic acid


batch size kg : 220



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 3-(2-Chloro Phenyl )ethyl 2-cyano pyridine 200 0.91 1.82


Reactant

3 Ice 800 3.64 7.27

4 Water 500 2.27 4.55 ----

5 Caustic Lye 300 1.36 2.73 NeutralizingAgent

Total 2250 10.23 20.45

Output

1 3-(-2-Chloro Phenyl)ethyl Pyridine carboxylic acid 220 1.00 2.00 Finished


Total 2250 10.23 20.45


(E-5) Iso Nicotinic acid

a) Material balance Diagram:

Heating

Stirring & Heating

Cooling & Centrifuge

Iso nicotinic acid crude

Process Water:500 Iso nicotinic acid crude

180 KG of Iso Nicotinic

Filtration

Heating to Dissolve

Drying

Acidic water as effluent:80

Effluent:1700

Centrifuge

Ammonia Liquid:500

ReactionSulfuric acid:400 Nitric acid:300

4-Methyl Pyridine:200


b) Reaction Chemistry :

Chemical Formula

Chemical Name

N

CH3

+ HNO 3

N

COOH

4-Methyl Pyridine Iso nicotinic acid

Suphuric Acid

Nitric AcidMolecular

Weight 93 63 123


Summary of mass balance for Iso Nicotinic Acid is given in Table.

Summary of Mass Balance – Iso Nicotinic Acid


batch size kg : 180



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 4-Methyl Pyridine 200 1.11 2.22

2 Nitric acid 300 1.67 3.33

3 Sulphuric acid 400 2.22 4.44

4 Liq. ammonia 560 3.11 6.22

Reactant

5 Water 500 2.78 5.56 --- Total 1960 10.89 21.78

Output

1 Isonicotinic acid 180 1.00 2.00 Finished Product

2 Effluent 1700 9.44 18.89

3 Acidic water as effluent 80 0.44 0.89 To ETP

Total 1960 10.89 21.78


(E-6) 8-Chloro Azatidine


Heating

Reflux

Cooling & TemperatureMaintaining

Cooling

Toluene: L5:

Layer Separation

Layer Separation

Cooling

Cooling & Centrifuge

Aqueous Layer

Organic Layer

THF:NMCP:

Water: Ammonia Solution:

Aqueous Layer

Reaction Ethylene Bromide:

THF:Iodine:

Mg Turning

CFML as Waste

Cooling Boric Acid:


b) Reaction Chemistry :

Step-I

ChemicalFormula

Chemical Name

N

Cl

NC

+N

CH3

MgCl

THF

TolueneSulphuric acid

N

Cl

N

O

CH3

3-[2-(3-chlorophenyl)ethyl]pyridine-2-carbonitrile Gignard reagent{3-[2-(3-chlorophenyl)ethyl]pyridin-2-yl}(1-methylpiperidin-4-yl)methanone

Heating & TemperatureMaintaining

Cooling & Quenching

Stirring Ammonia:Toluene:

HeatingExtraction

TolueneDegassing

Aqueous Layer

Stirring, Cooling, Filtration, Drying

8-ChloroAzatrdine


MolecularWeight

242.5 157.5 342.5

Step-II

Chemical Formula

Chemical Name {3-[2-(3-chlorophenyl)ethyl]pyridin-2-yl}(1-methylpiperidin-4-yl)methanone

N

Cl

N

O

CH3

Oleum

Sulphuric acidLiquor Ammonia

N

N

Cl

CH3

8-Chloro azatidine

MolecularWeight

342.5 324.5



Summary of mass balance for 8-Chloro Azatidine is given in Table.

Summary of Mass Balance – 8-Chloro Azatidine


batch size kg : 100



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 3-(2-Chloro Phenyl )ethyl 2-cyano pyridine 125.00 1.25 2.50

2 N-Methyl-4-Chloro Piperidine 125.00 1.25 2.50

3 Magnesium Turning 30.00 0.30 0.60

Reactant

4 Tetra Hydro Furane 540.00 5.40 10.80 Solvent

5 Iodine 0.10 0.00 0.00

6 Ethylene Bromide 3.00 0.03 0.06 Reactant

7 Water 1500.00 15.00 30.00 ---

8 Hydrochloric Acid 450.00 4.50 9.00

9 Oleum 900.00 9.00 18.00

10 Boric acid 200.00 2.00 4.00

11 Ammonia Solution 900.00 9.00 18.00

Reactant

12 Toluene(Fresh) 100.00 1.00 2.00

13 Toluene(Recovered) 1100.00 11.00 22.00

14 N-Hexane(Fresh) 100.00 1.00 2.00

15 N-Hexane (Recovered) 700.00 7.00 14.00

Solvent

Total 6773.1 67.73 135.46

Output

1 Methyl Loratadine 100 1.00 2.00 Finished Product

2 Effluent 4083 40.83 81.66 To ETP

3 Solid waste after distillation of solvents 50 0.50 1.00 To TSDF



5 Rec N-Hexane 700 7.00 14.00 Solvent

6 Toluene Loss 100 1.00 2.00

7 N-Hexane Loss 100 1.00 2.00 To Atm

8 Waste Tetra Hydro Furan 500 5.00 10.00 To TSDF

9 THF Loss 40 0.40 0.80

Total 6773 67.73 135.46


(E-7) Keto loratadine



b) Reaction Chemistry:

Chemical Formula

Chemical Name

N

Cl

HOOC

+ SOCl2 + AlCl3

MDC N

O

Cl

3-[2-(3-chlorophenyl)ethyl]pyridine-2-carboxylic acid KetoLoratadine

MolecularWeight

261.5 119 243.5


Summary of mass balance for Keto-Loratadine is given in Table.

Summary of Mass Balance – Keto-Loratadine


batch size kg : 50



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 3-(2-Chloro Phenyl )ethyl 2-cyano pyridine 100 2.00 4.00

2 Water 3000 60.00 120.00


Reactant


5 Methylene Di Chloride (Fresh) 100 2.00 4.00

6 Methylene Di Chloride (Recovered) 2400 48.00 96.00 Solvent

7 Thionyl chloride 150 3.00 6.00

8 Aluminium chloride 80 1.60 3.20 Reactant

9 Ice 1200 24.00 48.00 ---

10 Ethyl acetate (Fresh) 100 2.00 4.00

11 Ethyl acetate (Recovered) 1400 28.00 56.00

Solvent



13 Iso Propyl Alcohol (Recovered) 880 17.60 35.20

14 A.Carbon 5 0.10 0.20 Catalyst

Total 9910 198.20 396.40

Output

1 Keto Loratadine 50 1.00 2.00 Finished Product

2 Effluent 4613 92.26 184.52 To ETP

3 Residue after solvent recovery 25 0.50 1.00 To TSDF

4 Hydrochloric Acid Gas 210 4.20 8.40 ToScrubber

5 Waste A.Carbon mixed Hyflo 12 0.24 0.48 To TSDF

6 Rec Ethyl acetate 1400 28.00 56.00

7 Rec Methylene Di Chloride 2400 48.00 96.00


Recovered Solvent

9 Loss Methylene Di Chloride 100 2.00 4.00

10 Loss Iso Propyl Alcohol 120 2.40 4.80

11 Loss Ethyl acetate 100 2.00 4.00

To Atm

Total 9910 198.20 396.40


(F) 4-Chloro-4-Fluoro Butyrophenone


Mass Balance Diagram- APCM

4 chloro butyryl chloride: 85.71

MDC(Fresh): 57.14

MDC(Recovered): 257.14 Aluminium Chloride:114.29

Fluoro benzene: 57.14

Quenching

Cooling and Layer Separation

Water: 514.29 Conc- HCl:

57.14

MDC LayerCharcoal: 5.7

Filteration

100 kg of 4-Chloro-4-Fluoro Butyrophenone

(Finished Product)

MDC(Recovered): 257.14 MDC Loss: 57.14

Solid Waste : 17.14

Effluent: 694.29 HCl: 22.86

Water ScrubbingWater: 0.90

HCl gas: 0.40 Hydrochloric Acid: 1.30



ChemicalFormula

ChemicalName

F + Cl

Cl

O AlCl3 FCl

O

Fluoro Benzene Chloro butryl chloride 4-Chloro 4-Fluoro butyrophenone

MolecularWeight

96 141 200.5


Summary of mass balance for 4-Chloro-4-Fluoro Butyrophenone is given in Table.

Summary of Mass Balance – 4-Chloro-4-Fluoro Butyrophenone


batch size kg : 100


Quantity Sr. No.

Name of Raw Material Kg/Batch

Kg/Kgof

Product MT/Month

Remarks

Input

1 Fluoro benzene 57.14 0.57 1.14

2 4-Chloro butyryl chloride 85.71 0.86 1.71

3 Aluminium chloride 114.29 1.14 2.29

Reactant

4 Methylene Di Chloride(Fresh) 57.14 0.57 1.14

5 Methylene Di Chloride(Recovered) 257.14 2.57 5.14

Solvent

6 Water (Ice) 514.29 5.14 10.29 ---

7 Conc-Hydrochloric Acid 57.14 0.57 1.14 Reactant

8 Charcoal 5.71 0.06 0.11 Catalyst

Total 1148.57 11.49 22.97

Output

1 4-Chloro 4-Fluoro butyrophenone 100.00 1.00 2.00 Finished Product


2 Effluent 694.29 6.94 13.89 To ETP

3 Methylene Di Chloride (Recovered) 257.14 2.57 5.14 Recovere

d Solvent 4 Methylene Di Chloride Loss 57.14 0.57 1.14 To Atm


6 Hydrochloric Acid gas 22.86 0.23 0.46 ToScrubber

Total 1148.57 11.49 22.97

Summary of Mass Balance-4-Chloro-4-Fluoro Butyrophenone APCM





2 Hydrochloric Acid Gas 22.86 0.229 0.4571 To Scrubber

Total 76.19 1.524 3.0476


1 Hydrochloric Acid (30 %) 76.19 0.762 1.5238 Sale as By Product

Total 76.19 0.762 1.5238


(G-1) N-(2,6 Di methyl phenyl )-2-(Piperazinyl) acetamide

a) Mass Balance Diagram:

MDC Layer

Distillation Cyclohexane (Fresh): 12.5 Cyclohexane(Recovered):

112.5

Solid Waste: 6.3 Centrifuge and Drying under

vaccum

50 kg of N-(2,6 Di methyl phenyl )-2- (Piperazinyl) acetamide

(Finished Product)

MDC Recovery:390.6

Cyclohexane Recovery: 112.5

Water + IPA: 802.5

Dimer: 43.8

MDC Loss:100 Cyclohexane Loss:12.5

N-(2,6 Di methyl phenyl) 62.5 Chloro acetamide: 1.0

IPA: 350 MDC: 100

MDC Recovered: 390.6 Anhydrous Piperazine:

108.8 Water: 375

Sodium Sulphate: 6.3

Stirring Cooling followed by layer

separation



Step-I

Chemical Formula

Chemical Name

NH2

CH3

CH3

NH

CH3

CH3

ClO+

Cl

O

Cl

Toluene

K2CO3

2,6-dimethylaniline chloroacetyl chloride 2-chloro-N-(2,6-dimethylphenyl)acetamide

MolecularWeight

Step-II

Chemical Formula

Chemical Name

NH

CH3

CH3

ClO

2-chloro-N-(2,6-dimethylphenyl)acetamide

NH

CH3

CH3

O

NNH+

NH

NH

IPA

N-(2,6-dimethylphenyl)-2-(piperazin-1-yl)acetamide

PIperazine

MolecularWeight


C) Summury of Mass Balance: capacity MT/month 1

batch size kg 50

Working Days 26

Quantity Sr. No.

Name of Raw Material

Kg/Batch Kg/Kg of Product

MT/Month

Input

1N-(2,6 Di methyl phenyl) 2-Chloro acetamide

62.5 1.3 1.3

2 Anhydrous Piperazine 108.8 2.2 2.2

3 Iso Propyl Alcohol 350.0 7.0 7.0



6 Water 375.0 7.5 7.5

7 Sodium sulphate 6.3 0.1 0.1

8 Cyclo Hexane (Fresh) 12.5 0.3 0.3

9 Cyclo Hexane (Recovered) 112.5 2.3 2.3

Total 1518.1 30.4 30.4

Output

1 N-(2,6 Di methyl phenyl) 2-(piperazinyl) acetamide 50.0

1.0 1.0

2 Dimer of N-(2,6 Di methyl phenyl )-2-(Piperazinyl) acetamide 43.8

0.9 0.9

3 Water+ Iso Propyl Alcohol 802.5 16.1 16.1

4 Methylene Di Chloride Loss 100.0 2.0 2.0

5 Solid waste 6.3 0.1 0.1

6 CycloHexane(Rec) 112.5 2.3 2.3

7 CycloHexane Loss 12.5 0.3 0.3

8 Methylene Di Chloride(Rec) 390.6 7.8 7.8

Total 1518.1 30.4 30.4


(G-2) N-(2,6 Di methyl phenyl )-2-Chloro acetamide

c) Mass Balace Diagram:

86.2

d) Reaction Chemistry:

Chemical Formula

Chemical Name

NH2

CH3

CH3

NH

CH3

CH3

ClO+

Cl

O

Cl

Toluene

K2CO3

2,6-dimethylaniline chloroacetyl chloride 2-chloro-N-(2,6-dimethylphenyl)acetamide

MolecularWeight

121 113 197.5

e) Summury of Mass Balance:

Stirring

Centrifugeand Water washing

Toluene(Recovered):482.8

IPA(Recovered): 86.2

DryingToluene(Loss):17.2

IPA(Loss): 6.9 Solid Waste:34.5

Water:375 MDC(Fresh):100

MDC(Recovered): 390.6 Soda Carbonate: 29.7

2,6 dimethyl aniline: 34.5 Chloro acetyl Chloride: 38.6

IPA(Fresh): 6.9 IPA(Recovered): 86.2

Toluene:500

50 kg of N-(2,6 Di methyl phenyl )-2- Chloro acetamide

(Finished Product)



Kg/BatchKg/Kg

ofProduct

MT/Month Remarks

Input

1 2,6 dimthyl aniline 34.5 0.7 0.7

2 Chloro acetyl chloride 38.6 0.8 0.8

3 DM water 758.6 15.2 15.2

Reactant

4 Toluene (Fresh) 17.2 0.3 0.3

5 Toluene (Recovered) 482.8 9.7 9.7 Solvent

6 Soda carbonate 29.7 0.6 0.6 ---

7 Iso Propyl Alcohol (Fresh) 6.9 0.1 0.1 Solvent

8 Iso Propyl Alcohol (Recovered) 86.2 1.7 1.7 Reactant

Total 1454.5 29.1 29.1

Output

1 N-(2,6 Di methyl phenyl) 2-Chloro acetamide 50.00 1.0000 1.0000 Finished

Product 2 Effluent 776.9 15.5 15.5 To ETP

3 Toluene 482.8 9.7 9.7

4 Iso Propyl Alcohol 86.2 1.7 1.7 Recovered

Solvent

5 Solid waste 34.5 0.7 0.7 To TSDF

6 Toluene Loss 17.2 0.3 0.3 ---

7 Iso Propyl Alcohol Loss 6.9 0.1 0.1 --- Total 1454.5 29.1 29.1


(H-1) 5 - Chloro 1-(-4-Piperidinyl)-2-Benzimidazolone


N-Carbethoxy-4-Amino Piperidine : 160

2,5 DiChloro Nitro Benzene: 160

Sodium Carbonate: 125 Potassium Iodide: 1.0

Water: 4000 Raney Nickel fresh:2


Centrifuge Methanol(Fresh):600 Methanol(Recovered):

2400

Heating Reflux Raney Nickel: 8 Hydrazine Hydrate: 100

Nickel Filtration and Mass Transfer

R.Nickel Recovered : 8

Methanol Recovery followed by Chilling, Centrifuge and Drying

Recovered Methanol: 2400

Heating and Cooling

Urea: 120 Caustic Lye: 600

Water: 3000

A.Carbon : 20 HCl: 800 Hyflo: 15

Filtration followed by chilling and centrifuge

Effluent: 13721

Heating followed by filtration ,chilling and

centrifuge

Purified Water: 2000

A.Carbon: 10

A.Carbon mixed hyflo: 35

Methanol Loss: 600 Raney Nickel Loss:2


Mass Balance Diagram-APCM:

Purified Water: 3000 IPA(Fresh):150

IPA(Recovered): 1450 Heating, centrifuge

and Drying IPA Recovered: 1450 IPA Loss: 150

A.Carbon: 10 Heating followed by filtration, Methanol Recovery, chilling,

Centrifuge and Drying

Ammonia Gas: 50 Carbon

dioxide:80 Waste: 100

115 kg of 5 - Chloro 1-(-4-Piperidinyl)-2-

Benzimidazolone (Finished Product)

Water for Scrubber: 450

Ammonia Gas: 50 Water Scrubbing Ammonia Solution:500



Step-I

Chemical Formula

Chemical Name

+

NO2

Cl

ClN

NH2

COOEt

NO2

NH

ClN

COOEt

K2CO3

NaI

4-Amino N-CarbethoxyPiperidine 2,4, DiChloro nitrobenzene Ethyl 4(4 -Chloro -2- nitrophenyl)amino) Piperidine -1 -Carboxylate

+ KCl

MolecularWeight

172 192 327.5 74.5

Step-II

Chemical Formula

Chemical Name

NO2

NH

ClN

COOEt

Ethyl 4(4 -Chloro -2- nitrophenyl)amino) Piperidine -1 -Carboxylate

+ NH2NH2H2OMethanol

Raney Ni

NH2

NH

ClN

COOEt

Ethyl 4(4 -Chloro -2- aminophenyl)amino) Piperidine -1 -CarboxylateHydrazine

Hydrate

MolecularWeight

327.5 50 297.5

Step-III

Chemical Formula

Chemical Name

NH2

NH

ClN

COOEt

Ethyl 4(4 -Chloro -2- aminophenyl)amino) Piperidine -1 -Carboxylate

+ NH2CONH 2

WaterCharcoal

NaOH SolutionHCl Solution

MethanolSoda ash

NH

N

ClNH

O

+C2H5OH CO2++ NH3

5-(Chloro -1- (4-Piperidinyl)-2-Benzimidizolone

MolecularWeight

297.5 60 250.5



Summary of mass balance for 5-Chloro 1-(-4-Piperidinyl)-2-Benzimidazolone is given

in Table.

Summary of Mass Balance – 5 - Chloro 1-(-4-Piperidinyl)-2-Benzimidazolone


batch size kg : 115



Kg/BatchKg/Kg

ofProduct

MT/Month Remarks

Input

1 2,5 DiChloro Nitro Benzene 160 1.39 2.78

2 Potassium Iodide 1 0.01 0.02

3 Sodium Carbonate 125 1.09 2.17

Reactant

4 N-Carbethoxy-4-Amino Piperidine 160 1.39 2.78 Solvent

5 Water 12000 104.35 208.70 ---



8 Hydrazine Hydrate 100 0.87 1.74 Reactant


10 Urea 120 1.04 2.09 Reactant


12 A.Carbon 20 0.17 0.35 Catalyst

13 Hyflo 15 0.13 0.26 Reactant


15 Iso Propyl Alcohol(Recovered) 1450 12.61 25.22 Solvent


17 Raney Nickel fresh 2 0.02 0.03

Total 18729 162.86 325.72

Output

1 5-Chloro-1-(-4-Piperidinyl)2,3di hydro 1H Benzimidazolone 115 1.00 2.00 Finished

Product


2 Rec Methanol 2400 20.87 41.74

3 Rec Iso Propyl Alcohol 1450 12.61 25.22 Recovered

Solvent

4 Waste Carbon mixed hyflo 35 0.30 0.61 To TSDF

5 Effluent 13721 119.31 238.63 To ETP

6 Haz waste after distillation 100 0.87 1.74 To TSDF

7 Rec R.Nickel 8 0.07 0.14 Reuse

8 Ammonia Gas 50 0.43 0.87 ToScrubber

9 Carbon di oxide 80 0.70 1.39

10 Methanol Loss 600 5.22 10.43


12 Rec R.Nickel loss 2 0.02 0.03

To Atm

Total 18729 162.86 325.72


Summary of Mass Balance-5-Chloro 1-(-4-Piperidinyl)-2-Benzimidazolone APCM





2 Ammonia Gas 50.00 0.435 0.87 To Scrubber

Total 500.00 4.348 8.70


1 Liq. Ammonia 500.00 4.348 8.70 Sale as By Product

Total 500.00 4.348 8.70


(H-2) 3-(3-Chloro Propyl )-2,3 Di hydo1-H-Benzimidazolone




Step-I

ChemicalFormula

Chemical Name

NH2

NH2

+ CH3 OCH3

O O

NH

NO

CH3

CH2

o-Phenelene diamine Methyl acetoacetate 1-(prop-1-en-2-yl)-1,3-dihydro-2H-benzimidazol-2-one

Xylene+ H2O

MolecularWeight

108 116 174 18

Step-II

ChemicalFormula

ChemicalName

XyleneNH

NO

CH3

CH2

+Cl BrN

NH

O

Cl

1-(prop-1-en-2-yl)-1,3-dihydro-2H-benzimidazol-2-one

Bromo Chloro propane

1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one

MolecularWeight

174 157.5 210.5



Summary of mass balance for 3-(3-Chloro Propyl )-2,3 Di hydo1-H-Benzimidazoloneis given in Table.Summary of Mass Balance – 3-(3-Chloro Propyl )-2,3 Di hydo1-H-

Benzimidazolone


batch size kg : 160


Quantity Sr. No. Name of Raw Material Kg/

Batch Kg/Kg of Product

MT /Month

Remarks

Input

1 Xylene(Fresh) 50 0.31 0.63

2 Xylene(Recovered) 750 4.69 9.38 Solvent

3 Methyl aceto acetate 155 0.97 1.94

4 Ortho Phenylene Di Amine 180 1.13 2.25 Reactant


6 Water 1900 11.88 23.75 ----


8 A./Carbon 5 0.03 0.06 Catalyst

9 1,3 Dromo Chloro Propane 135 0.84 1.69

10 Tetra Butyl ammonium bromide 3 0.02 0.04 Reactant

Total 3678 22.99 45.98

Output

1 3(3-Chloro Propyl)2,3 Di Hydro 1H Benzimidazolone 160 1.00 2.00 Finished


3 Solid waste after distillation 50 0.31 0.63

4 Waste A.Carbon mixed Hyflo 10 0.06 0.13 To TSDF

5 Rec Xylene 750 4.69 9.38 Recovered Solvent

6 Xylene Loss 50 0.31 0.63 To Atm Total 3678 22.99 45.98


(I-1) 1,3,5 Tri Methoxy Benzene



Aniline: D.M. Water

Conc. HCBromine: Acetic Acid:

Methanol(Fresh): Methanol(Recovered):

Filtration followed by Drying

Water: Hydrogen Bromide gas: Nitrogen:

Sulphuric Acid: Sodium Nitrite: Drying

Separation DMF(Fresh):

DMF(Recovered): Sodium Methoxide:

Cupric Chloride:

Methanol(Recovered: DMF (Recovered): Methanol Loss: DMF Loss:

Reaction Mass MDC(Fresh): MDC(Recovered):

Water:

Distillation Water

1,3,5 Tri Methoxy Benzene (Finished Product)

MDC(Recovered): MDC Loss:

Solid waste:

Water for Scrubber: 2.0 HBr Gas: 0.90

Water Scrubbing Hydrobromic Acid: 2.90



Reaction Chemistry:

Step-I

Chemical Formula

Chemical Name

NH2

Br

Br

Br

NH2

+ 3 Br2

Acetic acid

Water + 3 HBr

Aniline Bromine 2,4,6 Tri bromo aniline Hydrogen Bromide

MolecularWeight

93 480 330 243

Step-II

Chemical Formula

Chemical Name

NH2

Br

Br

Br

+

2,4,6 Tri bromo aniline Sodium Nitrite

NaNO2

MetthanolBenzene

Sulphuric Acid

Br

Br

Br

1,3,5 Tri bromo benzene

+N2 Na2SO4 + H2O+

MolecularWeight

330 69 315

Step-III

ChemicalFormula

Chemical Name

Br

Br

Br

+

2,4,6 Tri bromo aniline Sodium Methoxide

CH3ONa

OCH3

OCH3

H3CO

1,3,5 Tri Methoxy benzene

+ NaBr3

DMFMethanol

Cupric chloride

Sodium Bromid

Water for Scrubber: 0.17

HBr Gas: 0.05 Caustic: 0.02

Water Scrubbing Sodium Bromide: 0.23


MolecularWeight

315 54 168 309


Summary of mass balance for 1,3,5 Tri Methoxy Benzene is given in Table.

Summary of Mass Balance – 1,3,5 Tri Methoxy Benzene


batch size kg : 50


Quantity Sr. No.

Name of Raw Material Kg/Batch

Kg/Kg of Product MT/Month

Remarks

Input

1 Aniline 45.5 0.9 1.8

2 Bromine 236.4 4.7 9.5

3 Acetic Acid 77.3 1.5 3.1

4 Sodium Nitrite 63.6 1.3 2.5

Reactant

5 Methanol (Fresh) 136.4 2.7 5.5


7 Sulphuric Acid 63.6 1.3 2.5

8 Cupric chloride 13.6 0.3 0.5 Reactant

9 DMF (Fresh) 90.9 1.8 3.6

10 DMF (Recovered) 318.2 6.4 12.7 Solvent

11 Sodium Methoxide 131.8 2.6 5.3

12 Conc-Hydrochloric Acid 45.5 0.9 1.8 Reactant

13 Water 2045.5 40.9 81.8 ----



Solvent

Total 5631.8 112.6 225.3

Output

1 1,3,5 Tri methoxy benzene 50.0 1.0 2.0 Finished Product

2 Water 2045.5 40.9 81.8 To TSDF

3 Methanol(Recovered) 954.5 19.1 38.2


4 DMF(Recovered) 318.2 6.4 12.7 Recovered Solvent

5 Hydrogen bromide (gas) 40.9 0.8 1.6 ToScrubber

6 Nitrogen 563.6 11.3 22.5 To Atm

7 Methylene Di Chloride(Recovered) 1272.7 25.5 50.9 Recovere

d Solvent 8 Solid Waste 22.7 0.5 0.9 To TSDF

9 Methanol Loss 136.4 2.7 5.5

10 DMF Loss 90.9 1.8 3.6

11 Methylene Di Chloride Loss 136.4 2.7 5.5 Total 5631.8 112.6 225.3

Summary of Mass Balance - 1,3,5 Tri Methoxy Benzene APCM

(I-2) 1,3 Di bromo aniline

a) Reaction Chemistry:

Step-I





2 HBr Gas 40.91 0.818 1.64 To Scrubber

Total 131.59 2.632 5.26 Water scrubber Output

1 Hydrobromic Acid (30 %) 131.59 2.632 5.26 Sale as By Product

Total 131.59 2.632 5.26 Alkali scrubber Input

1 Caustic 1.03 0.0009 0.0687 To Scrubber

2 Water 7.56 0.0063 0.5039

3 HBr Gas 2.05 0.0017 0.1364 Scrubbing

Media

Total 10.63 0.0089 0.7090 Alkali scrubber Output

1 Sodium Bromide 10.63 0.0089 0.7090 Sale as By Product

Total 10.63 0.0089 0.7090


ChemicalFormula

Chemical Name

NH2

SO2NH2

NH2

SO2NH2

BrBr

HBrH2O2+ +Water

4-aminobenzenesulfonamide 4-amino-3,5-dibromobenzenesulfonamide

MolecularWeight

172 34 81 330

Step-II

Chemical Formula

Chemical Name

NH2

BrBr

4-amino-3,5-dibromobenzenesulfonamide

NH2

SO2NH2

BrBr

+H2SO4 Steam Distilation

2,6 Dibromo aniline

MolecularWeight

330 98 251



Summary of mass balance for 2,6 Di Bromo Aniline is given in Table.

Summary of Mass Balance – 1,3 Di Bromo Aniline


batch size kg : 25



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Sulphanilamide 29.4 1.2 2.4

2 Hydrogen peroxide 23.5 0.9 1.9

3 Conc-Hydrobromic acid 70.6 2.8 5.6

Reactant

4 Water 1470.6 58.8 117.6 ---

5 Caustic Flakes 29.4 1.2 2.4 Neutralizing Agent

6 Conc –Hydrochloric acid 58.8 2.4 4.7

7 Sulphuric acid 29.4 1.2 2.4 Reactant

8 Cyclohexane Fresh 14.7 0.6 1.2

9 Cyclohexane Recovered 161.8 6.5 12.9 Solvent

Total 1888.2 75.5 151.1

Output

1 1,3 dibromo aniline 25.0 1.0 2.0 Finished Product

2 Effluent 1686.8 67.5 134.9 To ETP

3 Rec Cyclo hexane 161.8 6.5 12.9 Recovered Solvent

4 Cyclo hexane Loss 14.7 0.6 1.2 To Atm

Total 1888.2 75.5 151.1


(I-3) Selenic Ahnydride a) Material balance Diagram

Heating

U/VAC Methanol Recovery

Reaction Vessel Tetra Hydro Furane

IodineMg Turning

Dumping of mass

Aqueous LayerOrganic Layer

THF Recovery

Cooling

Recovered THF:591.3

Centrifuged mass Dioxane

Bromo Benzene

Stirring THF

Selenium

Stirring & Layer Separation

Methanol

MethanolDi methyl Sulfoxide

Chilling

Filtration


Hydrogen Peroxide Cooling

Stirring

Centrifuge

Mother Liquor

Benzene selannic anhydride

Unloading

Azeotrop

Cooling

Filtration Mother Liquor

Drying



Step-I

ChemicalFormula

Chemical Name

Mg Br

+ Se2

Se Se

DiPhenyl diselanideGrignard reagent Sealinium

MolecularWeight

362 79 312

Step-II

ChemicalFormula

Chemical Name

Se Se

DiPhenyl diselanide

SeO

O

2

Benzene selenic anhydrid

MolecularWeight

312 372


c) Summary of mass balance Summary of mass balance for Selenic Anhydride is given in Table.

Summary of Mass Balance – Selenic Anhdride


batch size kg : 40




Remarks

Input

1 Bromo benzene 173.9 4.3 8.7 Reactant

2 Tetra Hydro Furan (Fresh) 121.7 3.0 6.1 3 Tetra Hydro Furan (Recovered) 591.3 14.8 29.6

Solvent

4 Iodine 8.7 0.2 0.4

5 Mg Turnigs 27.8 0.7 1.4

6 Selanium 60.9 1.5 3.0

7 Conc-Hydrochloric acid 208.7 5.2 10.4

8 Ice 347.8 8.7 17.4

9 DMSO 34.8 0.9 1.7

Reactant

10 Methanol (Fresh) 20.0 0.5 1.0


12 Dioxane 87.0 2.2 4.3

13 Hydrogen peroxide 34.8 0.9 1.7 Reactant

14 Toluene (Fresh) 17.4 0.4 0.9

15 Toluene (Recovered) 69.6 1.7 3.5 Solvent

Total 1960.9 49.0 98.0

Output 1 Selenic anhydride

40.0 1.0 2.0 FP

2 Tetra Hydro Furan 591.3 14.8 29.6 To TSDF

3 Effluent 1066.1 26.7 53.3 To ETP

4 Toluene (Recovered) 69.6 1.7 3.5

5 Methanol (Recovered) 156.5 3.9 7.8 Recovered

Solvent

6 Toluene Loss 17.4 0.4 0.9

7 Methanol Loss 20.0 0.5 1.0 To Atm

Total 1960.9 49.0 98.0


(I-4) 2- Nitro Ethanol



Chemical Formula

Chemical Name

CH3 NO2 + (HCHO)nOH

O2N

Nitro methane Paraformaldehyde 2-Nitro Ethanol

Molecular Weight

61 30 91

Nitro Methane : 1771.9 Para formaldehyde: 78.1

Methanolic KOH: 9.4 N-Hexane(Fresh): 25.0

N-Hexane (Recovered): 125.0

Reaction Vessel

Distillation Di phenyl ether(Fresh): 10.0 Di phenyl ether(Recovered): 125.0

Stirring followed by filtration

100 kg of 2-Nitro Ethanol (Finished Product)

Effluent: 1662.5 N-Hexane(Rec):125

N-Hexane(Loss): 25 Solid Waste: 100

Sulphuric Acid: 3.1

Di phenyl ether(Recovered):125

Di phenyl ether Loss: 10



Summary of mass balance for 2-Nitro Ethanol is given in Table.

Summary of Mass Balance – 2-Nitro Ethanol


batch size kg : 100



Kg/Batch Kg/Kg

ofProduct

MT/Month Remarks

Input

1 Nitro methane 1771.9 17.7 35.4

2 Para formaldehyde 78.1 0.8 1.6

3 Sulphuric acid 3.1 0.0 0.1

4 Methanolic KOH (3N) 9.4 0.1 0.2

Reactant

5 Di phenyl ether (Fresh) 10.0 0.1 0.2

6 Di phenyl ether (Recovered) 125.0 1.3 2.5

7 N-Hexane (Fresh) 25.0 0.3 0.5

8 N-Hexane (Recovered) 125.0 1.3 2.5

Solvent

Total 2147.5 21.5 43.0

Output

1 2-Nitro ethanol 100.0 1.0 2.0 Finished Product

2 Di phenyl ether(Recovered) 125.0 1.3 2.5

3 N-Hexane(Recovered) 125.0 1.3 2.5 Recovered

Solvent

4 N-Hexane Loss 25.0 0.3 0.5

5 Di phenyl ether Loss 10.0 0.1 0.2 To Atm

6 Solid waste 100.0 1.0 2.0 To TSDF

7 Effluent 1662.5 16.6 33.3 To ETP

Total 2147.5 21.5 43.0


2.7 SOLVENT RECOVERY SYSTEM

The industry is engaged in the manufacturing of synthetic organic chemicals,

which require solvents during various unit processes. Presently the unit uses

various solvents viz. Methanol, chloroform, Toluene, Benzene, Methylene Di

Chloride, N-Hexane, thionyl chloride, Iso Propyl Alcohol, Ethyl Acetate and after

proposed expansion few more solvents like, Acetone, Heptanes, Cyclo Hexane,

Carbon Tetra Chloride, Mono Ethyl Glycol, Tetra Hydro Furane, and Xylene will

be used.

The spent solvent generated during the manufacturing process will be

recovered by way of distillation and will be reused in the process. The process of

the solvent recovery system is described hereunder;

After completion of the reaction, the whole mass in the reactor will be

pumped to re-boiler through candle filter and then subjected to the

distillation to separate finished product and recover solvent.

Firstly, the mass will be distilled at required temperature where pure solvent

will be distilled out depending on their boiler points and it will be collected in

the recovered solvent storage tank and reused in the process.

The recovered solvent will be reused in the process and residue will be sent

to TSDF site for the disposal by incineration.

Vaccum will also be applied as per requirement during distillation.

The overall requirements and mass balance for the solvent based on mass

balance of each product and summary has been worked out which is given

in Table-2.6 & Table-2.7 respectively. The schematic diagram of the solvent

recovery system is shown in the Drawing- 2.1.

Measures for achieving maximum solvent recovery:

The entire manufacturing activities & distillation process will be carried out

in totally closed system.

Regular maintenance of the pipeline and valves & fittings will be carried

out regularly to avoid any leakages.


Distillation column will be connected with two numbers of condensers

where cooling water and chilled water will be used as media and also

equipped with vaccum system.

The condenser will be provided with the sufficient HTA and residence time

to achieve more than 80% recovery.

During the manufacturing activity as well as during distillation process 11 - 25%

of the total solvent will be lost; approx. 75 - 89% of solvent will be recovered

during the process. The fresh solvent requirement will depend on solvent loss

during distillation as well as manufacturing activity.

Table –2.6: Solvent Consumption & Mass BalanceSolvent requirement,

MT/Month Solvent requirement,% Group

Codeof

ProductSolvent

Fresh Recover Total Fresh Recover Total

Total Spent

Solvent

Methanol 0.18 3.38 3.56 5.00 95.00 100.0 A-1

Chloroform 6.67 121.60 128.27 5.20 94.80 100.0 124.98

Methanol 2.22 4.44 6.67 33.33 66.67 100.0 Toluene 3.33 63.33 66.67 5.00 95.00 100.0 A-2Chloroform 3.33 63.33 66.67 5.00 95.00 100.0

131.11

A-3 Chloroform 13.64 122.73 136.36 10.00 90.00 100.0 122.73 Methanol 2.00 8.67 10.67 18.75 81.25 100.0

A-4Chloroform 3.67 33.33 37.00 9.91 90.09 100.0

42.00

Methanol 2.50 14.00 16.50 15.15 84.85 100.0 A-5

Chloroform 3.00 62.00 65.00 4.62 95.38 100.0 76.00

Methanol 2.00 8.67 10.67 18.75 81.25 100.0 A-6

Chloroform 2.67 73.33 76.00 3.51 96.49 100.0 82.00

Methanol 0.89 2.67 3.56 25.00 75.00 100.0 A-7

Chloroform 6.67 121.60 128.27 5.20 94.80 100.0 124.27

Toluene 28.57 142.86 171.43 16.67 83.33 100.0 A-8

Chloroform 14.29 114.29 128.57 11.11 88.89 100.0 257.14

A-9 N-Hexane 3.33 30.00 33.33 10.00 90.00 100.0 30.00 Chloroform 9.09 127.27 136.36 6.67 93.33 100.0

A-10N-Hexane 9.09 127.27 136.36 6.67 93.33 100.0

254.55

N-Hexane 9.09 127.27 136.36 6.67 93.33 100.0 A-11

Chloroform 9.09 100.00 109.09 8.33 91.67 100.0 227.27

A-12 Toluene 1.36 16.82 18.18 7.50 92.50 100.0 16.82 A-13 N-Hexane 9.09 127.27 136.36 6.67 93.33 100.0 263.64

A

A-13 Chloroform 9.09 100.00 109.09 8.33 91.67 100.0


Solvent requirement, MT/Month Solvent requirement,%

Group Code

of Product

Solvent Fresh Recover Total Fresh Recover Total

Total Spent

Solvent

IPA 4.55 36.36 40.91 11.11 88.89 100.0 Toluene 11.67 75.00 86.67 13.46 86.54 100.0 IPA 6.67 33.33 40.00 16.67 83.33 100.0 A-14 Chloroform 16.67 83.33 100.00 16.67 83.33 100.0

191.67

A-15 Toluene 2.00 30.00 32.00 6.25 93.75 100.0 30.00 Methanol 5.56 50.00 55.56 10.00 90.00 100.0 Chloroform 11.11 55.56 66.67 16.67 83.33 100.0 A-16 N-Hexane 5.56 38.89 44.44 12.50 87.50 100.0

144.44

Max Methanol 5.56 50.00 55.56 10.00 90.00 100.0

Max Toluene 28.57 142.86 171.43 16.67 83.33 100.0 Max Chloroform 16.67 127.27 136.36 12.22 93.33 105.6 Max N-Hexane 9.09 127.27 136.36 6.67 93.33 100.0

Max IPA 6.67 36.36 40.91 16.30 88.89 105.1

263.64

B-1 Toluene 0.78 12.78 13.56 5.74 94.26 100.0 12.78

MDC 0.83 2.50 3.33 25.00 75.00 100.0 N-Hexane 0.83 11.67 12.50 6.67 93.33 100.0 B-2Thyonil chloride 11.67 2.08 13.75 84.85 15.15 100.0

16.25

Toluene 5.00 36.67 41.67 12.00 88.00 100.0 Chloroform 12.50 137.50 150.00 8.33 91.67 100.0 B-3Acetone 3.33 26.67 30.00 11.11 88.89 100.0

200.83

B-4 Toluene 1.47 11.76 13.24 11.11 88.89 100.0 11.76 B-5 Toluene 8.33 158.33 166.67 5.00 95.00 100.0 158.33

Toluene 33.33 633.33 666.67 5.00 95.00 100.0 B-6

MDC 33.33 166.67 200.00 16.67 83.33 100.0 800.00

B-7 Methanol 2.22 25.56 27.78 8.00 92.00 100.0 25.56 B-8 Methanol 10.00 40.00 50.00 20.00 80.00 100.0 40.00

Chloroform 25.00 100.00 125.00 20.00 80.00 100.0 Methanol 10.00 70.00 80.00 12.50 87.50 100.0 B-9IPA 10.00 70.00 80.00 12.50 87.50 100.0

240.00

B-10 Methanol 2.78 25.00 27.78 10.00 90.00 100.0 25.00 B-11 Methanol 6.67 60.00 66.67 10.00 90.00 100.0 60.00

Methanol 13.33 66.67 80.00 16.67 83.33 100.0 Chloroform 13.33 120.00 133.33 10.00 90.00 100.0 Acetone 13.33 66.67 80.00 16.67 83.33 100.0

B-12

N-Hexane 13.33 93.33 106.67 12.50 87.50 100.0

346.67

B

B-13 Methanol 2.78 25.00 27.78 10.00 90.00 100.0 25.00



Group Code

of Product


Total Spent

Solvent

B-14 Acetone 11.43 34.29 45.71 25.00 75.00 100.0 34.29 B-15 Chloroform 33.33 133.33 166.67 20.00 80.00 100.0 133.33 B-16 Toluene 6.25 65.25 71.50 8.74 91.26 100.0 65.25

Toluene 10.00 150.00 160.00 6.25 93.75 100.0 IPA 8.00 80.00 88.00 9.09 90.91 100.0 B-17Tetra Hydro Furan 18.00 36.00 54.00 33.33 66.67 100.0

266.00

Toluene 57.14 228.57 285.71 20.00 80.00 100.0 IPA 16.00 142.86 158.86 10.07 89.93 100.0 B-18Tetra Hydro Furan 16.00 40.00 56.00 28.57 71.43 100.0

411.43

Toluene 33.33 244.44 277.78 12.00 88.00 100.0 B-19 Iso propyl

Alcohol 22.22 111.11 133.33 16.67 83.33 100.0 355.56

B-20 Toluene 50.00 200.00 250.00 20.00 80.00 100.0 200.00 B-21 MDC 5.56 50.00 55.56 10.00 90.00 100.0 50.00

Toluene 22.67 17.33 40.00 56.67 43.33 100.0 B-23 Tetra Hydro

Furan 36.00 36.00 72.00 50.00 50.00 100.0 53.33

Acetone 12.50 50.00 62.50 20.00 80.00 100.0 B-24

Methanol 25.00 100.00 125.00 20.00 80.00 100.0 150.00

Max Toluene 57.14 633.33 690.48 8.28 91.72 100.0

Max Methylene Dichloride 33.33 166.67 200.00 16.67 83.33 100.0 Max N-Hexane 13.33 93.33 106.67 12.50 87.50 100.0

Max Chloroform 33.33 137.50 170.83 19.51 80.49 100.0 Max Acetone 13.33 66.67 80.00 16.67 83.33 100.0

Max Methanol 25.00 100.00 125.00 20.00 80.00 100.0 Max Iso propyl Alcohol 22.22 142.86 158.86 13.99 89.93 103.9

Max THF 36.00 40.00 72.00 50.00 55.56 105.5 Max Thyonil Chloride 11.67 2.08 13.75 84.85 15.15 100.0

800.00

C-1 IPA 0.14 1.29 1.43 10.00 90.00 100.0 1.29 C-2 IPA 0.92 36.00 36.92 2.49 97.51 100.0 36.00

C-3 Ethyle acetate 1.67 9.44 11.11 15.00 85.00 100.0 9.44

MDC 1.25 10.00 11.25 11.11 88.89 100.0 C-4

IPA 2.50 112.50 115.00 2.17 97.83 100.0 122.50

MDC 3.33 41.67 45.00 7.41 92.59 100.0

C

C-5Acetone 3.33 66.67 70.00 4.76 95.24 100.0

108.33



Group Code

of Product


Total Spent

Solvent

Max of Methylene Dichloride 3.33 41.67 45.00 7.41 92.59 100.0 Max of Iso propyl Alcohol 2.50 112.50 115.00 2.17 97.83 100.0

Max of Acetone 3.33 66.67 70.00 4.76 95.24 100.0 Max of Ethyle Acetate 1.67 9.44 11.11 15.00 85.00 100.0

122.50

D-1 Toluene 0.67 9.33 10.00 6.67 93.33 100.0 9.33 D-2 Benzene 1.82 10.91 12.73 14.29 85.71 100.0 10.91

Chloroform 1.76 10.59 12.35 14.29 85.71 100.0 D-3

Heptane 1.76 28.24 30.00 5.88 94.12 100.0 38.82

Methanol 4.20 3.00 7.20 58.33 41.67 100.0 D-4

MDC 0.60 6.00 6.60 9.09 90.91 100.0 9.00

D-5 Toluene 0.45 1.73 2.19 20.70 79.30 100.0 1.73 D-6 Methanol 1.98 0.16 2.14 92.31 7.69 100.0 0.16

Xylene 1.00 8.00 9.00 11.11 88.89 100.0 D-8

Methanol 1.50 8.50 10.00 15.00 85.00 100.0 16.50

Xylene 0.86 12.00 12.86 6.67 93.33 100.0 D-9

Methanol 1.29 9.43 10.71 12.00 88.00 100.0 21.43

MIBK 11.11 77.78 88.89 12.50 87.50 100.0

D

D-10 Retarter Solvent 5.56 61.11 66.67 8.33 91.67 100.0

138.89

Max of Toluene 0.67 9.33 10.00 6.67 93.33 100.0

Max of Heptane 1.76 28.24 30.00 5.88 94.12 100.0 Max of MDC 0.60 6.00 6.60 9.09 90.91 100.0

Max of Methanol 4.20 9.43 10.71 39.20 88.00 127.2 Max of Xylene 1.00 12.00 12.86 7.78 93.33 101.1

Max of MIBK 11.11 77.78 88.89 12.50 87.50 100.0 Max of Retarter 5.56 61.11 66.67 8.33 91.67 100.0

Max of chloroform 1.76 10.59 12.35 14.29 85.71 100.0 Max of benzene 1.82 10.91 12.73 14.29 85.71 100.0

138.89

E-1 Toluene 1.05 14.74 15.79 6.67 93.33 100.0 14.74 E-2 Chloroform 1.11 7.78 8.89 12.50 87.50 100.0 7.78

Methanol 2.50 7.50 10.00 25.00 75.00 100.0 MEG 1.67 11.67 13.33 12.50 87.50 100.0 Toluene 1.67 18.33 20.00 8.33 91.67 100.0 Chloroform 3.33 21.67 25.00 13.33 86.67 100.0

E-3

IPA 2.00 8.00 10.00 20.00 80.00 100.0

67.17

E

E-6 Toluene 2.00 22.00 24.00 8.33 91.67 100.0 46.00



Group Code

of Product


Total Spent

Solvent

N-Hexane 2.00 14.00 16.00 12.50 87.50 100.0 THF 0.80 10.00 10.80 MDC 4.00 96.00 100.00 4.00 96.00 100.0 Ethyl Acetate 4.00 56.00 60.00 6.67 93.33 100.0 E-7

IPA 4.80 35.20 40.00 12.00 88.00 100.0

187.20

Max of Toluene 2.00 22.00 24.00 8.33 91.67 100.0

Max of Chloroform 3.33 21.67 25.00 13.33 86.67 100.0 Max of Methanol 2.50 7.50 10.00 25.00 75.00 100.0

Max of Mono Ethyl Glycol 1.67 11.67 13.33 12.50 87.50 100.0 Max of IPA 4.80 35.20 40.00 12.00 88.00 100.0

Max of N-Hexane 2.00 14.00 16.00 12.50 87.50 100.0 Max of MDC 4.00 96.00 100.00 4.00 96.00 100.0

Max of Ethyl Acetate 4.00 56.00 60.00 6.67 93.33 100.0 Max of THF 0.80 10.00 10.80 7.41 92.59 100.0

187.20

F F-1 MDC 1.14 5.14 6.29 18.18 81.82 100.0 5.14

Max of MDC 1.14 5.14 6.29 18.18 81.82 100.0 5.14

Toluene 0.34 9.66 10.00 3.45 96.55 100.0

G-1 IPA 0.14 1.72 1.86 7.41 92.59 100.0

11.38

MDC 2.00 7.81 9.81 20.38 79.62 100.0 GG-2 Cyclo

Hexane 0.25 2.25 2.50 10.00 90.00 100.0 10.06

Max of Toluene 0.34 9.66 10.00 3.45 96.55 100.0

Max of IPA 0.14 1.72 1.86 7.41 92.59 100.0 Max of MDC 2.00 7.81 9.81 20.38 79.62 100.0

Max of Cyclo Hexane 0.25 2.25 2.50 10.00 90.00 100.0

11.38

Methanol 10.43 41.74 52.17 20.00 80.00 100.0

H-1 Iso propyl Alcohol 2.61 25.22 27.83 9.38 90.63 100.0

80.00 H

H-2 Xylene 0.63 9.38 10.00 6.25 93.75 100.0 9.38

Max of Methanol 10.43 41.74 52.17 20.00 80.00 100.0 Max of IPA 2.61 25.22 27.83 9.38 90.63 100.0

Max of Xylene 0.63 9.38 10.00 6.25 93.75 100.0 80.00



Group Code

of Product


Total Spent

Solvent

Methanol 5.45 38.18 43.64 12.50 87.50 100.0 DMF 3.64 12.73 16.36 22.22 77.78 100.0 I-1 MDC 5.45 50.91 56.36 9.68 90.32 100.0

101.82

I-2 Cyclo Hexane 1.18 12.94 14.12 8.33 91.67 100.0 12.94

THF 6.09 29.57 35.65 17.07 82.93 100.0 Methanol 1.00 7.83 8.83 11.33 88.67 100.0 I-3 Toluene 0.87 3.48 4.35 20.00 80.00 100.0

40.87

Di phenyl ether 0.20 2.50 2.70 7.41 92.59 100.0

I

I-4 N-Hexane 0.50 2.50 3.00 16.67 83.33 100.0

5.00

Max of Methanol 5.45 38.18 43.64 12.50 87.50 100.0 Max of DMF 3.64 12.73 16.36 22.22 77.78 100.0

Max of MDC 5.45 50.91 56.36 9.68 90.32 100.0 Max of Cyclo Hexane 1.18 12.94 14.12 8.33 91.67 100.0

Max of Tetra Hydro Furan 6.09 29.57 35.65 17.07 82.93 100.0 Max of Toluene 0.87 3.48 4.35 20.00 80.00 100.0

Max of Di phenyl ether 0.20 2.50 2.70 7.41 92.59 100.0 Max of N-Hexane 0.50 2.50 3.00 16.67 83.33 100.0

101.82

Total Spent Solvent 1710.57

Table-2.7: Detailed summary of Total solvent requirement

Solvent Requirement, MT/Month Solvent Requirement, % Solvent

Fresh Recovered Total Fresh Recovered Total Methanol 54.94 246.85 297.08 18.49 83.09 101.59

Toluene 89.60 820.66 910.25 9.84 90.16 100.00 Chloroform 55.10 286.44 332.20 16.59 86.23 102.81 N-Hexane 24.92 237.11 262.03 9.51 90.49 100.00

IPA 38.94 353.86 384.45 10.13 92.04 102.17 MDC 48.98 376.77 426.89 11.47 88.26 99.73

Acetone 16.67 133.33 150.00 11.11 88.89 100.00 Ethyl Acetate 5.67 56.00 60.00 9.44 93.33 102.78

Heptane 1.76 28.24 30.00 5.88 94.12 100.00 Xylene 1.62 21.38 22.86 7.11 93.52 100.62

Cyclo Hexane 1.43 15.19 16.62 8.58 91.42 100.00 Benzene 1.82 12.73 16.36 11.11 77.78 88.89


Solvent Requirement, MT/Month Solvent Requirement, % Solvent

Fresh Recovered Total Fresh Recovered Total Tetra Hydro Furan 22.89 29.57 35.65 64.20 82.93 147.12

Thyonil chloride 11.67 2.08 13.75 84.85 15.15 100.00

MIBK 11.11 77.78 88.89 12.50 87.50 100.00 Di phenyl ether 0.20 2.50 2.70 7.41 92.59 100.00

Retarter 5.56 61.11 66.67 8.33 91.67 100.00

DMF 3.64 12.73 16.36 22.22 77.78 100.00 Mono Ethyle Glycol 1.67 11.67 13.33 12.50 87.50 100.00


Drawing-2.1: Schematic Diagram of the Solvent Recovery System

Specification of Distillation Column

Diameter & Height : 0.3 m dia & 3.0 m. ht

MOC : 316 L

Specification of Condenser

Nos. : 2

Cooling Media: : Cooling water/ Chilled Water

Heat Transfer Area : 4 & 2 Sq. m.

Residence Time : 1 hr

Vacuum : 752 mm of Hg

VACUUM =752 mm of Hg

RE-BOILER

C/W OUT

CONDENSER - 1

REFLUX

C/W IN

DIS

TILL

ATI

ON

CO

LUM

N

STEAM

Recovered Solvent

CONDENSER -2CHILLEDWATER IN

CHILLED WATER OUT


2.8 MATERIAL REQUIREMENTS, HANDLING, STORAGE AND TRANSPORTATION

2.8.1 RAW MATERIAL REQUIREMENT

Details of product wise raw material consumption for the proposed project are

given in Table - 2.8.

Table-2.8: Details of Product wise Raw Material Requirement

Quantity, MT/Month Name of Raw Material Code of

Product

Kg/Kg of

product Group

maximum Total

1,3 DiFluoro Benzene C-4 0.63 3.13 3.13 1,3 Dromo Chloro Propane H-2 0.84 1.69 1.69 2,5 DiChloro Nitro Benzene H-1 1.39 2.78 2.78 2,6 dimthyl aniline G-2 0.69 0.69 0.69 2-Amino Pyrdine E-3 0.69 1.39 1.39 2-Chloroacetic acid t-butyl ester D-6 0.55 1.65 1.65 2-Tert butoxy-2-oxo-ethyl (2-2,6 dichlorophenyl)amino)phenyl acetate D-5 1.51 4.54 4.54

B- 24 0.83 8.33 E-5 0.91 E-7 1.25

2.50 3-(2-Chloro Phenyl )ethyl 2-cyano pyridine

F-1 2.00 4.00

14.83

4-(4-chloro-1-oxo butyl)alfa alfa di methyl phenyl acetic acid D-4 1.00 3.00 3.00

4-(-4-Chloro 1-Oxobutyl)2,2,di methyl phenyl a. acid D-10 1.00 10.00 10.00

4-(p-chloro pheny)4-Hydroxy Piperidine B- 25 1.13 11.25 11.25 4-Amino 1,2,4 Traizole C-4 0.83 4.13 4.13 4-Chloro p-Fluoro phenol B- 25 1.25 12.50 12.50

B- 16 0.89 4-Chloro Piperidine

B- 17 1.50 15.00 15.00

4-Methyl Pyridine E-6 1.11 2.22 2.22 4-Phenyl 4-Hydroxy piperidine B- 20 2.50 25.00 25.00 Activated Carbon F-1 0.10 0.20 0.20

A-9 1.17 11.667 E-3 1.39 E-4 1.13

2.78 Acetic acid

I-1 1.55 3.09

17.54

Acetic Anhydride A-9 1.00 10.000 10.00

A-12 0.14 A-8 4.29

42.86

B- 12 1.33 Acetone

B- 14 3.43 34.29

80.48



Product

Kg/Kgof

productGroup

maximum Total

B- 16 2.50 B- 17 0.75 AcetoneB- 25 1.25 B- 3 0.33

AcetoneC-5 0.67 3.33

Acetonitrile E-4 0.83 1.67 1.67 B- 17 0.06 B- 18 0.17 B- 19 0.07

1.71

C-1 0.01 0.03 H-1 0.17

Activated Carbon

H-2 0.03 0.35

2.09

D-1 1.11 Alfa Alfa Di methyl phenyl acetic acid

D-3 2.35 7.06 7.06

C-4 0.78 3.90 Aluminium chloride

F-1 1.60 3.20 7.10

AminoGuanidine bi carbonate C-2 1.54 7.69 7.69 C-3 0.44 C-4 2.50

12.50

B- 10 0.22 B- 11 0.67 B- 14 0.29 B- 22 0.22 B- 6 1.67

Ammonia Gas

B- 7 0.28

16.67 29.17

E-4 3.75 Ammonia Solution

E-7 9.00 18.00 18.00

Anhydrous Piperazine G-1 2.18 2.18 2.18 Aniline I-1 0.91 1.82 1.82 Azacyclonol D-10 0.89 8.89 8.89 Benzene B- 23 3.00 30.00 30.00 Benzillic acid B- 23 1.74 17.39 17.39 Benzoyl chloride B- 9 2.20 22.00 22.00 Benzyl Amine A-2 0.83 8.33 8.33 Benzyl Cyanide D-2 0.61 1.82 1.82 Beta- Phenyl Ethyl Amine A-7 0.44 4.44 4.44 Boric acid E-7 2.00 4.00 4.00

Bromine I-1 4.73 9.45 9.45



Product

Kg/Kg of

product Group

maximum Total

B- 19 0.56 5.56 Bromo Benzene

I-3 4.35 8.70 14.25

Caustic Flakes I-2 1.18 2.35 2.35 A-10 2.36 A-11 2.27 A-13 2.27 A-16 1.39 A-2 1.33 A-4 2.67 A-5 2.00 A-6 0.67 A-7 0.89 A-8 4.29

42.86

B- 12 2.67 B- 17 1.50 B- 18 2.14 B- 19 2.78 B- 2 1.20 B- 21 1.06 B- 3 2.67 B- 9 1.50

27.78

D-3 1.76 D-7 0.15

5.29

E-4 2.08 E-5 1.36

4.17

F-1 5.00 10.00 H-1 5.22

Caustic Lye

H-2 1.56 10.43

100.53

A-14 1.58 15.83 B- 17 2.00 B- 18 1.71 B- 19 1.67

20.00 Caustic Potash

D-2 15.76 47.27

83.11

C-5 1.00 5.00 Caustic Soda Lye D-4 1.20 3.60

8.60

B- 25 0.13 1.25 Charcoal

C-2 0.31 1.54 2.79

C-4 0.53 2.63 Chloro Acetyl chloride D-7 0.42 1.26

4.66



Product

Kg/Kgof

productGroup

maximum Total

G-2 0.77 0.77 Chloro Benzene B- 19 1.67 16.67 16.67

B- 12 1.33 B- 15 3.33 B- 3 1.25 B- 9 2.50

33.33

A-1 0.67 A-10 0.91 A-11 0.91 A-13 0.91 A-14 1.67 A-16 1.11 A-2 0.33 A-3 1.36 A-4 0.37 A-5 0.30 A-6 0.27 A-7 0.67 A-8 1.43

16.67

E-3 0.56 E-4 1.67

3.33

Chloroform

D-3 0.59 1.76

55.10

I-2 2.35 I-1 0.91 I-2 2.82 I-3 5.22

10.43 Conc –Hydrochloric acid

D-7 0.03 0.09

10.53

CTC D-3 0.59 1.76 1.76 Cupric chloride I-1 0.27 0.55 0.55

G-1 0.25 0.25 Cyclo Hexane

I-2 0.59 1.18 1.43

DFTA C-5 1.00 5.00 5.00 A-10 1.09 A-16 0.67

10.91 Di BOC

B- 12 1.07 10.67 21.58

Di Methyl Carbonyl chloride E-4 1.08 2.17 2.17 Di Methyl Sulfate D-2 0.91 2.73 2.73 Di methyl Sulfoxide D-2 3.03 9.09 9.09 Di phenyl ether I-4 0.10 0.20 0.20



Product

Kg/Kg of

product Group

maximum Total

Diclofenec sodium D-6 0.82 2.47 2.47 Dioxane I-3 2.17 4.35 4.35 DM water G-2 15.17 15.17 15.17

B- 2 0.03 0.25 DMF

I-1 1.82 3.64 3.89

DMSO I-3 0.87 1.74 1.74 C-3 0.33 1.67

Ethyl acetateF-1 2.00 4.00

5.67

B- 5 0.92 B- 6 3.67

36.67 Ethyl chloro formate

A-15 1.20 12.00 48.67

B- 24 0.02 0.20 Ethylene Bromide

E-7 0.03 0.06 0.26

C-1 1.50 C-2 0.52 C-3 1.11

7.50 Formic acid

D-5 2.27 6.82

14.32

Heptane D-3 0.59 1.76 1.76 E-4 0.50 1.00 C-1 1.71 C-3 0.56

8.57 Hydrazien Hydrate

H-1 0.87 1.74

11.31

A-10 3.64 A-13 2.73 A-2 0.89 A-4 3.00 A-5 2.50 A-6 3.33 A-7 1.00 A-8 7.86

78.57

B- 17 2.47 B- 18 2.14 B- 19 1.67 B- 24 3.00 B- 6 16.67

166.67

C-4 3.00 15.00 D-1 3.33

D-10 4.44

Hydrochloric Acid

D-2 3.64

44.44

78.57



Product

Kg/Kgof

productGroup

maximum Total

D-4 1.20 D-8 0.33 D-9 0.29 E-7 4.50 9.00 H-1 6.96

Hydrochloric Acid

H-2 1.56 13.91

B- 16 0.27 Hydrochloric Acid Gas

B- 17 1.50 15.00 15.00

B- 1 0.06 B- 10 0.06 B- 11 0.16 B- 13 0.08 B- 14 0.06 B- 22 0.07 B- 3 0.20 B- 4 0.07 B- 7 0.07

Hydrogen Gas

B- 8 0.05

2.00 2.00

E-4 1.30 2.60 I-2 0.94 Hydrogen Peroxide I-3 0.87

1.88 4.48

B- 17 0.03 B- 18 0.11 B- 19 0.04 B- 20 0.25

2.50

C-1 0.00 0.01

Hyflo

H-1 0.13 0.26

2.78

Industrial solvent D-4 1.40 4.20 4.20 B- 17 0.001 B- 18 0.003 B- 24 0.001

0.03 Iodine

I-3 0.22 0.43

0.46

Iron Powder D-3 0.01 0.02 0.02 Iso Butyl amine A-6 1.00 10.00 10.00

B- 17 0.80 B- 18 1.60 B- 19 2.22 B- 9 1.00

22.22

Iso Propyl Alcohol

C-1 0.03 2.50

47.80



Product

Kg/Kg of

product Group

maximum Total

C-2 0.18 C-4 0.50 G-1 7.00 G-2 0.14

7.00

H-1 1.30 2.61 A-13 0.45 A-14 0.67

6.67

E-4 1.00 2.00

Iso Propyl Alcohol

F-1 2.40 4.80 Iso Propyl amine A-5 1.00 10.00 10.00

D-3 3.53 10.59 Liq Bromine

E-3 1.11 2.22 12.81

Liq. ammonia E-6 3.11 6.22 6.22 B- 24 0.20 2.00

Magnesium Turning E-7 0.30 0.60

2.60

Meta chloro Benzyl cyanide E-4 1.25 2.50 2.50 A-11 1.09 A-13 1.09 A-14 1.50

15.00 Methane sulfonic acid

C-5 0.40 2.00

17.00

B- 10 0.28 B- 11 0.67 B- 12 1.33 B- 13 0.28 B- 14 7.14 B- 15 0.67 B- 17 2.00 B- 18 2.86 B- 19 2.67 B- 22 2.78 B- 23 4.35 B- 25 2.50 B- 7 0.22 B- 8 1.00 B- 9 1.00

71.43

D-1 3.33 D-4 1.40

D-10 3.56

Methanol

D-6 0.66

35.56

179.92



Product

Kg/Kgof

productGroup

maximum Total

D-8 0.50 D-9 0.43 H-1 5.22 10.43 A-1 0.02 A-11 3.18 A-13 5.45 A-16 0.56 A-2 0.22 A-4 0.20 A-5 0.25 A-6 0.20 A-7 0.09 A-8 0.21

54.545

E-4 1.25 2.50 I-1 2.73

Methanol

I-3 0.50 5.45

Methanolic KOH (3N) I-4 0.09 0.19 0.19 Methyl aceto acetate H-2 0.97 1.94 1.94

A-1 2.40 A-2 1.83 A-3 2.27 A-4 2.00 A-5 3.00 A-6 2.67 A-7 2.40

Methyl acrylate

A-8 5.71

57.14 57.14

Methyl Amine A-1 0.44 4.444 4.44 Methyl methacrylate A-8 2.86 28.571 28.57 Methyl Nicotinate E-4 1.29 2.58 2.58

C-4 0.25 C-5 0.67

3.33

D-4 0.20 0.60 B- 2 0.08 B- 22 0.56 B- 6 3.33

33.33

E-7 2.00 4.00 F-1 2.00 4.00 G-1 2.00

Methylene Di Chloride

G-2 2.00 2.00

52.72



Product

Kg/Kg of

product Group

maximum Total

I-1 2.73 5.45

I-3 0.70 1.39 B- 18 0.29 Mg Turnigs B- 19 0.33

3.33 4.72

MIBK D-10 1.11 11.11 11.11 A-3 0.91

MMA Solution A-8 2.86

28.57 28.57

Mono ethyl amine solution A-3 0.91 9.09 9.09 Mono Ethyl Glycol E-4 0.83 1.67

A-14 3.33 33.33 35.00

N-(2,6 Di methyl phenyl) 2-Chloro acetamide G-1 1.25 1.25 1.25

N,N Di Methyl Aniline D-7 0.49 1.47 1.47 B- 7 1.11

N-Benzyl-4-Piperidone B- 8 1.25

12.50 12.50

B- 13 1.11 N-BOC-4-Piperidone

B- 14 1.43 14.29 14.29

B-17 N-Carbethoxy 4-Piperidone

B- 15 0.83 8.33 8.33 B- 12 1.33 B- 9 2.00

20.00 N-Carbethoxy-4-Amino Piperidine

H-1 1.39 2.78 22.78

A-10 1.82 A-11 1.82 A-13 1.82 A-14 1.67 A-16 1.11

18.18

B- 10 1.11 B- 18 1.43 B- 19 1.67 B- 22 1.11 B- 3 3.33

N-Carbethoxy-4-Piperidone

B- 4 1.18

33.33

51.52

A-10 0.91 A-11 0.91 A-13 0.91 A-16 0.56

N-Hexane

A-9 0.33

9.09

24.92



Product

Kg/Kgof

productGroup

maximum Total

B- 12 1.33 B- 2 0.08

13.33

E-7 1.00 2.00 N-Hexane I-4 0.25 0.50 Nitric acid E-6 1.67 3.33 3.33 Nitro methane I-4 17.72 35.44 35.44

B- 24 0.83 B- 5 0.83 B- 6 3.33 B- 23 0.70 B- 2 1.20

33.33 N-Methyl-4-Chloro Piperidine

E-7 1.25 2.50

35.83

N-Methyl-4-Hydroxy Piperidine B-2 1.20 12.00 12.00 A-15 1.00 10.00 B- 1 1.11 N-Methyl-4-Piperidone B- 11 1.33

13.33 23.33

n-Propyl amine A-4 0.67 6.667 6.67 Oleum E-7 9.00 18.00 18.00 Ortho Phenylene Di Amine H-2 1.13 2.25 2.25 Para Bromo chloro benzene B- 17 0.62 6.17 6.17 Para Di Bromo Benzene B- 18 2.29 22.86 22.86 Para formaldehyde I-4 0.78 1.56 1.56 Para Toluene sulfonic acid A-14 1.83 18.33 18.33

B- 15 0.17 Pd/C (5%)

B- 20 0.25 2.50 2.50

D-8 1.67 Phenyl acetic acid

D-9 1.43 5.00 5.00

D-8 0.58 Phosphoric acid

D-9 0.57 1.75 1.75

D-8 0.70 Phosphorus pentoxide

D-9 0.71 2.14 2.14

Piperidine B- 15 0.83 8.33 8.33 Piperidone Base A-9 0.83 8.333 8.33 Piperidone Monohydrate Hydrochloric Acid A-12 0.23 2.27 2.27

Potassium Bi Carbonate D-10 0.67 6.67 6.67 Potassium carbonate B- 25 0.63 6.25 6.25 Potassium Hydroxide B- 15 0.33 3.33 3.33

D-10 0.01 0.06 Potassium Iodide

H-1 0.01 0.02 0.07



Product

Kg/Kg of

product Group

maximum Total

Potassium permanganate D-4 2.00 6.00 6.00 D-8 1.67

Pthalic anhydride D-9 1.43

5.00 5.00

Pyridine E-2 1.05 2.11 2.11 D-8 0.23 0.69 B- 1 0.01 B- 10 0.02 B- 11 0.07 B- 13 0.08 B- 14 0.06 B- 22 0.03 B- 3 0.03 B- 4 0.01 B- 7 0.03 B- 8 0.03

0.83 Raney Nickel

H-1 0.07 0.14

1.66

Retarter Solvent D-10 0.56 5.56 5.56 Selanium I-3 1.52 3.04 3.04

A-10 2.27 22.73 Soda ash

G-2 0.59 0.59 23.32

Sodamide E-2 0.32 0.63 0.63 D-8 0.05

Sodium acetate D-9 0.04

0.15 0.15

Sodium Bicarbonate D-4 0.10 0.30 0.30 B- 9 1.25 12.50 D-1 0.28

D-10 0.08 0.83

E-3 0.14 0.28 Sodium Carbonate

H-1 1.09 2.17

15.79

Sodium Cyanide E-4 0.54 1.08 1.08 D-8 0.33 1.00

Sodium Hydroxide D-9 0.29

1.00

A-1 0.83 A-2 0.67 A-3 0.91 A-4 0.67 A-5 1.00 A-6 0.75

Sodium Methoxide

A-7 0.83

10.00

22.73



Product

Kg/Kgof

productGroup

maximum Total

B- 23 0.70 6.96 E-4 0.25 0.50

I-1 2.64 5.27

C-4 0.90 4.50 Sodium Nitrite

I-1 1.27 2.55 7.05

B- 15 0.17 B- 20 0.25

2.50

D-7 0.06 0.18 Sodium Sulphate

G-1 0.13 0.13

2.81

D-3 1.18 3.53 E-4 7.50 E-5 2.05

15.00 Sulfuric acid

F-1 2.50 5.00

23.53

Sulphanilamide I-2 1.18 2.35 2.35 B- 20 0.25 2.50 E-6 2.22 4.44 I-1 1.27 I-2 1.18

Sulphuric acid

I-4 0.03 2.55

9.49

TBAB D-6 0.01 0.04 0.04 Tert-Butyl alcohol D-7 0.30 0.90 0.90 Tetra Butyl ammonium bromide H-2 0.02 0.04 0.04

B- 17 1.80 B- 18 1.60 B- 19 6.00 B- 24 3.60 B- 24 3.60

60.00

I-3 3.04 6.09

Tetra Hydro Furan

E-7 5.00 10.00

76.09

F-1 3.00 6.00 Thionyl chloride

B- 2 1.17 11.67 17.67

B- 1 0.08 B- 16 0.63 B- 17 1.00 B- 18 5.71 B- 19 3.33 B- 20 5.00 B- 23 4.87

Toluene

B- 24 4.00

90.00 126.33



Product

Kg/Kg of

product Group

maximum Total

B- 3 0.50 B- 4 0.15 B- 5 0.83 B- 6 3.33 B- 9 9.00 D-1 0.22 D-2 1.52 D-4 0.20 D-5 0.15

4.55

A-12 0.14 A-14 1.17 A-15 0.20 A-2 0.33 A-8 2.86

28.57

E-2 0.53 E-4 0.83 E-7 1.00

2.00

G-2 0.34 0.34

Toluene

I-3 0.43 0.87 A-11 1.36

Tri methyl ortho formate A-13 1.36

13.64

Tri Methyl Silyl Iodide C-5 1.67 8.33 8.33 Urea H-1 1.04 2.09 2.09

H-2 0.31 0.63 D-8 0.33 Xylene D-9 0.29

1.00 1.62

, Di methyl4-(1-oxobutyl)phenyl ethyl acetate D-4 1.00 3.00 3.00


2.8.2. HANDLING

All the raw materials, by products and finished products are handled as per the

standard practice and same practice will be continued after proposed

expansion. Also, all the pipes and equipment will be kept cleaned to avoid any

blockage and deposits. Pressure tests of the reactors will be carried out before

every start–up of the process to find out any leakage. All the process and

storage equipment used for the handling of chemicals will be maintained

properly to avoid any leakage or spillage of the chemical. All protective and

safety precautions will be taken while cleaning up spills. Also all storage tanks,

transfer lines, valves, fittings and every joint are inspected by third party

periodically. For handling of liquid chemicals pumping system will be used

which is very safe and simple to operate. Drum trolley will be used for safe

handling and transfer of hazardous chemicals as well as hazardous waste from

one place to another place in the plant area.

2.8.3. STORAGE

Industry has already provided adequate storage area of 48 m2 and proper

storage facilities for all the finished products which will be adequate for the

proposed expansion. Separate storage area of 1463 m2 has provided to store

different types of hazardous raw materials and it will be expanded upto 1795 m2

after proposed expansion. Hazardous solid waste is stored at a distance place

from the other plant activities with storage area of 47.50 m2 which will be

continued after proposed expansion. The unit has also provided separate

storage area of 41 m2 for fuels used in the plant. The storage yard of chemicals is

isolated from other plant activities and it has equipped with necessary safety

provisions and suitable control measures. The storage area is properly

ventilated. Fire extinguishers and safety showers will be provided in tank farms.

Spark proof equipment will be used during handling and storage. The details of

storage capacity, source and mode of transportation of Raw Material, Product

and By-Products are given in Table- 2.9.


2.8.4. TRANSPORTATION

The vehicles for transportation of raw material, products and by-product will be

parked at specified loading facilities where fire extinguishers along with the

safety gazettes will be provided. Spark arresters will be fitted on all the tankers

entering inside factory. All the raw materials required for proposed expansion

and all the products will be transported through tanks or trucks by roadway. All

the necessary precautions will be taken while carrying out transport of the

above materials as per the Hazardous Rules of transportation, Central Motor

Vehicle Act-1988 & 1989.

Table-2.9 Details of Products, By-Products and Raw Material Storage, Source and mode of Transportation

Sr. No. Name of chemical

Type of Packing/ Storage

Physical Form

Packing Size Kg /

Nos. & Size of Storage

Tanks

Maximum Storage

Capacity, MT

Market/Source

Products

1 Derivatives of Piperidones Solid 25 kg Export/

Local

2 Derivatives of Piperidines Solid 25 kg

10Export/ Local

3 Derivatives of Triazoles Solid 25 kg 5 Export/ Local

4 Fexofinadine Intermediates Solid 25 kg 3 Export/

Local

5 Loratadine intermediates & others Solid 25 kg 2 Export/

Local

6 Haloperidol Intermediate Solid 25 kg 2 Export/

Local

7 Ranozaline Intermediates Solid 25 kg 1 Export/

Local

8 Domperidone Intermediates Solid 25 kg 2 Export/

Local

9Other bulk drug intermediate & chemicals

Fiber/ HDPEDrum

Solid 25 kg 2 Export/ Local




Physical Form

Packing Size Kg /


Tanks

Maximum Storage

Capacity, MT

Market/ Source

By Products

1 Hydrochloric Acid (30 %) Liquid 200 Lit Local

2 Hydrobromic Acid (30 %) Liquid 200 Lit Local

3 Sodium Hypo Sulphite Liquid 200 Lit Local4 Liq. Ammonia Liquid 200 Lit Local5 Sodium Bromide Liquid 200 Lit Local

6

Dimer of N-(2,6 Di methyl phenyl )-2-(Piperazinyl) acetamide

HDPE Drum

Liquid 200 Lit

25

Local

Raw Materials

1 Methyl acrylate MSDrum Liquid 180 Lit 36.0 Import/

India

2 Sodium Methoxide MSDrum Powder 100 kg 15.0 Import/

India 3 Caustic Soda Lye Tank Liquid 15000 Lit 15.0 GIDC

4 Chloroform MSDrum Liquid 300 Lit 30.0 Import/

India 5 Methanol Tank Liquid 12000 Lit 15.0 GIDC 6 Toluene Tank Liquid 12000 Lit 15.0 GIDC

7 Mono Methyl anine solution Tank Liquid 10000 Lit 15.0 Out of

Gujarat

8 Mono Methyl amine Gas Cylinder Gas 400 kg 1.2 Out of

Gujarat

9 Raney Nickel HDPE Carboy Solid 10 kg 0.2 Out of

Gujarat 10 Hydrogen Gas Cylinder Gas 1kg 6 11 Nitrogen Gas Cylinder Gas 2 kg 6 12 Ammonia Gas Cylinder Gas 50 kg 1.5 13 Hydrochloric Acid Tanker Liquid 10000 Lit 20.0 14 Benzaldehyde MS Drum Liquid 210 Lit 15.0 15 Thionyl chloride GI Drums Liquid 300 Lit 9.0

Within Gujarat

16 Di Methyl Formamide MS Drum Liquid 200 Lit 1.0 Out of Gujarat

17 N-Hexane MS Drum Liquid 200 Ltr 5.0 Out of Gujarat

18 Ethyl chloro fomate MSPE Drum Liquid 200 Lit 5.0 Out of

Gujarat

19 Mg Turning Bags Solid 30 kg 0.5 Out of Gujarat

20 Tetra Hydro Furan MS Drum Liquid 180 Lit 5.4 Out of Gujarat




Physical Form

Packing Size Kg /


Tanks

Maximum Storage

Capacity, MT

Market/Source

21 Para Bromo chloro Benzene Bags Solid 50 kg 1.0 Out of

Gujarat

22 Para Di Chloro Benzene

HDPECarboy Solid 50 kg 2.0 Out of

Gujarat 23 Iodine Bags Solid 5 kg 0.01 GIDC 24 Caustic Potash Bags Solid 50 kg 5.0 GIDC

25 Activated Carbon Bags Solid 20 kg 1.0 Out of Gujarat

26 Hyflo Bags Solid 16.8 kg 0.5 Out of Gujarat

27 Hydrazine Hydrate HDPECarboy Liquid 200 Lit 25.0 Import/

India

28 Formic acid HDPECarboy Liquid 35 Lit 15.0 GIDC

29 Benzyl Cyanide MS Drum Liquid 200 Lit 5.0 Out of Gujarat

30 Denatured spirit MS Drum Liquid 250 Lit 15.0 Out of Gujarat

31 Di Methyl Sulfoxide HDPECarboy Liquid 210 Lit 12.0 Out of

Gujarat

32 Mono ethylene glycol MS Drum Liquid 200 Lit 8.0 Out of Gujarat

33 Mono Glyme MS Drum Liquid 200 Lit 8.0 GIDC 34 Aluminium chloride Bags Solid 50 kg 5.0 GIDC

35 Acetic Anhydride HDPECarboy Liquid 35 Lit 5.0 GIDC

36 4 Chloro Butyryl chloride

HDPECarboy Liquid 50 Lit 2.0 GIDC

37 Mix solvent MS Drum Liquid 200 Ltr 5.0 GIDC

38 Potassium Permanganate Bags Powder 50 kg 5.0 Out of

Gujarat 39 Sodium Bi Sulfite Bags Powder 50 kg 1.0 GIDC

40 Methylene Di chloride HDPEDrums Liquid 250 Lit 12.0 GIDC

41 Carbon tetra chloride HDPEDrums Liquid 300 Lit 2.0 GIDC

42 Heptane MS Drum Liquid 200 Ltr 5.0 GIDC

43 Cyclo Hexane MS Drum Liquid 200 Ltr 5.0 Out of Gujarat

44 Methyl Iso Butyl Ketone MS Drum Liquid 160 lit 5.0 Out of Gujarat

45 Azacyclonol Fibre Drum Solid 50 kg 5.0 Out of

Gujarat

46 Potassium Iodide Bags Solid 10 kg 0.2 Out of Gujarat

47 Sodium Bi Carbonate Bags Solid 50 kg 5.0 GIDC




Physical Form

Packing Size Kg /


Tanks

Maximum Storage

Capacity, MT

Market/ Source

48 Potasium Bi Carbonate Bags Solid 50 kg 5.0 GIDC 49 Sodium Carbonate Bags Solid 50 kg 5.0 GIDC

50 2,5 Di Chloro Nitro Benzene Bags Solid 50 kg 3.0 Out of

Gujarat

51 Meta chloro Benzyl cyanide

MSPE Drum Liquid 100 lit 2.0 Out of

Gujarat

52 Methyl Nicotinate Bag Solid 50 kg 2.0 Out of Gujarat

53 Sulfuric acid Bottle Liquid 60 lit 6.0 GIDC 54 Liq Ammonia Bottle Liquid 50 lit 6.0 GIDC 55 Hydrogen Peroxide Bottle Liquid 50 lit 5.0 GIDC 56 Acetic acid Bottle Liquid 35 lit 5.0 GIDC 57 Sodium Cyanide MS Drum Liquid 50 lit 2.0 GIDC 58 Boric acid Bags Solid 50 kg 1.0 GIDC 59 Oleum Tank Liquid 12000 lit 12.0 GIDC

60 1,3,Di Fluoro Benzene MS Drum Liquid 200 lit 0.5 Out of Gujarat

61 Chloro acetyl chloride MSPE Drum Liquid 200 lit 1.0 Out of

Gujarat

62 Tri Methyl chloro silane MSPE Drum Liquid 170 lit 1.0 Out of

Gujarat

63 Tri Methyl Sulfoxonium Iodide

HDPE Carboy Powder 25 lit 2.0 GIDC

64 Sodium Nitrite Bags Solid 50 kg 2.0 GIDC 65 Acetone Tank Liquid 12000 lit 12.0 GIDC 66 Iso Propyl Alcohol Tank Liquid 12000 lit 12.0 GIDC

67 Para Di Bromo Benzene Bags Solid 50 kg 0.5 Out of

Gujarat

68 Ortho Phenylene Di Amine Bags Solid 50 kg 2.0 Out of

Gujarat

69 Methyl aceto acetate HDPE Carboy Liquid 35 lit 2.0 Out of

Gujarat

70 Tetra Butyl ammonium Bromide

HDPE Carboy Powder 10 kg 0.5 Out of

Gujarat

71 Xylene MS Drum Liquid 200 Ltr 5.0 Out of Gujarat

72 Fluoro benzene MS Drum Liquid 200 lit 2.0 Out of Gujarat

73 Pyridine MS Drum Liquid 200 lit 2.0 Out of Gujarat

74 Nitric acid HDPE Carboy Liquid 50 lit 5.0 GIDC

75 Liquid Bromine Bottles Liquid 3 lit 5.0 GIDC

76 Iron Powder Pakcet Powder 1 kg 0.05 GIDC




Physical Form

Packing Size Kg /


Tanks

Maximum Storage

Capacity, MT

Market/Source

77 Hydro bromic acid HDPEDrums Liquid 200 lit 5.0 GIDC

78 Chloro Benzene MS Drum Liquid 250 lit 2.0 Out of Gujarat

79 Bromo Benzene MS Drum Liquid 50 lit 2.0 Out of Gujarat

80 Para Toluene Sulfonic acid Bags Solid 50 kg 1.0 GIDC

81 Acetonitrile MS Drum Liquid 160 lit 2.0 GIDC

82 ammonium chloride Bags Solid 50 kg 0.5 Out of Gujarat

83 Ethylene Di Chloro Tetra acetic acid

HDPECarboy Solid 10 kg 0.1 Out of

Gujarat 84 Urea Bags Solid 50 kg 1.0 GIDC

85 Mono ethyl amine Tank Liquid 170 lit 2.00 Out of Gujarat

86 Di Boc MSPE Lined Drum

Liquid 50 lit 1.0 Import

87 Benzoyl chloride MS Drum Liquid 200 lit 1.0 Out of Gujarat

88 Common salt Bags Powder 50 kg 3.0 GIDC 89 Methane sulfonic acid Bags Solid 50 kg 1.0 GIDC

90 Tri methyl ortho formate MS Drum Liquid 200 lit 1.0 Out of

Gujarat 91 Benzyl amine MS Drum Liquid 200 lit 5.0 Import

92 Nitro Methane HDPEDrum Liquid 50 lit 0.5 Out of

Gujarat

93 Diclofenac sodium O/T

MSPE Drum

Powder 50 kg 2.0 Out of Gujarat

94 Ethyl acetate MS Drum Liquid 160 lit 2.0. Out of Gujarat

2.9 INFRASTRUCTURAL FACILITIES

2.9.1 LAND

The unit is located at survey no. 47, Hadmtala Industrial Area, Rajkot Gondal

Highway, Taluka Kotda Sangani, Dist. Rajkot, Gujarat. At present the unit is

having land admeasuring 21,138 m2, which is adequate to accommodate the

proposed expansion. Thus, there will not be any need of additional land. Out of

total land available, the unit has developed green belt area of 1,935.07 m2


which will be increased up to @ 4,483 m2 area for the betterment of the

environment. The detail break up of area is shown in Table-2.10. Moreover, key

plan and plan Layout is shown in Drawing – 2.2 & 2.3 respectively.

Table- 2.10: Break-up of Area

Area (Sqmt) Sr. No. Particular

Existing Proposed Total % of Total

Land

1 Process Plant 1,780 1,470 3,250 15.37

2 Product Storage 48 0 1463 6.92

3 Utility 257 143 400 1.89

4 Storage of Hazardous Chemicals 1,463 332 1,795 1.79

5 Storage of Fuel 41 0 41 0.19

6 Hazardous Waste Storage area 48 0 48 0.22

7 Effluent Treatment Plant 332 204 535 2.53

8 Green Belt 1,935 2,548 4,483 21.21 9 Roads 6,408 1,530 7,938 37.55 10 Parking Area 86 0 86 0.41

11 Administrative Area 341 0 341 1.61

12 Rain Water Harvesting Area 0 245 245 1.16

13 Undeveloped 8,401 -6471 1,930 9.13

Total 21,138 0.0 21,138 100.00

2.9.2 Details of Equipments/Vessels/Reactor and Utilities

As the proposed expansion will be carried out in the existing premises, existing

infrastructure facilities will be utilized with the addition of some new machinery

after proposed expansion. The lists of existing plant machineries as well as after

proposed expansion are given in Table-2.11.


Table-2.11: Details of plant machinery for the existing and after Proposed Expansion

Sr.No.

Reactors/Vessel/Equipments MoC Process/

Activity Qty. Size/ Capacity

Existing1 Reaction Vessel MS Reaction 2 5.0 KL 2 Reaction Vessel SS 316 Reaction 3 5.0 KL 3 Reaction Vessel SS 316 Reaction 2 4.0 KL 4 Reaction Vessel SS 316 Reaction 2 3.0 KL 5 Reaction Vessel SS 316 Reaction 4 2.0 KL 6 Reaction Vessel SS 316 Reaction 1 1.0 KL 7 Reaction Vessel SS 316 Reaction 4 0.75 KL 8 Reaction Vessel SS 316 Reaction 4 0.50 KL 9 Reaction Vessel SS 304 Reaction 1 2.0 KL

10 Reaction Vessel SS 304 Reaction 1 3.0 KL 11 Reaction Vessel Glass Lined Reaction 1 6.3 KL 12 Reaction Vessel Glass Lined Reaction 1 5.0 KL 13 Reaction Vessel Glass Lined Reaction 3 3.0 KL 14 Reaction Vessel Glass Lined Reaction 2 1.0 KL 15 Crystallizer SS 304 Crystallization 1 2.0 KL 16 PP/FRP Vessel PP/FRP Quenching 1 3.0 KL 17 Centrifuge SS 316 Filtration 4 36” 18 Tray Dryer SS 304 Drying 2 48 Trays 19 Sparkler Filter SS 316 Filtration 1 18” 20 Catalyst Filter SS 316 Filtration 1 14”

21 HVD Unit SS 316 High Vac Distn 2 0.30 KL

22 Vacuum Tray Dryer SS 304 Drying 1 22 Trays

23 Vacuum Tray Dryer SS 316 Drying 1 20 Trays

24 SS Pumps SS 316 RM Handling 6 12.00 KL/Hour

Proposed

1 Solvent Recovery Plant SS 316 Solv.

recovery 1 0.5 KL/Hour

2 Reaction Vessel SS 316 Reaction 3 2.0 KL 3 Reaction Vessel SS 316 Reaction 3 3.0 KL 4 Reaction Vessel SS 316 Reaction 4 5.0 KL 5 Sparkler Filter SS 316 Filtration 2 24” 6 Fluid Bed Dryer SS 316 Drying 2 125 KG 7 Cooling Tower FRP Cooling 3 200 TR 8 Neutsch Filter SS 316 Filtration 6 0.50 KL 9 Press Filter SS 316 Filtration 4 0.10 KL


Sr.No.

Reactors/Vessel/Equipments MoC Process/

Activity Qty. Size/ Capacity

10 Reactor SS 316 Reaction 2 6.5 KL 11 Reactor SS 316 Reaction 2 5.0 KL 12 Reactor SS 316 Reaction 1 4.0 KL 13 Reactor SS 316 Reaction 1 3.0 KL 14 Reactor SS 316 Reaction 5 2.0 KL 15 Reactor Glass Lined Reaction 3 3.0 KL 16 Reactor MSGL Reaction 1 3.0 KL 17 Reactor MSGL Reaction 1 1.0 KL 18 Centrifuge SS 316 Filtration 3 200.0 KG 19 Reactor MSGL Reaction 1 6.3 KL

Details of Utility

21 Steam Boiler MS/ CI/CS SteamGeneration 1 3000 Kg per

hour

22 Water jet Vacuum Pumps SS 316 Vacuum

Generation 12 3000 LPM

23 Water jet Vacuum Pumps PP/Teflon Vacuum

Generation 6 2000 LPM

24 Cooling Tower FRP Cooling water 2 250 TR

25 Refrigeration Plant MS/ CI/CS/ Copper

Brine for process 1 -30 Deg C

10 TR

26 Refrigeration Plant MS/CI/CS/Copper Brine for process 1 -10 Deg C

20 TR

27 Solvent Recovery Plant SS 316 Solvent

Recovery 1 5 KL


Drawing-2.2: Key Plan

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P

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2.10 RESOURCE CONSUMPTION

2.10.1 WATER

Presently the entire water requirement of M/s. Sam Fine Chem Ltd. is met

through own bore well and same source will be utilized after proposed

expansion.

The total fresh water requirement for existing unit is 23.4 KL/day for domestic,

gardening and Industrial purpose. After proposed expansion, it will be increased

up to 61.4 KL/day. Thus, the additional water requirement for proposed

expansion will be 38.0 KL/day. Domestic water requirement will be increase

from 2.0 KL/day to 6.5 KL/day after proposed expansion.

As per Guidelines issued by Central Ground Water Authority, Ministry of Water

Resources, New Delhi vide Letter No. 21-4/Guidelines/CGWA/2009-832, Dated

14/10/2009, the unit falls under Semi critical zone and Ground water

development in the region is 70-100 %.

The total water requirement of the plant is 61.4 KL/day, which does not exceed

the limit of 100 KL/day as per CGWA guidelines. Thus, it is not mandatory for the

unit to obtain permission from CGWA for the abstraction of ground water.

2.10.2. FUEL REQUIREMENT

Presently, the unit has installed one steam boiler (1.0 TPH) and thermic fluid

heater (6.0 Lac Kcal/hr). Earlier, Furnace Oil was used as fuel; now, the unit has

switched over to agricultural waste.

During proposed expansion, the unit will install new steam boiler (2.0 TPH) which

will be kept working and thus the existing steam boiler (1.0 TPH) will remain as

stand by. Existing thermic fluid heater will also keep working.

The unit has also provided one stand by D.G.set (500 KVA), where HSD is used as

fuel. D.G. set will be used in case of main power failure only. The detail of

existing and proposed fuel consumption is given in Table-2.12.


Table- 2.12: Details of Fuel Consumption for the existing and Proposed Expansion:

Status Daily Fuel ConsumptionSr.

No. Fuel Used In Existing Proposed Existing Total after

expansion

1 Steam Boiler – 1.0 TPH Working Stand by

2 Steam Boiler – 2.0 TPH NA Working

3

Agricultural Waste

Thermic Fluid Heater – 6.0 Lac Kcal/ hr

Working Working

2.4 MT/DAY

12.0 MT/DAY

4 HSD D. G. set – 500 KVA

Standby Stand by 100 lit 400 lit

2.10.3 ELECTRICITY REQUIREMENT

At present the total connected load of power is about 350 KVA and which is

expected to be increased up to about 750 KVA after proposed expansion. Thus,

the additional power requirement for the proposed expansion will be 400 KVA,

which will be procured from Paschim Gujarat vij Company Ltd. (PGVCL)

subsidiary of Gujarat Electricity Board (GEB).

2.10.4 MANPOWER REQUIREMENT

The manpower is one of the main resource requirements for the operation and

maintenance of the plant in a better and efficient way. At present, total 109

numbers of staff is required which will increase up to 168 after proposed

expansion. Thus, there will be additional 59 nos. of manpower will be required

for the proposed expansion. The details of Manpower requirement for existing

unit as well as for proposed expansion are given in Table- 2.13.


Table – 2.13: Details of Manpower requirement

Man

agem

ent

Staf

f*

Supe

rviso

ry

Staf

f*

Cle

rks*

Wor

kers

*

Tota

l*

Descriptions

E P T E P T E P T E P T E P T

Administration 2 1 3 2 1 3 3 1 4 7 7 14 14 10 24

Plant (Production & other services

personnel) 7 4 11 30 12 42 1 2 3 40 21 61 78 39 117

Stores & Dispatch 1 1 3 4 4 8 - - - 12 5 17 17 10 27

Total 10 6 17 36 17 53 4 3 7 59 33 92 109 59 168 *E-Existing, P-Proposed, T-Total after proposed expansion

2.11 ENVIRONMENTAL POLLUTION AND CONTROL MEASURES

2.11.1 WATER POLLUTION

A) DETAILS OF WATER CONSUMPTION & WASTEWATER GENERATION

M/s. Sam Finechem Ltd. is the existing unit and proposes to increase the

production capacity by manufacturing new products of same category. Water

is mainly required for manufacturing process, APCE and steam boiler to make

up the losses, besides it is also require for the cooling tower makeup and

washing. Based on the material balance and technical experience of the unit,

the water consumption and wastewater generation for various categories have

been calculated. The entire water requirement of the proposed unit will be met

through own bore well. Presently, total fresh Industrial water consumption is 21.0

KLD including process, APCE, boiler, cooling and washing, which will increased

up to 39.5 KLD. Water required for domestic and gardening purpose is 2.0 KLD

which will be increased up to 6.5 KLD after proposed project.

The product wise water consumption & waste water generation is given in Table

– 2.14 and category wise water consumption and waste water generation is

given in Table – 2.15 & Table – 2.16. The water balance diagram for existing and

after proposed expansion is given in Drawing-2.4 & Drawing-2.5 respectively.


Table – 2.14: Product wise Water Consumption & Wastewater Generation after proposed expansion

Water Consumption, Liter Wastewater Generation, Liter Sr. No. Stream

Per Batch Per Kg Per Day Per Batch Per Kg Per Day

A-1 PROCESS 10500.0 11.7 4487.2 10990.0 12.2 4696.6 A-2 PROCESS 0.0 0.0 0.0 3800.0 4.2 1623.9 A-3 PROCESS 1000.0 9.1 3496.5 1065.0 9.7 3723.8 A-4 PROCESS 4390.0 14.6 5628.2 6430.0 21.4 8243.6 A-5 PROCESS 3100.0 15.5 5961.5 4570.0 22.9 8788.5 A-6 PROCESS 2000.0 6.7 2564.1 3905.0 13.0 5006.4 A-7 PROCESS 5000.0 5.6 2136.8 8680.0 9.6 3709.4 A-8 PROCESS 40.0 1.1 439.6 900.0 25.7 9890.1 A-9 PROCESS 50.0 1.7 641.0 85.0 2.8 1089.7

A-10 PROCESS 800.0 7.3 2797.2 1800.0 16.4 6293.7 A-11 PROCESS 1400.0 12.7 4895.1 1950.0 17.7 6818.2 A-12 PROCESS 0.0 0.0 0.0 10.0 0.5 192.3 A-13 PROCESS 1400.0 12.7 4895.1 2200.0 20.0 7692.3 A-14 PROCESS 295.0 4.9 1891.0 790.0 13.2 5064.1 A-15 PROCESS 350.0 0.7 269.2 650.0 1.3 500.0 A-16 PROCESS 600.0 6.7 2564.1 740.0 8.2 3162.4 MAX of A-Process 10500.0 15.5 5961.5 10990.0 25.7 9890.1 B-1 PROCESS 500.0 2.8 1068.4 0.0 0.0 0.0

PROCESS 2500.0 3.3 1282.1 3632.0 4.8 1862.6 B-2

APCE 3212.8 4.3 1647.6 1479.2 2.0 758.5 B-3 PROCESS 500.0 8.3 3205.1 677.5 11.3 4342.9 B-4 PROCESS 500.0 2.9 1131.2 402.0 2.4 909.5 B-5 PROCESS 400.0 3.3 1282.1 430.0 3.6 1378.2 B-6 PROCESS 400.0 13.3 5128.2 1056.0 35.2 13538.5 B-7 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-8 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-9 PROCESS 750.0 15.0 5769.2 1425.0 28.5 10961.5 B-10 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-11 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-12 PROCESS 800.0 12.3 4733.7 1115.0 17.2 6597.6 B-13 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-14 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-15 PROCESS 20.8 0.8 320.5 0.0 0.0 0.0 B-16 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 B-17 PROCESS 3000.0 15.0 5769.2 3436.0 17.2 6607.7 B-18 PROCESS 2142.9 42.9 16483.5 2728.6 54.6 20989.0 B-19 PROCESS 1666.7 33.3 12820.5 2222.2 44.4 17094.0 B-20 PROCESS 25.0 5.0 1923.1 134.0 26.8 10307.7 B-21 PROCESS 600.0 3.3 1282.1 804.0 4.5 1717.9




B-22 PROCESS 1000.0 8.7 3344.5 1200.0 10.4 4013.4

B-23 PROCESS 1500.0 10.0 3846.2 2313.0 15.4 5930.8

B-24 PROCESS 125.0 2.5 961.5 219.0 4.4 1684.6

MAX of B- Process 3000 42.9 16483.5 3632.0 54.6 20989.0

MAX of B- APCE 3212.8 4.3 1647.6 1479.2 2.0 758.5

C-1 PROCESS 0.0 0.0 0.0 0.0 0.0 0.0

C-2 PROCESS 0.0 0.0 0.0 512.0 1.0 196.9

PROCESS 0.0 0.0 0.0 0.0 0.0 0.0 C-3

APCE 396.0 1.0 190.4 440.0 1.1 211.5

PROCESS 2500.0 12.5 2403.8 4746.0 23.7 4563.5 C-4

APCE 140.0 0.7 134.6 200.0 1.0 192.3

C-5 PROCESS 1200.0 8.0 1538.5 1410.0 9.4 1807.7

MAX of C-Process 2500.0 12.5 2403.8 4746.0 23.7 4563.5

MAX of C- APCE 396.0 1.0 190.4 440.0 1.1 211.5 D-1 PROCESS 500.0 2.8 320.5 1690.0 9.4 1083.3 D-2 PROCESS 2600.0 15.8 1818.2 1685.0 10.2 1178.3

PROCESS 1500.0 8.8 1018.1 2526.0 14.9 1714.5 D-3 APCE 676.1 4.0 458.9 1045.1 6.1 709.4 D-4 PROCESS 1000.0 4.0 461.5 1675.0 6.7 773.1 D-5 PROCESS 1667.0 3.0 349.7 3250.0 5.9 681.8 D-6 PROCESS 549.5 2.2 253.6 646.0 2.6 298.2 D-7 PROCESS 225.6 2.3 260.3 336.1 3.4 387.8 D-8 PROCESS 666.7 6.7 769.2 1100.0 11.0 1269.2 D-9 PROCESS 285.7 2.9 329.7 661.4 6.6 763.2 D-10 PROCESS 300.0 1.5 173.1 1416.0 7.1 816.9 MAX of D-Process 2600.0 15.8 1818.2 3250.0 14.9 1714.5

MAX of D -APCE 676.1 4.0 458.9 1045.1 6.1 709.4 E-1 PROCESS 400.0 2.1 161.9 450.0 2.4 182.2 E-2 PROCESS 500.0 2.8 213.7 880.0 4.9 376.1

E-3 PROCESS 4500.0 37.5 2884.6 7041.0 58.7 4513.5

E-4 PROCESS 500.0 2.3 174.8 2030.0 9.2 709.8

E-5 PROCESS 500.0 2.8 213.7 1700.0 9.4 726.5 E-6 PROCESS 1500.0 15.0 1153.8 4083.0 40.8 3140.8

PROCESS 3000.0 60.0 4615.4 4613.0 92.3 7096.9 E-7 APCE 490.0 9.8 753.8 700.0 14.0 1076.9




MAX of E- Process 4500.0 60.0 4615.4 7041.0 92.3 7096.9

MAX of E- APCE 490.0 9.8 753.8 700.0 14.0 1076.9

PROCESS 514.3 5.1 395.6 694.3 6.9 534.1 F-1

APCE 53.3 0.5 41.0 76.2 0.8 58.6

MAX of F -Process 514.3 5.1 395.6 694.3 6.9 534.1

MAX of F - APCE 53.3 0.5 41.0 76.2 0.8 58.6

G-1 PROCESS 758.6 15.2 583.6 776.9 15.5 597.6

G-2 PROCESS 375.0 7.5 288.5 802.5 16.1 617.3

MAX of G-Process 758.6 15.2 583.6 802.5 16.1 617.3

PROCESS 12000.0 104.3 8026.8 13721.0 119.3 9177.9 H-1

APCE 450.0 3.9 301.0 500.0 4.3 334.4

H-2 PROCESS 1900.0 11.9 913.5 2658.0 16.6 1277.9

MAX of H-Process 12000.0 104.3 8026.8 13721.0 119.3 9177.9

MAX of H -APCE 450.0 3.9 301.0 500.0 4.3 334.4

PROCESS 2045.5 40.9 3146.9 0.0 0.0 0.0 I-1

APCE 98.2 2.0 151.1 142.2 2.8 218.8

I-2 PROCESS 1470.6 58.8 4524.9 1686.8 67.5 5190.0

I-3 PROCESS 0.0 0.0 0.0 1066.1 26.7 2050.2

I-4 PROCESS 0.0 0.0 0.0 1662.5 16.6 1278.8

MAX of I -Process 2045.5 58.8 4524.9 1686.8 67.5 5190.0

MAX of I - APCE 98.2 2.0 151.1 142.2 2.8 218.8

Total - Process 44813.3 -- -- 59773.3

Total - APCE 3543.9 -- -- 3368.2


Table – 2.15: Category wise Water Consumption

Water Consumption, m3/day Sr.No. Category E* P* T* 1 Domestic 2.0 4.5 6.5 2. Gardening 0.4 15.0 15.4 3. Industrial

a. Process Fresh 2.0 11.9 13.9

Reuse 3.0 28.6 31.6 b. APCE 1.0 2.6 3.6 c. Boiler Fresh 11.0 -11.0 0.0 Reuse 1.0 21.0 22.0 d. Cooling 6.0 12.0 18.0 e. Washing 1.0 3.0 4.0

Total Industrial (Fresh + Reuse) 25.0 68.1 93.1

Industrial Reuse 4.0 49.6 53.6 Total Industrial (Fresh) 21.0 18.5 39.5

Total (Domestic + Gardening + Industrial) 23.4 38.0 61.4

Table – 2.16: Category wise Wastewater Generation

Wastewater Generation, m3/daySr.No. Category

E* P* T* 1 Domestic 2.0 4.0 6.0 2. Gardening Nil Nil Nil 3. Industrial a. Process 4.0 57.0 61.0 b. APCE 1.3 3.5 4.8 c. Boiler 0.0 2.0 2.0 d. Cooling 0.0 0.0 0.0 e. Washing 1.0 3.0 4.0 Total Industrial (Generation) 6.3 65.5 71.8

E-Existing, P: Proposed, T: Total after proposed expansion


Drawing – 2.4: Water Balance Diagram (Existing)

Note: All quantities are expressed In KL / Day.

To soak pit via septic tank system

Loss(11.0)Loss(1.0)

Fresh Water (23.4)

Fresh Industrial (21.0)

Domestic(2.0)

Gardening(0.4)

Boiler(Make up)

(11.0)

(Nil)

Cooling(Make up)

(6.0)

(Nil)

Washing

(1.0)

(1.0)

APCE

(1.0)

(4.0)

Process

(2.0)

To ETP, Evaporator & TFD

Zero Industrial Effluent Discharge

Reuse (3.0)

Reuse(1.0)

(6.3)

Solid waste from Dryer (1.0)

(1.3)

Evaporation Loss (1.3)


Drawing – 2.5: Water Balance Diagram (After proposed expansion)

Cooling (Make up)

To soak pit via septic tank system

Domestic (6.5)

Note: All quantities are expressed In KL / Day.

Loss(18.0) Loss(20.0)

Fresh Water (61.4)

FreshIndustrial

(39.5)

Gardening (15.4)

Boiler(Make up)

(Nil)

(2.0)

(18.0)

(Nil)

Washing

(4.0)

(4.0)

APCE

(3.6)

(4.8)

Process

(13.9)

To ETP, MEE & TFD

Zero Industrial Effluent Discharge

Reuse(31.6) Reuse

(22.0)

(71.8)

Solid waste from Dryer (13.4)

(61.0)

Evaporation Loss (4.8)


B) WASTEWATER MANAGEMENT SYSTEM

At present industrial effluent generation @ 5.0 KL/day is taken to own effluent

treatment plant comprising of primary treatment units where waste water is

treated by physico chemical treatment. The treated waste water is further

passed through Multiple Effect Evaporator followed by Thin Film Dryer. After

evaporation and condensation, water is reused as boiler feed water & in

process. The solid waste generated is disposed to the Gujarat Enviro Protection

Infrastructure Ltd. (GEPIL) TSDF site. Thus, the unit maintains "Zero Effluent

Discharge."

After proposed expansion the waste water generation will be @ 71.8 KL/day.

New effluent treatment plant having total capacity of 75 KL/Day with the same

treatment scheme will be installed along with the additional multiple effect

evaporators & thin film dryer. Then the treated water will be reused as boiler

feed water & in process. Thus, there will be a Zero Effluent Discharge from the

proposed expansion also.

Domestic effluent is discharged into soak pit through septic tank and same

practice will be continued after the proposed expansion.

The detail of existing & proposed effluent treatment plant is given hereunder in

Table-2.17 (A) & (B) and schematic flow diagram of proposed ETP is given in

Drawing - 2.6.

Table-2.17 (A) : Detail of effluent treatment plant (Existing)

Sr.No. Units N

os.

Leng

th, m

Wid

th,

m

Liqui

dDe

pth,

m

Liqui

dVo

lum

e,

m3

1. Oil & Grease Trap 3 1.50 1.20 2.0 10.8

2. Neutralization cum Treatment Tank 2 10.0 3.0 2.0 120.0

3. Settling Tank 1 3.0 3.0 2.0 18.0

4. Sludge Drying Bed 3 5.0 2.0 1.0 30.0


Table-2.17 (B) : Detail of effluent treatment plant (Proposed)

Treatment Scheme:

(1) Oil Grease trap:

The wastewater generating from various manufacturing activities is first

passed through oil & Grease chamber where emulsified oil, grease and

other floating matter is removed or skimmed off manually.

(2) Neutralization cum collection tank:

The raw effluent generated due to manufacturing activities will be

collected in neutralization cum collection tank where it will be neutralize by

chemical dosing.

(3) Chemical Dosing Tanks (Lime, Alum and Polyelectrolyte Dosing Tank):

The chemical dosing tanks will be provided for the preparation of chemical

solution required for the primary treatment such as hydrated lime and

alum.

(4) Primary Settling tank/Primary Clarifier:

Presently, effluent from collection tank is led to Primary settling tank where

the effluent is retained for the certain period in a relatively quiescent state.

Sr. No. Units N

os.

Leng

th, m

Wid

th,

m

Liqui

dDe

pth,

m

Liqui

dVo

lum

e, m

3

1. Oil & Grease Trap 3 1.50 1.20 2.0 10.8

2. Neutralization cum Treatment Tank 2 10.0 3.0 2.0 120.0

3. Chemical Dosing Tank 2 1.0 1.0 1.2 2.4

4. Primary Clarifier 1 4.0 3.0 37.70

5. Treated water collection Tank 1 4.0 3.0 3.0 36.0

6. Filter Press 1 24'' X 24"X 35 Plates

7. Sludge collection Tank 1 3.0 3.0 3.0 27.0


Thus, chemical flocs having higher specific gravity then the liquid are tends

to settle to the tank bottom.

During proposed expansion, the effluent from collection tank will be led to

Primary clarifier where with same phenomenon; chemical flocs will be

settled to the tank bottom. The clear supernatant effluent from tank

overflow will be taken to the treated water collection tank.

(5) Sludge drying bed/Filter Press

Presently, settled sludge from the bottom of Primary settling tank is drained

into Sludge drying bed. Here free water from the sludge is filter through bed

and filtrate is taken back to the neutralization tank. The sludge after drying

is removed, collected and stored in to hazardous waste storage area.

During proposed expansion, the settled sludge at the bottom of the clarifier

will be collected in sludge collection tank from where it will be taken to

filter press through mud pump. The filtered sludge will be removed,

collected and stored in to hazardous waste storage area.

(6) Treated water collection tank

A treated effluent from primary settling tank/clarifier will be collected here.

The whole wastewater will be then passed through Multi Effect Evaporator

and thin film dryer.

Multi Effect Evaporator System/Thin Film Dryer:

Multi effect evaporator is used to evaporate entire quantity of effluent. Thin Film

Dryers is used for continuous drying of heat sensitive products with total solvent

recovery. Finally evaporated and condensed water is reused for manufacturing

process. Concentrated Sludge generated during the MEE system is transferred

to Sludge drying bed. The dried sludge is packed and stored in solid waste

storage site and finally sent to TSDF site of Gujarat Enviro Protection

Infrastructure Ltd. (GEPIL) for final disposal.

During the study period composite sampling of the effluent, treated in the ETP

has been carried twice in a month and the details of analysis of the samples

taken form inlet of MEE is given in Table – 2.18.


Table – 2.18: Sampling analysis of effluent at inlet of the MEE

Sr.No.

Date of Sampling pH TDS TSS COD BOD O&G Cl- SO4-2 NH3-

N1 12/10/10 7.38 1408 120 60 21 0.8 985 40 1.8 2 26/10/09 7.12 1468 116 72 26 0.9 897 52 1.7 3 18/11/10 7.25 1554 64 118 30 1.2 410 74 1.7 4 28/11/10 7.34 1612 61 98 32 0.8 435 70 1.6 5 09/12/10 7.26 1880 75 103 28 0.9 765 56 1.5 6 20/12/10 7.15 1798 83 88 23 1.0 694 50 1.8

GPCB Norms 6.5-8.5 2100 100 100 30 10 600 1000 50

Drawing- 2.6: Flow Diagram of Effluent Treatment Plant


The details of Technical Specification and operating parameters for existing

Multiple (Triple) Effect Evaporator and Thin Film Dryer (TFD) are given in Table-

2.19 & Table-2.20 respectively along with the Drawing-2.7.

Table 2.19: Technical Specification of MEE

EQUIPMENT MULTIPLE EFFECT EVAPORATOR (2FF+1FC)

TYPE TRIPLE EFFECT EVAPORATOR WITH TVR

CAPACITY 1,186 kg/h WATER EVAPORATION

MOC TUBES SS 316 VAPOUR CONTACT PARTS SS 304

OPERATING PARAMETERS Unit Value

Feed rate (kg/h) 1,482

Feed temperature OC 30 Initial solids (%) 8.0

Total suspended solids PPM < 500

Specific gravity of feed Kg/m3 1.04

Solids in concentrate (%) 40

Concentrate output (kg/h) 296

Water evaporation (kg/h) 1,186

SERVICES/UTILITIES REQUIRED

Dry saturated steam Requirement at 8 kg/cm2-g

(kg/h) 285

Steam economy (kg of water evaporation / kg of steam)

-- 4.17

Cooling water circulation Rate at 30°c

(m3/h) 18

Power installed (excluding cooling tower and cooling water pump)

(kW) 20

Power consumed (kWH/H) 16

Compressed air requirement at 6 kg/cm2-gpressure

(nm3/h) 4

Cooling water inlet temp. (°C) 30 – 32

Cooling water outlet temp. (°C) 38 – 40

Tolerance:All performance figure within +5%All consumption figure within +10%


Table-2.20: Technical specification of TFD

EQUIPMENT Thin Film Dryer

CAPACITY 124 evaporation kg/h water

Parameters Unit Value

Feed rate kg/h 220

Initial feed solid content % 40

Final moisture in dry baggable

product % 8 - 10

Water evaporation kg/h 124

Solid output in baggable form at 8% -10% moisture content

kg/h 96

Dry saturated steam requirement at 7 kg/cm2-g pressure

kg/h 161

Electrical load (excluding cooling tower and Cooling water pump)

kW 18

Normal consumption kWH/hr 15

Cooling water circulation Rate at 30°c – 32°c

m3/h 12

Cooling water inlet temp. °C 30 – 32

Cooling water outlet temp. °C 38 – 40

Tolerance:

All performance figure within + 5%

All consumption figure within +10%

Rap

id E

nviro

nmen

tal I

mpa

ct A

sses

smen

t Rep

ort

P

age

: 281

of 2

94

Cha

pter

-2 P

roje

ct D

escr

iptio

n

Draw

ing-

2.7

: P &

I Di

agra

m o

f Effl

uent

Trea

tmen

t Pla

nt


2.11.2 AIR POLLUTION

As unit proposes to expand production capacity of existing products with the

introduction of some new products of the same category, the source of air

pollution will remain same after proposed expansion. Only quantity of gaseous

pollutants will increase as mentioned below. There will be also chances of

fugitive emission due to manufacturing activities and raw material handing and

transportation.

(A) Process Gas Emissions

The various process gases viz, HCl, HBr, Ammonia and SO2 will be generated

from the manufacturing of various products. The details of gaseous pollutants

emission due to existing as well as proposed manufacturing activities are given

in Table – 2.21 & Table – 2.22 respectively.

Adequate scrubbing system is provided for the control of process gas emission.

The details of process gas stacks and scrubbing system (existing & proposed)

are given hereunder in Table-2.23 and Table-2.24 respectively. The schematic

diagram of air pollution control measure is given as Drawing – 2.8 & 2.9.

Table – 2.21: Details of existing Air Pollution Measures for Process Gas Emission

Air Pollution Control Equipment Sr. No.

Scrubberattached to

ReactorAir Pollutant

1st Stage 2nd Stage

1. APCM-1 HCl and SO2, HBr, HCl Water Scrubber –A

Caustic Scrubber-B

Table – 2.22: Details of proposed Air Pollution Measures for Process Gas Emission

Air Pollution Control Equipment Sr. No.

Scrubberattached to

Reactor Air Pollutant

1st Stage 2nd Stage1. APCM-2 HCl and HBr Scrubber –C Scrubber-D

2. APCM-3 NH3 Scrubber –E --


Table – 2.23: Details of Process Gas Stack

Sr.No. Stack attached to Height

(m) Dia.(m)

Temp(°C)

PolluantConcentration

mg/NM3

1. APCM-1 15 0.05 40

2. APCM -2 15 0.05 40

HCl < 20 mg/Nm3

SO2 < 40 mg/Nm3

HBr < 30 mg/Nm3

3. APCM -3 12 0.025 40 NH3 < 175 mg/Nm3

Table – 2.24: Details of Scrubbing System

Sr.No.

Size of Scrubber, meter

(Ht. & Dia.)

Scrubbing Media

Capacity of Scrubbing Tank, KL

PumpCapacity

M3/Hr Output

Existing

A 6.0 x 0.30 Water 1.0 7.5 HCl (30 %), HBr (24.45), Liquor

NH3 (10%)

B 4.5 x 0.30 Caustic 1.0 18.0 To ETP

Proposed

C 6.0 x 0.30 Water 1.0 7.5 HCl (30 %), HBr (24.45), Liquor

NH3 (10%)

D 4.5 x 0.30 Caustic 1.0 18.0 To ETP

E 6.0 x 0.30 Water 1.0 7.5 Liquor NH3 (10%)


Drawing–2.8 – Schematic Diagram of Air Pollution Control Equipment (2 nos.)–HCl, HBr /SO2

Caustic Solution

HCl, HBr /SO2 gas

Caustic Solution Storage

Tank

SMF

Circulation Pump

Circulation Pump

Water Tank

By Product (HCl / HBr)

Outlet Gas

Blower

By Product (NaBr/NaHSO3)


Drawing –2.9 – Schematic Diagram of Air Pollution Control Equipment – NH3

B) FLUE GAS EMISSION

Presently, the unit has installed one steam boiler (1.0 TPH - Working) and thermic

fluid heater (6 Lac Kcal/hr – stand by) where FO was used as fuel. Now, the unit

has switched over to agricultural waste to be use as fuel. Unit will install new

steam boiler (2.0 TPH) during proposed expansion. Thus, existing steam boiler

(1.0 TPH) will be kept stand by. Existing Thermic fluid heater will be kept working.

There will be common stack attached to existing/proposed steam boiler and

thermic fluid heater, thus there is no need of any additional flue gas stack after

proposed expansion. However, fuel consumption and hence flue gas volume

NH3 gas

Blower

Water tank

SMF

Liq. NH3

(sold as by product)

Circulation Pump


will be increased after proposed expansion. Since, agricultural waste is used as

fuel in the steam boiler and thermic fluid heater; the unit has provided separate

Cyclone Separator attached to the each as an APCM, which will be adequate

after proposed expansion.

Adequate stack height of 31 m is provided for proper dispersion of pollutant to

the common stack of boiler & thermic fluid heater. The unit has also provided

one D. G. set (500 KVA) where HSD is used as fuel. D.G. Set will be used in case

of main power failure only. The flue gas emission will be well within gaseous

emission norms described by the GPCB. The details of flue gas are given

hereunder in Table-2.25.

Table – 2.25: Details of Flue Gas Stack

Status* Sr. No.

Stack Attach to E P

Ht. m

Dia.m Type of Fuel Concentration

of Polluants

AirPollution Control

Measures Steam

Boiler-1 TPH W S Cyclone Separator

Steam Boiler-2 TPH NA W Cyclone

Separator 1Thermic

Fluid Heater-6 Lac Kcal/

hr

W W

31 0.45 Agricultural waste

Cyclone Separator

2 D.G. set-500 KVA S S 31 0.1 HSD

PM < 150 mg/Nm3

SO2 < 100 ppm NOx < 50 ppm

Not Required

*E-Exiting, P-Proposed expansion, W-Working, S-Stand by NA-Not Applicable

STACK HEIGHT CALCULATION & VERIFICATION:

As per the GPCB/CPCB guidelines, the evaluation of height for the stack

proposed by the unit has been worked out considering capacity of fuel

consumption and is explained in Table-2.26.


Table – 2.26: Stack height calculation

Stack Height Parameter Unit Value

Stack ID -- 1Stack Attached to -- Steam Boiler Fuel name -- Agricultural Waste

Working Hours Nos. 20 MT/Day 12.00 Fuel Consumption MT/Hour 0.60

Based on Sulfur ContentSulfur Content % 0.08 Total Sulfur Load Kg/hr 0.48000 Sulfur Removed by limestone Dosing % 0.00 Sulfur Capture by limestone Dosing Kg/hr 0.00 Sulfur Emission into Flue gas Kg/hr 0.480

Kg/hr 0.96 SO2 emission into flue Gas gm/sec 0.2667 Stack Height required Meter 13.83 Based on Ash Content Ash Content % 19.40 Total Ash Load MT/hr 0.1164

% 60Bottom Ash Removal MT/hr 0.0698 Ash Load to APCE MT/hr 0.0466

Ash Removed by Air pollution Equipment % 80

Ash removed by APCE MT/hr 0.0372 MT/hr 0.0093 PM Emission into Flue Gas gm/sec 2.587

Stack Height required Meter 20.94 Final Stack Height required Meter 20.94 Stack Height Proposed Meter 31.0

Thus the maximum height required is 20.94 m, whereas the proposed stack height is 31 meter which will be adequate for proper dispersion of the flue gas.

During the study period monitoring of the common stack attached to the

existing/proposed steam boiler & thermic fluid heater as well as process gas

stack attached to and scrubber has been carried out monthly and the details

of stacks gas emissions are given in Table – 2.27. Copy of Monthly analysis report

by third party is attached as Annexure-XVI.


Table – 2.27: Analysis of Gas StackCommon stack attached to boiler & thermic fluid heater Stack attached to Scrubber

Sr.No.

SamplingDate PM,

mg/Nm3SOX,ppm

NOX,ppm

HClMg/Nm3

HBr,Mg/Nm3

SO2Mg/Nm3

1 12/10/10 77 6.8 0.72 10.8 - 12.8 2 26/10/09 96 7.1 0.64 8.7 - 10.7 3 18/11/10 104 5.4 0.45 4.9 - 15.2 4 28/11/10 112 6.3 0.54 - 1.8 19.4 5 09/12/10 82 5.4 0.40 - 2.0 12.6 6 20/12/10 114 5.7 0.45 5.6 - 10.9

GPCB Norms 150 100 50 20 5 40

C) FUGITIVE EMISSIONS:

There are chances of fugitive emission due to storage & handling and loading

unloading of Raw materials, product and by-product, manufacturing activity,

transportation of vehicles and scrubbing system. The unit will take adequate

precaution for the control of fugitive emission.

An action plan to control and monitor secondary fugitive emissions from all the

sources as per the latest permissible limits issued by the Ministry vide G.S.R. 414(E)

dated 30th May, 2008

G.S.R 414(E) dated 30th May is related to Sponge iron Plant (Rotary Kiln),

whereas ours is a Bulk drug and drug intermediate manufacturing unit and

therefore an action plan to control and monitor secondary fugitive emissions

from all the sources as per the latest permissible limits issued by the Ministry vide

G.S.R. 414(E) dated 30th May, 2008 is not applicable to our unit. Copy of the

G.S.R. 414(E) is attached as Annexure-III for reference.

However, Unit has taken following control measures for fugitive emission and

same will be followed after proposed expansion.


Control Measures For Fugitive Emission during material handling and process:

The entire manufacturing activities are carried out in the closed reactors

and regular checking and maintenance of reactors and distillation

column is carried out to avoid any leakages.

All the motors of pumps for the handling of hazardous chemicals are

flame proof and provided with suitable mechanical seal with stand by

arrangement.

Vacuum distillation with double condenser system is adopted.

The Control of all parameters on a continuous basis is done by adequate

control valves, pressure release valves and safety valves etc.

All the flange joints of the pipe lines are covered with flange guards.

All the raw materials are stored in isolated storage area and containers

are tightly closed.

Precautionary measures are also being taken while handling various

hazardous chemicals.

There is also provision of adequate ventilation system in process plant and

hazardous chemical storage area.

A regular preventive maintenance will be planned to replace or rectify all

gaskets, joints etc.

The unit has also developed green belt within the factory premises to

control the fugitive emission from spreading in to surrounding

environment.

Control measures for Fugitive Emission during Transportation Activity

The project site is located in the Industrial area, which is well connected to the

National Highway No. 8B. Hence there is an easy and fast accessibility within the

Industrial area. The area has good road network within and all roads are pucca

and asphalted. Hence there is almost no chance of particulate matter got

airborne due to the vehicular movement. Incremental traffic due to the

proposed expansion of M/s. Sam Finechem Ltd. will be very less and hence

there will be very less chance of air pollution due to the vehicular emission from


the proposed project. However, the unit proposes to adopt following measures

to reduce the air pollution due to the transportation activity.

All the internal roads within premises will be asphalted or concreted to

avoid dust formation caused by movement of vehicles.

Adequate parking space for trucks within the premises will be provided.

Transporter will be instructed to cover the trucks, entering in to the

premises for transportation of raw materials and products, by tarpaulin

sheets.

The PUC of the vehicles entering the industrial premises will be checked

regularly.

The owned vehicles will be serviced at a regular interval of time.

2.11.3 HAZARDOUS / SOLID WASTE GENERATION

The main sources of hazardous waste generation from proposed manufacturing

activity will be Process Waste viz. Spent Solvent, Spent Carbon, Spent Catalyst

and Distillation Residue and Dried sludge generated from effluent treatment

plant. The ancillary source of hazardous waste generation will be discarded

bags/bottles/drums/Carboys/Containers from storage and handling of raw

materials and spent oil generation from plant machinery. The details of

hazardous waste generation and handling / Management are given in Table-

2.28.


Table-2.28: Detail of Hazardous Waste Generation and management

Quantity per Annum Source Type of waste Cat.

E P T

Physical- Chemical

Form

Method of Disposal

Spent Solvent 20.2 2.16 KL

1710.57 KL

@1712.73 KL/Annum

Liquid- Organic

Collection, Storage,

recovery & reuse within the

process

Distillation Residue 36.2 7.2

MT 275.0

MT 282.2

MT Semisolid inorganic


Transportation, Disposal by

incineration at near by CHWIF.

Spent Catalyst 35.2 0.05 MT

0.1MT 0.15 MT

Collection, Storage & reuse

within the process or sold to registered reprocessors

Spent Carbon 28.2 0.6MT 14.0 MT 14.6 MT

Used Ion Exchange

Resin 34.2 0.05

MT 0.1MT

0.15 MT

Semisolid organic

Process

Solid waste from

Centrifuge 36.1 8.5

MT 375.0

MT 382.5 MT Solid Inorganic

EMS ETP Waste 34.3 14.4 MT 12.0 MT 26.4 MT Solid-

organic


Transportation & disposal at

TSDF site

Raw Material

Storage & Handling

Discarded Container

bags/bottles/ drums/Carboys

33.3 3.6MT 32.4 MT 36.0 MT Solid-

Inorganic

Send back to vendor for reuse OR

Decontaminate and sell

Plant and Machineries Used Oil 5.1 0.09

KL 2.0KL 2.09 KL Liquid-

Organic

Reused as lubricant within

premises

Calorific value of the organic waste is given in Table -2.29.

Sr. No Particular Calorific Value

1. ETP Sludge < 300 K.cal/Kg

2. Distillation Residue 1000-1500 K.cal/Kg

The unit has provided designated storage area of 1,463 sq. m for the hazardous

waste storage within premises having impervious floor and roof cover system


and leachate collection system which will be expanded upto 1,795 sq. m during

proposed expansion.

The unit has already obtain membership of the nearest TSDF/CHWIF site of

Gujarat Enviro Protection Infrastructure Ltd. (GEPIL) for disposal of resins, spent

carbon, distillation residue & ETP waste. As no incineration will be carried out on

site thus, no need to provide design details of the Incinerator.

The unit will developed proper procedure for handling of ETP and other

hazardous waste.

1. The ETP sludge generated will be collected in the HDPE bags/MS drums

after complete sun drying.

2. The bags will be sealed or tightly closed.

3. The tightly closed HDPE bags will be labled as “ETP Sludge/Hazardous

waste”.

4. After that the bag will transferred through the trolley to the designated

storage area.

5. The bags will be sent to nearest TSDF/CHWIF site at a regular interval of

time for final disposal.

6. Proper log book and record of the waste generated, disposed at TSDF site

or sold data will be maintained.

Discarded container/Barrels/Bottles/Bags/drums will be sent back to vendor or it

will be reused again in the plant after decontamination. The unit will also

develop proper procedure for decontamination of discarded

container/barrel/Bottles/Bags/drums which is given below.

1. Empty container/barrel/Bottles/Bags/drums will be sent to

decontamination area after ensuring that it is completely empty and the

lids are tightly closed.

2. Treated wastewater of the existing ETP will be used to clean the

containers/Barrels/Liners.

3. 20 to 30 lit of water will charged and lid will be closed properly.


4. Container/Barrels/Liners/drums will be rolled on the ground for 2 to 3

minute and than will be emptied. The procedure will be repeated for 2 to

3 times. The water from cleaning will be sent to propose Effluent

Treatment Plant.

5. The second wash will be carried out by 10% solution of either acid or

alkali. Then final wash will be carried out with treated water.

6. The label “DECONTAMINATED” will be sticked on washed containers

/Barrels/Liners/drums and it will be transfer to decontaminated storage

area.

7. From the storage area containers/Barrels/Liners/drums will be reuse or sell

to scrap vendor.

The unit will also keep the records of the empty container generated and

disposed in the register.

2.11.4 NOISE POLLUTION

Noise is an unwanted sound and excessive noise is harmful to health and

diminishes the quality of life. Thus, noise is considered as one of the potential

pollutant. Management of noise includes the monitoring and controlling of

noise levels, at source, the transmission paths and the surrounding environment.

There will not be any major source of noise generation due to proposed project.

The only source of noise generation is the vibrating noise from the operation of

plant and machineries from the proposed manufacturing activity. One of the

auxiliary sources of noise generation would be from transportation within and

out side the premises. However, for the abatement of noise pollution, following

precautions will be taken by the unit;

Latest low noise D.G. Sets are in place with acoustic enclosure to reduce

the noise generation.

Proper and timely oiling, lubrication and preventive maintenance will be

carried out for the machineries and equipments to reduce noise

generation.


The noise generation will be mitigated by installing noise barriers/absorbers

around stationery noise sources. Adequate noise control measures such as

anti vibration pad for equipment with high vibration will be provided.

All the vibrating parts will be checked periodically and serviced to reduce

the noise generation. The equipment, which generates excessive noise, will

be provided with enclosures etc.

To minimize the adverse effect on the health, Ear muffs/ earplugs will be

provided to the workers working under high noise area.

To reduce the noise generation during the transportation activities; the

transport contractor will be instructed kept vehicle periodically serviced

and maintain as per the requirement of latest trend in automobile industry.

Only those vehicles with PUC’s will be allowed for the transportation.

The transport contractor will be informed to avoid unnecessary speeding of

vehicles inside the premises.

Noise monitoring will be done regularly at different parts of the plant.

Green belt area will be developed to prevent the noise pollution outside

the factory premises.

c) Summary of mass balance - Gujarat Pollution Control...

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