Brief Summary of the Project

Sr.
Item Details
No.
1. Name & Address of the M/s. OC Specialities Pvt. Ltd.
Project Plot No. E-18, Tal. Mohol, Chincholi MIDC Area, Solapur, Maharashtra
2. Name of the applicant & Mr. Vikas M. Shah
Designation Director
3. Type of Project Proposed Fine Chemical Intermediates Manufacturing Unit
4. Capacity of Project Manufacturing set-up shall be for production of 21 products.
5. Land acquired • Total Land – 8450 Sq. M.
• Built - Up Area – 3149.8 Sq. M.
• Open Space Available – 3647.2 Sq. M.
• Green Belt Area in MIDC plot – 2166.85 Sq. M. (59.40 % of open space)
6. Cost of the Project
Total Investment – Rs. 5.14 Crores.
7. Production Capacities
Sr. Name of the Product Quantity Uses
No. (MT/M)
1. Sodium Bromide Soln. Oil Drilling Additive &
OR 390 Water treatment
Sodium Bromide 232 chemicals
Powder
Zinc Hydroxy OR 106 Additive in Natural
Zinc Oxide 74 Rubber
2. Di Isopropyl Ethyl Amine Pharma Intermediate
18.18
(DIPEA)
3. Methyl-2-Chloro Phenyl Pharma Intermediate
10.3
Acetate
4. 4 Methoxy Phenyl Pharma Intermediate
10
Acetone
5. Pharma & Diamide
2,3 Dichloro Pyridine 10
Intermediate
6. 2-Amino-2-Phenyl Pharma Intermediate
6.5
Butyric Acid
7. Ortho Hydroxy Phenyl Cosmetic Intermediate
15
Acetic Acid
8. 2 Coumaranone 12.4 Pharma Intermediate
9. 3-Isochromanone 12 Pharma Intermediate
10. 2,6 Dichloro Benzoyl 22.1 Intermediate for
Chloride Fungicide
11. Methyl-2-Dimethylamino- Pharma Intermediate
10
2-Phenyl Butyrate
12. 2-Dimethylamino-2- Comestics Intermediate
3.01
Phenyl Butanol
13. P-Bromonisole / 4-Bromo Pharma Intermediate.
16.5
Anisole
14. Para Bromo Pharma Intermediate.
Phenetole/4- 14.5
Bromophenetole
15. 2,4 - Dichloro phenyl Intermediate for
39.75
acetyl Fungicide.
16. 2,5 – Dimethyl phenyl Intermediate for
32.5
acetyl chloride Insecticide.
Sr.
Item Details
No.
17. Indoline 36.25 Cosmetics Intermediate
18. Ethyl Phenyl Glyoxalate Cosmetics Intermediate
28.42
(EPG)
19. Ethyl – 1- Hydroxy Pharma Intermediate
33
cyclohexane carboxylate
20. Ethyl – 1- Hydroxy cyclo Pharma Intermediate
35.25
pentane carboxylate
21. 3 – chloro – 2 - 36 Polymer synthesis.
hydrazinylpyridine
Name of the Byproduct
1. Sodium sulphite 182.07 Detergent Soap
soln.25%
2. HCl 30% 75.59 Reused for Chlorination
3. Sodium Nitrite soln.30% 30.42 Reused
4. Distillation residue of P- 3.6 Solvent
xylene
5. Ammonium Chloride 36 Used as buffer solution
8. Air Pollution Control A D.G. Set of 200 KVA capacity would be installed. HSD would be used as
Measures fuel and the consumption rate would be about 75 Lit./Hr. The D.G. Set
would be operated only during power failure.

Sr.
Description Specifications
No.
(a) Stack Number (s) 1 1
(b) Attached to Boiler TFH DG Set
(c) Capacity 3 TPH 6 Lakhs 200 KVA
Kcal/Hr
(d) Fuel type Coal/Biomass Coal/Biomass HSD
(e) Fuel quantity 18 MT/Day/ 100 Kg/Hr / 75 Lit. / Hr.
36 MT/Day 220 Kg/Hr
(f) Material of RCC M.S
construction
(g) Shape Round Round
(round/rectangular)
(h) Height, m (above 30 M 3M
ground level)
(i) Diameter/size, in 0.5 M 0.1 M
meters
(j) Ash Content % Coal - 5 % / Biomass – 3 % 0.1 %
(k) Sulphur content % Coal - 1 % 1%
(l) Control equipment Multicyclone Multicyclone --
preceding the stack Dust Dust
Collector Collector
(MDC) (MDC)
followed by followed by
Bag Filter Bag Filter
Sr.
Item Details
No.
9. Water Requirement
Sr. No. Description Water Consumption
(M3/Day)
#
1. Domestic 5
($4 + #1)
2. Industrial
#
a. Processing 17
b. Washing *3
c. Cooling *8
d. Boiler Feed *8
e. Scrubber *2
38
Industrial Total
(#17 + *21)
3. Other (Gardening) *2
• 45
Grand Total
(#18 + *$27)
Note: Out of the total water consumption, 23 CMD (57%) is DEE
Condensate to be recycled, 0.5 CMD for Ash quenching.
#
MIDC Water Source, * Use of the condensate water from the DEE and
$
Rain water

10. Effluent Generation

Sr. No. Description Effluent Generation
(M3/Day)
1. Domestic 4.5
2. Industrial
a. Processing 20
b. Lab & Washing 2.5
c. Cooling Blow Down 1
d. Boiler Blow Down 1
e. Scrubber 0
Industrial Total 24.5
Total (1 & 2) 29
• Grand Total 29
11. Solid Waste Type of Waste Solid waste generation Disposal
Coal Ash 1.5 MT/Day Sold to brick
manufacturers for
Biomass Ash 1 MT/Day secondary use
12. Hazardous Waste
Sr. Description Quantity Mode of
No. Disposal
1. Cat.: 34.3 - ETP 0.35 MT/Day CHWTSDF
Sludge
2. Cat.: 28.1 - 13.14 MT/M Outside
Process Residue (3.6 MT/M would be sold to Parties/
outside parties and 9.54 CHWTSDF
MT/M would be forwarded
to CHWTSDF)
3. Cat.: 20.3 - 21.2 MT/M CHWTSDF
Distillation Residue
Sr.
Item Details
No.
13. Green Belt
Total land area for Proposed Fine Chemicals & Intermediates
manufacturing unit is 8450 Sq. M.

Proposed Green Belt Area– 2166.85 M2 (59.40 % of open space)

1070 nos. of trees would be planted under the proposed green belt
development plan.
 MANUFACTURING PROCESS

1. SODIUM BROMIDE / ZINC HYDROXIDE / ZINC OXIDE

[Solid NaBr / NaBr Liquid 40%]

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. Zinc Bromide 70% 6000 Kg = 42000 Kg (100%)
2. Caustic Soda 1600 Kg
3. Water 4800 Ltrs

A] REACTION:

ZnBr + 2 NaOH Zn (OH)2 + 2 NaBr

Zinc Bromide Caustic Soda Zinc Hydroxide Sodium Bromide

M.W. = 224 M.W. = 2 X 40 M.W. = 99 M.W. = 224
= 80 = 208

B] BRIEF PROCESS:

Charge:
• 4800 Ltrs water, add under stirring.
• 1600 Kg Sodium Hydroxide Flakes stirred to dissolve completely.

Add:
6000 Kg Zinc Bromide Solution (70%) from top in 3 Hrs, stir well for 1 Hrs & centrifuged
washed with 100 Ltrs water.

Output:
• Sodium Bromide 40 % solutions 9750 Kg.
• Zinc Hydroxide (wet Cake 30% moisture content) 2650 Kg.

69
 2. DI ISOPROPYL ETHYL AMINE [DIPEA]

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)
1. DI Isopropyl Amine [DIPA] 3030 Kg
2. DI Ethyl Sulphate [DES] 2100 Kg
3. Caustic Soda Flakes (47%) 1160 Kg = 545 Kg on 100%
4. Water 400 Ltrs

A] REACTION:
C3H7
C3H7
2NH + (C2H5)2SO4 + NaOH 2N C2H5 + NaHSO4 + H2O
C3H7
C3H7

Di Isopropyl Di Ethyl Caustic Soda Di Isopropyl Sodium Bi Water

Amine Sulphate M.W. = 40 Ethyl Amine Sulphate M.W.= 18
M.W. = 2 X 101 M.W. = 154 M.W. = 2X 129 M.W.= 120
= 202 = 258

B] BLOCK DIAGRAM:

Recovery of DIPA 570 Kg

Di Isopropyl Amine (3030

Di Ethyl Sulphate (2100 Kg)

Distillation
Of
Caustic Soda Solution (47% 1160 Kg) Ethylation 3750 kg organic
(100% 545 Kg) layer Output
3030 Kg
Water 400 Ltrs

Aqueous
Layer 2940
Kg
C] BRIEF PROCESS: 150 Kg Pitch

Charged Isopropyl Ethyl Amine & Diethyl Sulphate stirred well, then slowly added from
the top caustic solution after completion of addition, heated for 3 Hrs. allow it to settle.
Separate aqueous layer & organic layer. Organic layer is taken for recovery of DIPA &
fractional distillation of DIPEA

70
 3. METHYL-2-CHLORO PHENYL ACETATE

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. 2-Chlorophenyl Acetic Acid 1000 Kg
2. Methanol 500 Kg
3. Sulphuric Acid (98%) 50 Kg
4. Sodium Carbonate 3 Kg
5. Water
Solution
12 Kg

A] REACTION:

CH2COOH CH2COOH

Cl H2SO4 Cl
+ CH3OH

OCPA Methanol Methyl-2-Chlorophenyl

M.W. = 170.5 M.W = 32 Acetate
M.W. = 184.5

B] BLOCK DIAGRAM:
Methanol
Recovered 300
Sodash Solution (15 Kg) Kg (Recycled)

Methanol 500 Kg
Methyl-2-
2-Chlorophenyl Acetic Acid 1000 Kg Chlorophenyl
Esterification
Acetic Acid
Distillation 1030 Kg
Sulphuric Acid (98% 50 Kg) Pure
99.5%

Waste Sulphuric Aqueous Pitch 55 Kg

Acid 165 Kg Layer 15 Kg

180 Kg

71
 C] BRIEF PROCESS:

Charged Methanol, 2-Chlorophenyl Acetic Acid & Sulphuric Acid. Start heating,
maintain reflux temperature for 4 Hrs. Start recovery of excess of Methanol which is
recycled in the next batch. Allow it to settle. Separate aqueous Sulphuric Acid then add
Sodium Carbonate solution to neutralize the mass, separate aqueous
layer. Organic material taken for distillation.

4. 4-METHOXY PHENYL ACETONE

•
List of Raw Material
Sr. No. List of Raw Materials Batch Qty. (Kg)
1. 4-Methoxy Benzaldehyde / P-Anisaldehyde 1000
2. 2-Chloro Methyl Propionate 975
3. Sodium Methoxide (Powder) 440
4. Sulphuric Acid (98%) 400
5. Caustic Soda Flakes 300
6. Water 1750

CH3
A] REACTIONS:
CH C COOH3
1) H3CO O
CH
CHO NaCOH3 H3CO
+ CH3 CH COOH3 + NaCl +CH3OH
Sodium
Methoxide
M.W. = 122.5
Sodium
Para Methyl-2-Chloro Epoxy Ester Methanol
Chloride
Anisaldehyde Propionate M.W. = 222 M.W. = 32
M.W. = 58.5
M.W. = 136 M.W. = 122.5

2)
CH3 CH3

CH C COOH3 CH C COONa
O O

H3CO H3CO
+ NaOH + CH3OH

Epoxy Ester Caustic Soda Glycidic Acid Methanol

M.W. = 222 M.W. = 40 Sodium Salt M.W. = 32
M.W. = 230
 3) CH3 CH3
CH C COONa CH C COOH
O O

H3CO H3CO
2 + H2SO4 2X + Na2SO4

Glycidic Acid Sulphuric Acid Glycidic Acid Sodium Sulphate

Sodium Salt M.W. = 98 M.W. = 2 X 208 M.W. = 142
M.W. = 2x 230 = 416
= 460

CH3

4) CH C COOH CH2 C CH3

O
O

H3CO H3CO
2X 2X + CO2

Glycidic Acid 4- Methoxy Phenyl Carbon

M.W. = 2 X 208 Acetate Dioxide
= 416 M.W. = 2 X 164 M.W. = 44
= 328

B] BLOCK DIAGRAM:

400 Kg 98% + CO2

Caustic Soda
323 Kg
Para Anisaldehyde 300 Kg 100 Ltrs Water
1000 Kg + Methanol
Water 1650 Dilute Sulphuric 515 Kg
Ltrs Acid (80%)

2- Chloromethyl
Propionate Decarboxylation &
975 Kg Epoxidation Hydrolysis of Separation of Distillation
Ester Aqueous Layer 4-Methoxy
Phenyl
Acetate
Sodium Methoxide 440 Kg Pitch 200 Kg 1000 Kg
Aqueous Pure 99%
Layer 2827 Kg
C] BRIEF PROCESS:
2-Chloromethyl Propionate is charged along with Para-Anisaldehyde under stirring.
Reaction mass is cooled & Sodium Methoxide is charged lot-wise. After completion of
addition stirred for 3-4 Hrs till reaction is completed. Add Caustic Soda solution &
material is heated to reflux. Dilute sulphuric acid is added slowly till pH is 2. Reaction
mass is maintained at reflux temperature till completion of reaction. Allow it to settle to
remove aqueous layer. Organic layer is taken for distillation to get pure 4-Methoxy
Phenyl Acetone.
 5. 2, 3-DICHLORO PYRIDINE

FOR STEP I & II

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. 3-Amino Pyridine 250
2. Hydrochloric Acid [35-37% w/w] 2500
3. Hydrogen Peroxide [50% w/w] 194
4. Sodium Nitrite [NaNO2] 194 31 %
soln
5. Water 420
6. Water 1750

FOR STEP III

Sr. No. List of Raw Materials Batch Qty. (Kg)
1. (35-37% w/w) Hydrochloric Acid 400
2. Sulphuric Acid 42
3. Cupric Chloride Dihydrate 42
4. Sodium Hydroxide Flakes 835 40%
w/w
5. Water 1570

A] REACTIONS:

STEP- I CHLORINATION OF 3-AMINO PYRIDINE:

NH2 NH2

Cl

+ HCl + H2O2 + 2H2O

N N

3-Aminopyridine Hydrochloric Hydrogen 3-Amino-2- Water

M.W. = 94.12 Acid Peroxide Chloropyridine M.W. = 18
(35-37%) (50% w/w) M.W. = 128.56
M.W. = 36.5 M.W. = 34

STEP- II DIAZOTISATION OF 3-AMINO-2-CHLOROPYRIDINE:

NH2 N NCl

Cl Cl
2HCl
+ NaNO2 + + 2H2O + NaCl
0-5°C

N N

Diazonium
3-Amino-2- Sodium Salt Water Sodium
Chloropyridine Nitrite M.W. = 18 Chloride
M.W. = 128.56 M.W. = 69 M.W. = 58.5

74
 B] BLOCK DIAGRAM: Hydrochloric N2 gas
Acid (30%) 74 Kg
400 Kg 2, 3-Dichloropyridine
210 Kg Water
+ wet 320 Kg
NaNO2 194 Kg Cupric +
Chloride Caustic Soda Water 1875 Ltrs.
42 Kg 835 Kg (Recycled)
420 Kg
Hydrochloric Acid (30%) Water
Sulphuric Water Isopropyl Alcohol
2500 Kg
Acid 1570 Kg 75 Kg
(80%)
3-Amino Crystallization
Pyridine Steam of 2, 3-
250 Kg Chlorination Diazotisation Decomposition of
Distillation Dichloro-
Diazonium Salt
pyridine 300 Kg

Hydrogen Peroxide (50%) 2, 3-

194 Kg Aqueous Dichloropyridine
Effluent 250 Kg Dry
4408 Kg Mother Liquor 125 Kg
for IPA recovery
IPA recovered 50 Kg
Bottom Discarded 75 Kg
C] BRIEF PROCESS:

STEP – I CHLORINATION OF 3-AMINO PYRIDINE:

3-Amino Pyridine is treated with Hydrochloric Acid [35% - 37% w/w] and Hydrogen
Peroxide [50% w/w].

STEP – II DIAZOSATION OF 3-AMINO-2-CHLOROPYRIDINE:

3-Amino-2-Chloropyridine formed in above step is treated with Sodium Nitrite

solution. Diazonium Salt formed.

STEP – III DECOMPOSITION OF DIAZONIUM SALT INTO 2, 3

DICHLOROPYRIDINE

Diazonium Salt is further reacted with previously heated solution of salt and acid. The
evolved Nitrogen gas is scrubbed. On addition of (40% w/w) caustic solution to adjust
pH 7-7.5 pass stream and product 2, 3-dichloropyridine starts distillating out along with
steam water.

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. Para Cresol 1080
2. Air (Oxygen) 320
3. Caustic Soda 65
4. Water 2000
5. Hydrochloric Acid 30% 200

75
 A] REACTION:

Para + Air [2(O)] P-Hydroxy + P-Hydroxy + Water

Cresol Benzaldehyde Benzoic Acid

B] BLOCK DIAGRAM:
Water
Caustic Soda Water 500 Kg
5 Kg 1500 Kg

Para Cresol 1080 Kg

P-Hydroxy
Alkali Centrifuging
Oxidation Drying Benzaldehyde
Treatment 1300 Kg
Oxygen (Air) 320 Kg 1000 kg

Aqueous Layer for

P-Hydroxy Benzoic
Acid Recovery

Acidification by
HCl 30%
200 kg

P - Hydroxy
Benzoic Acid Aqueous effluent
200 kg 2165 Kg

C] BRIEF PROCESS:

Para Cresol along with catalyst and water is fed continuously to the oxidation reactor and air
is passed at desired temperature. After maintaining period, material is continuously
withdrawn from the oxidation reactor at fixed interval. The material is further treated with
dilute Caustic Soda Solution to remove p-Hydroxy Benzoic Acid. The slurry is fed to
centrifuge washed & dried to get p-Hydroxy Benzaldehyde. The alkali aqueous layer is
neutralized with Hydrochloride acid 30% and precipitated
p-Hydroxy Benzoic Acid is centrifuged, washed & dried.

76
 6. 2-AMINO-2-PHENYL BUTYRIC ACID

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

Moles Per Mole
1. Propiophenone 550 Kg = 4.10 1
2. Methanol 700 Kg
3. Ammonium Bicarbonate 660 Kg = 8.35 2.036
4. Sodium Cyanide 225 Kg = 4.59 1.12
5. Acetic Acid 135 Kg = 2.25 0.55
6. Water 800 Kg + 1725 kg
7. Sodium Hydroxide Flakes 675 Kg = 16.87 4.11
8. Hydrochloric Acid (30% w/w) 2000 Kg = 16.44 4.00
600 Kg (100 %)

A] REACTIONS:
HN
1) O O C C O
II
C – C2H5 C2H5 C NH

+ NaCN + 2NH4HCO3 + NaHCO3 + NH4OH + H2O

Propiophenol Sodium Ammonium 5-Phenyl-5- Sodium Ammonium Water

M.W. = 134 Cyanide Bicarbonate Ethyl Hydention Bicarbonate Hydroxide M.W. = 18
M.W. = 49 M.W. = 2 X 79 M.W. = 204 M.W. = 84 M.W. = 34
= 158
2)
HN
O C C O COONa

C2H5 C NH C2H5 C NH2

+ NaOH + 2H2O + NH4HCO3

5-Phenyl-5- Ethyl Caustic Soda Water Sodium Salt 9, 2- Ammonium

Hydention M.W. = 40 M.W. = 2X 18 Amino- 2- Phenyl Bicarbonate
M.W. = 204 = 36 Butyric Acid M.W. = 79
M.W. = 201
3) COONa
COOH
C2H5 C NH2
C2H5 C NH2

+ HCl + NaCl

Sodium Salt 9, 2- Hydrochloric Acid 2-Amino -2- Phenyl Sodium Chloride

Amino- 2- Phenyl M.W. = 36.5 Butyric Acid M.W. = 58.5
Butyric Acid M.W. = 179
M.W. = 201

77
 B] BLOCK DIAGRAM:

Acetic Acid
135 Kg

Caustic Soda Water

Water
675 Kg 1525 Kg
300 Ltrs
Propiophenone
550 Kg

Ammonium Bicarbonate
660Kg 1000 Kg 5-Phenyl
Autoclave Neutralization -5-Ethyl Hydention
Sodium Cyanide Centrifuging
225 Kg 7.75 Autoclave
Water
500 Ltrs Aqueous
Layer
STAGE – II 2070 Kg

Water
HCl 30% 200 Ltrs
2000 Kg Water Vapour
150 Kg

650 Kg Dry
Drying 800 Kg 2 –Amino, 2- Phenyl
Neutralization Centrifuging 2 –Amino, 2- Phenyl Butyric Acid
7.0 Butyric Acid

Aqueous
Layer
4600 Kg

C] BRIEF PROCESS:

Charge in to autoclave, Propiophenone, Methanol, Ammonium Bicarbonate, Sodium

Cyanide, Water. Close the autoclave. Heat to get desire temperature & pressure. After
completion of reaction, material is acidified to adjust pH 7.0 then centrifuged to get 5-
Phenyl-5-Ethyl Hydention. It is further treated in autoclave with Caustic Soda solution. It is
further neutralized with 30% HCl to adjust pH 7.0 to 7.5. It is then centrifuged washed
with water, dried to get 2-Amino-2-Phenyl Butyric Acid.

78
 7. ORTHO HYDROXYL PHENYL ACETIC ACID /
2-HYDROXY PHENYL ACETIC ACID

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)
1. 2-Chloro Phenyl Acetic Acid 1000
2. Caustic Soda Flakes 940
3. Copper Sulphate.7H2O 40
4. Hydrochloric Acid (30% w/w) 2850
5. Water 2200

A] REACTIONS:
1)
CH2COOH CH2COONa

Cl ONa
+ 3NaOH + NaCl + 2H2O

Ortho Chloro Caustic Soda Sodium Salt of 2- Sodium Water

Phenyl Acetic M.W. = 3 X 40 Hydroxy Phenyl Chloride M.W. = 2 X 18
Acid = 120 Acetic Acid M.W. = 58.5 = 36
M.W. = 196

2)
CH2COONa CH2COONa

ONa ONa
+ 2 HCl + 2NaCl

Sodium Salt of 2- Hydrochloric 2-Hydroxy phenyl Sodium

Hydroxy Phenyl Acid Acetic Acid Chloride
Acetic Acid M.W. = 2X 36.5 M.W. = 152 M.W. = 2 X 58.5
M.W. = 196 = 73 = 117

3)

NaOH + HCl NaCl + H2O

Caustic Soda Hydrochloric Sodium Water

M.W. = 40 Acid Chloride M.W. = 18
M.W. = 36.5 M.W. = 58.5

79
 B] BLOCK DIAGRAM:

Hydrochloric
Acid (30%)
2200 Kg
Water Vapour
150 Kg
HCL 30% 650 Kg
2 chlorophenyl
Water 200 Kg
Acetic Acid 1000 Kg

Caustic Soda
Flakes 940 Kg Ist Neutralize nd
II Neutralize
Autoclave Solution Solution Drying Wet cake
Centrifuging
Water Pressure pH 2.0 900 Kg
2000 Ltrs 14-16 Kg 6.5 to 7.0

Copper Sulphate.7H2O Aqueous

40 Kg Layer
6070 Kg
750 Kg 2-Hydroxy
Phenyl Acetic Acid

C] BRIEF PROCESS:

In autoclave charge water, caustic Soda flakes, Copper Sulphate.7H2O and Orthochloro
Phenyl Acetic Acid and heated till desire pressure is reached.

Reaction temperature is maintain till completion of reaction. Autoclave is cooled and

material transferred to neutralization tank. The hydrochloric Acid is added till pH 6.5 to 7.0
and allowed to settle. The bottom Copper sludge is separated. The material is further
neutralized to pH 2. It is then cooled to 200C.It is then cooled to 200C. It is centrifuged,
washed with water, dried to get

80
 8. 2-COUMARANONE

List of Raw Materials:

Sr. No. List of Raw Material Batch Qty. (Kg)
1. Ortho Hydroxy Phenyl Acetic Acid 750

A] REACTION:

CH2COOH

CH2
OH
C
+O 2 + H 2O

O
2-Hydroxy Phenyl 2-Coumaranone Water
Acetic Acid M.W. = 134 M.W. = 18
M.W. = 152

B] BLOCK DIAGRAM:

100 Kg water Vapour

Ortho Hydroxy Phenyl

Acetic Acid 750 Kg Distillation
of 620 Kg
Dehydration
Crude 2- 2-Coumaranone
Coumaranone

30 Kg Pitch
C] BRIEF PROCESS:

Ortho Hydroxy Phenyl Acetic Acid is charged into reactor and heated to 150° C to distilled
out water of reaction. Vacuum is applied and crude 2-Coumanone is distilled to get pure
2-Coumanone

81
 9. 3- ISO CHROMANONE

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)
1. Ortho Methyl Phenyl Acetic Acid 1000
2. Mono Chlorobenzene 1500
3. Catalyst 20
4. Chlorine 408
5. Ammonia 840
6. Water 2000
7. Toluene 600

A] REACTIONS:

1) CH3 CH2 Cl

CH2OOH CH2OOH

+ Cl2 + HCl

Ortho-methyl Chlorine 2- Chloromethyl Hydrochloric

Phenyl Acetic Acid M.W. = 71 Phenyl Acetic Acid Acid
M.W. = 150 M.W. = 184.5 M.W. = 36.5

2)
CH2 Cl

CH2OOH CH2
O
+ NH4OH + NH4Cl
C O
CH2

2- Chloromethyl Ammonia 3- Iso Chromanone Ammonium

Phenyl Acetic Acid M.W. = 148 Chloride
M.W. = 184.5 M.W. = 53.5

82
 B] BLOCK DIAGRAM:

Hydrochloric
Acid (30%)
210 Kg
N2 Toluene 600 Kg

840 Kg Ammonia Water 2000 Kg 600 Kg

(25%) MCB (Recovered) 3-Iso Chromanone
1300 Kg 99.5
Ortho methyl phenyl
Acetic Acid 1000 Kg
MCB Recovery 3- Iso Centrifuging
Mono Chloro Crystallization
Benzene 1500 Kg Chlorination Cyclisation by Distillation Chromanone &
625 Kg
pH 6.8-7.0 Distillation Drying
Catalyst
20 Kg Aqueous effluent
3298 Kg
Pitch
Chlorine 408 Kg Toluene (550 Kg)
60 Kg
Toluene recovered (400 Kg)
Crude 3-IC (25 Kg)

C] BRIEF PROCESS:

Charge into glass lined reactor 2-Methyl Phenyl Acetic Acid, Mono Chlorobenzene and
Catalyst .chlorine is pass at 900C till desire conversion is obtained. The evolved
hydrochloric acid is scrubbed in to water. After completion of reaction nitrogen is purged
to remove HCl from the system. Material is cooled to 250C and ammonia solution is
added till pH 6.5 -7. After reaching pH 6.5 -7 organic layer is separated & washed with
water, unreacted 2-Methyl Phenyl Acetic Acid is recovered by acidification of aqueous
layer. Organic layer is distilled to recovered MCB. The bottom left material 3-IC is distilled
under high Vaccum and further crystallized in Toluene. Toluene is recovered from mother
liquor by distillation.

83
 10. 2, 6- DICHLORO BENZOYL CHLORIDE

List of Raw Materials:

Sr. No. List of Raw materials Batch Qty. (Kg)
1. 2,6 Dichloro Benzaldehyde 900
2. Nitric Acid 60% 1350
3. Sodium Hydroxide Flakes 230
4. HCl 30% 650
5. Thionyl Chloride 1170
Thionyl Chloride (Recovered) 500
Thionyl Chloride (Consumption) 670
6. Water 650

A] REACTIONS:
1)
CHO COOH
Cl Cl Cl Cl

+ HNO3 + HNO2

2, 6 Dichloro Nitric Acid 2, 6 Dichlorobenzoic Nitrous Acid

Benzaldehyde M.W. = 63 Acid
M.W. = 175 M.W. = 191
2)
COOH COONa
Cl Cl Cl Cl

+ NaOH + H 2O

2, 6 Dichlorobenzoic Sodium Hydroxide 2, 6 Dichlorobenzoic Water

Acid M.W. = 40 Acid Sodium Salt M.W. = 18
M.W. = 63 M.W. = 213
3)
COONa COOH
Cl Cl Cl Cl
+ HCl + NaCl

2, 6 Dichlorobenzoic Hydrochloric Acid 2, 6 Dichlorobenzoic Sodium Chloride

Acid Sodium Salt M.W. = 40 Acid M.W. = 58.5
M.W. = 213 M.W. = 191
4)
COOH COOH
Cl Cl Cl
Cl
+ SOCl2 + SO2 + HCl

2, 6 Dichlorobenzoic Thionyl 2, 6 Dichlorobenzoyl Sulphur Hydrochloric

Acid Chloride Chloride Dioxide Acid
M.W. = 191 M.W. = 119 M.W. = 209.5 M.W. = 64 M.W. = 36.5
84
 B] BLOCK DIAGRAM:

Nitrous acid Caustic Soda Water

240 Kg 230 Kg 500 Kg HCl 30%
650 Kg

2, 6
Dichlorobenzaldehyde
900 Kg
Neutralization Acidification
Oxidation Centrifuging 2, 6 DCBA pH 6.5-7.0
Nitric Acid 60% 980 Kg
w/w 1350 Kg

1030 Kg Nitric
Acid 48%
Recycled
SO2 390 Kg

Thionyl
Water Water
Chloride HCl 215 Kg Thionyl
150 Kg 30 Kg Chloride
500 Kg
Recycled

Centrifuging Pure 2,
2, 6 DCBA Drying 6
2, 6 DCBA Distillation Dichloro
wet cake 950 Kg Benzoyl
950 Kg
980 Kg Chloride
Pitch
190 Kg

1505 Kg
Aqueous
to ETP

C] BRIEF PROCESS:

STEP – I : OXIDATION OF 2,6 DICHLORO BENZALDEHYDE

2, 6 Dichloro Benzaldehyde is treated with nitric acid 60%.The evolved nitric acid is
Scrubbed into caustic soda solution to get sodium nitrite solution which is sold in the
market. The 2, 6 Dichloro Benzoic acid formed is cooled & centrifuged. It is further
neutralized with caustic soda solution, clarified and neutralized with Hydrochloric acid
30%. The Precipitated 2, 6 Dichloro Benzoic acid is centrifuge, washed with water &
dried.

Step – II

The dry 2, 6 Dichloro Benzoic acid is further treated with Thionyl Chloride. The
evolved gas of Sulphur Dioxide is scrubbed in to caustic soda solution and Hydrogen
Chloride gas is scrubbed in to water scrubber. After completion of reaction excess
Thionyl Chloride is distilled & recycled and bottom material is Vaccum distilled to get
pure 2, 6 Dichloro Benzoyl Chloride.

85
 11. METHYL – 2 – DIMETHYL AMINO – 2 – PHENYL BUTYRATE

Sr. List of Raw Materials Batch Qty. (Kg)

No. Moles Per Mole
1. 2-Amino-2-Phenyl Butyric Acid 1000 = 5.586 1
2. Toluene 1800
3. Dimethyl Sulphate 760 = 6.03 1.079
4. Sodium Hydroxide Flakes 40 = 1.0
5. Formic Acid 800 = 14.78 2.646
6. Formaldehyde 37% w/w 407 Kg 100% 1100 = 13.56 2.427
7. Water 1800

A] REACTIONS:

1)
COOH COOCH3

NH2 C C2H5 NHCH3 C C2H5

Toluene
+ (CH3)2SO4 + H2SO4

2-Amino - 2 – Dimethyl Methyl -2 – Mono Sulphuric Acid

Phenyl Butyric Sulphate Methyl Amine-2- M.W. = 98
Acid M.W. = 126 Phenyl Butyrate
M.W. = 179 M.W. = 207

2)

COOCH3 COOCH3

NHCH3 C C2H5 N(CH3)2 C C2H5

+ HCOOH + CH2O + CO2 + H2O

Methyl -2 – Mono Formic Formaldehyde Methyl-2-Dimethyl Carbon Water

Methyl Amine-2- Acid M.W. = 30 Amino – 2 – Dioxide M.W. = 18
Phenyl Butyrate M.W. = 46 Phenyl Butyrate M.W. = 44
M.W. = 207 M.W. = 221

86
 B] BLOCK DIAGRAM:
CO2 490 kg

Water Caustic Soda Formic Acid Formaldehyde

1500 Kg 30 Kg 800 Kg 37% 1100 Kg
Water NaOH 10 Kg
2-Amino-2-Phenyl 300 Kg
Butyric Acid 1000kg
Toluene Neutralization Methylation
1800 Kg Esterification &
pH 7-7.5
Methylation
Aqueous Aqueous
Dimethyl Sulphate Layer Effluent
760 Kg 2370 Kg 1600 Kg

Toluene 1600 Kg
Recycled

Vaccum 1000 Kg
Methyl-2-Dimethyl
Distillation Amino-2-Phenyl
Butyrate

Pitch
40 Kg

C] BRIEF PROCESS:

In a reactor, Toluene, 2-Amino-2-Phenyl Butyric Acid and Dimethyl Sulphate is charged.

After completation of reaction. Water is added. Organic layer is separated and
neutralized with caustic soda solution to pH 7 to 7.5.Organic layer is mixed with
Formaldehyde solution 37 %,formic acid 85% and reflux till completation of reaction.
Aqueous layer is separated and washed with water and neutralized with Caustic soda
solution. Toluene is recovered by distillation and recycled. The Bottom material is
Vaccum distilled. Pitch is drained.

87
 12. 2- DIMETHYL AMINO – 2 – PHENYL BUTANOL

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. Methyl-2-Dimethylamine-2-Phenyl 550
Butyrate
2. Toluene 720
3. Toluene (R) 870
4. Vitride 70% in Toluene Vitride 750 + Toluene 320
=1070
5. Sodium Hydroxide Flakes 280
6. Water 2000

A] REACTION:

COOCH3 CH2OH

N(CH3)2 C C2H5 N(CH3)2 C C2H5

7% Vitride

Methyl-2-Dimethyl 2-Dimethyl Amino-2-Phenyl

Amino-2-Phenyl Butanol
Butyrate

B] BLOCK DIAGRAM:
Sodium Hydroxide Water 2000 Kg Toluene (R) 870 Kg
280 Kg recycled

Toluene 720 Kg

Methyl-2-Dimethyl 2-(Dimethyl
Toluene Amino)-2-Phenyl
Amino-2-Phenyl
Butyrate 550 Kg Reduction Recover Butanol 430 Kg

Vitride 70% 1070 Kg

Aqueous
Layer
3150 Kg

C] BRIEF PROCESS:

In a S.S. reactor, toluene is charged along with Methyl-2-Dimethylamine-2-Phenyl Butyrate.

Vitride 70% is added from the top slowly. After completion of addition reaction is maintain
till completion. The effluent of Vitride is decomposed by addition of Caustic soda solution.
The organic layer is separated. Toluene is recovered by distillation and Product is drained
from the bottom.

88
 13. 4 – BROMO ANISOLE

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. Anisole 100
2. HBr 1625
3. Hydrogen Peroxide 50% 750 Mixed to get 30% w/w
1250 Kg
4. Water 500

5. Sodium Thiosulphate 25 Soln. 525 Kg

6. Water 500

A] REACTION:

OCH3 OCH3

+ HBr + H2O2 + 2 H2O

Br
Anisole Hydrobromic Hydrogen P. Bromo Water
M.W. = 108 Acid Peroxide Anisole M.W = 2 X 18
M.W. = 81 M.W. = 34 M.W = 187 = 36

B] BLOCK DIAGRAM:

Sodium thiosulphate solution 10 kg

water vapor
525 kg

Anisole 1000 kg
Distillation of
Hydrobromic Acid
Bromination Crude P. Bromo 1820 kg
48% 1625 kg
Anisole Crude P.
Hydrogen Peroxide
1845 Kg Bromo Anisole
30%
1250 kg

2030 kg 550 kg 160 kg filter

89
 C] BRIEF PROCESS:

In the glass lined reactor anisole and Hydrobromic Acid (48%) is charged. The materials are
cooled to 50C and then add slowly Hydrogen peroxide (30%) solution. Reaction is
exothermic. Chilling is required. Temperature is controlled between 10-120C throughout
the addition of Hydrogen peroxide solution after completion of reaction. Material is stirred at
10-150C for 1 hr check completion of reaction. conversion repeated is above 99%. If it is less
then stirred 1 hr more. After completion of reaction material allowed to settle. Separate out
bottom organic material for aqueous layer. Organic material recharged and washed with 5%
sodium Thiosulphate solution till colour changes to light yellow. Material is allowed to settle.
separate Organic layer for aqueous layer and taken for Vacuum distillation to get pure form.

14. 4 - BROMOPHENETOLE

List of Raw Materials:

Sr. No. List of Raw Materials Batch Qty. (Kg)

1. Phenetole 1000
2. Hydrobromic Acid (HBr) [48% 1450 = 696 Kg (100%)
w/w]
3. Hydrogen Peroxide (H2O2) [50% 670 = 335 Kg (100%)
w/w] 30% soln.
4. Water 430
5. Sodium Thiosulphate 25
6. Water 500

A] REACTION:

OC2H5 OC2H5

+ HBr + H2O2 + 2H2O

Br
Phenetole Hydrobromic Hydrogen Water
M.W. = 122.17 Acid Peroxide Para – Bromo M.W. = 2 X 18
M.W. = 81 M.W. = 34 Phenetole = 36
M.W. = 201.06

90
 B] BLOCK DIAGRAM: 10 Kg
Sodium thiosulphate Water
solution (5% w/w) 525 Kg Vapour

Phenetole 1000 Kg Crude

Crude
Hydrobromic Acid P - Bromo – P - Bromo –
1450 Kg P – Bromophenetole
(48% w/w) 1450 Kg Bromination Phenetole Phenetole
Pure 99%
1682 Kg 1657 Kg
Hydrogen Peroxide 2, 4 – Dibromophenetole
30% w/w) 1100 Kg Pure 175 Kg
550 Kg
1868 Kg 2, 4- Dibromo Distillation of
Aqueous
Aqueous effluent Phenetole 2, 4- Dibromo
effluent 197 kg Phenetole
22 Kg
Pitch

C] BRIEF PROCESS:

In a glass lined reactor, Phenetole and Hydrobromic acid (48 %) are charged. The
material is cooled to 50C and then add slowly Hydrogen Peroxide (30 % w/w) solution.
Reaction is exothermic. Chilling is required. Temperature controlled between 10-120C
throughout the addition of Hydrogen peroxide solution. After completion of reaction
material is stirred at 10-150C for 1 hr. Check completion of reaction. Conversion
expected is above 99%. If it is less than that stirred 1hr more. After completion of reaction
material is allowed to settle. separate out bottom organic material from aqueous layer.
Organic material is recharged and washed with 5% w/w sodium thiosulphate solution. Till
colour changes to light yellow material is allowed to settle. Separate organic layer from
aqueous layer and taken for vacuum distillation to get pured form.

15. 2, 4 – DICHLORO PHENYL ACETYL CHLORIDE

List of Raw materials:

Sr. Name of Raw Material Batch quantity

No. in Kg
1 2,4-Dichloro benzyl chloride 2000
2 Triethyl amine 20
3 Sodium cyanide 500
4 Water 4844
5 Toluene 1000
6 Sodium Hydroxide 486
7 Conc. HCl 1800
9 Thionyl chloride 944

91
 A] REACTIONS:

Stage I: Cyanation

Cl CN

Cl Cl
water,TEA
+ NaCN Toluene
+ NaCl

Cl Cl
(2,4-dichlorophenyl)acetonitrile,MW=186 Sodium Chloride,MW=58.5
2,4-Dichloro benzyl chloride,MW=195.5 sodium cyanide,MW=49

Stage II: Hydrolysis

CN COONa

Cl Cl
NaOH,Toluene + NH 3

Cl Cl
(2,4-dichlorophenyl)acetonitrile,MW =186 (2,4-dichlorophenyl)acetic acid sodium Am m onia,MW =17
salt,MW =227

HCl

COOH

Cl

+ NaCl

Cl
(2,4-dichlorophenyl)acetic acid,MW =205 Sodium Chloride,MW =58.5

Stage III: Chlorination

COOH
COCl

Cl
Cl
SOCl2 + HCl(g) + SO2(g)

Cl
Cl
Hydrochloric acid,MW=36.5 Sulfur dioxide,MW=64
(2,4-dichlorophenyl)acetic acid,MW=205 (2,4-dichlorophenyl)acetyl chloride,MW=223.5

92
 B] FLOW CHART:
Stage I :Cyanation

4)Sodium cyanide solution(500 kg in 2000 kg water)

1)Toluene(1000 Kg)
Cyanation
2)2,4-dichloor benzyl chloride(2000 Kg)

3)Triethyl amine(20 Kg) 5)Sodium Hypoch

(10% 100 Kg)

Organic layer Aqueous waste
contains excess sodium
cyanide

Organic layer Aqueous waste after

hypo treatment (2620
kg)

6)recovered toluene(950 Kg)

Crude
7)Pitch(150 kg)

Pure Stage I (1800 kg)

93
 Stage II (Hydrolysis)

1)Water(1944 Kg) 4)Ammonia gas(157 Kg)

Hydrolysis
2)Sodium Hydroxide(486 Kg)

3)Stage I(1800 Kg)

5)HCl(1800 Kg)
Isolation

6)Water washing(900 Kg) 7)Waste aqueous

Filtration
layer(5183 Kg)

Stage II(1590 kg)

Stage III (chlorination)

1)Thionyl chloride (944 Kg) 3)Sulfur dioxide gas(496

Chlorination
kg)

2)Stage II(1590 Kg) 4)HCl gas(283 Kg)

Distillation

Crude

Pure (1590 Kg)

5)Pitch (165 Kg)

94
 C] BRIEF PROCESS:
Stage I : Cyanation

2,4 dichloro benzyl chloride is coverted into cyanide by using sodium cyanide and toluene as
a solvent and triethyl amine as a base.The product is isolate by layer separation.The organic
layer is distilled out to recover toluene followed by fractional distillation gives pure product
stage I as (2,4-dichlorolphenyl)acetonitrile.The aqueous layer contains extra sodium cyanide
is destroyed by using sodium hypochlorite as a oxidizing agent.

Stage II : Hydrolysis

Stage I is hydrolyzed to acid using sodium hydroxide as a hydrolyzing agent.The product is

isolated by acidifying with hydrochloric acid and it is isolated by filtration followed by water
washing gives wet product which on drying gives stage II as a 2,4-dichloro phenyl acetic
acid.

Stage III: Chlorination:

Stage II i.e 2,4-dichloro phenyl acetic acid is converted into acid chloride using thionyl
chloride as a chlorinating agent.the liberated and hydrochloric acid gas is scrubbed into
water and sulphur dioxide gas into alkali scrubber which converts into sodium sulfite .The
product is isolated by fractional distillation gives pure product as 2,4-dichloro phenyl acetyl
chloride.

95
 16. 2,5 – DIMETHYL PHENYL ACETYL CHLORIDE

List of Raw materials:

Sr. Name of Raw Material Batch quantity

No. in Kg
1 P-xylene 1500
2 p-formaldehyde 1110
3 Conc. HCl 6095
4 Sodium carbonate 44
5 water 3669
6 Zinc Chloride 45
7 Sodium cyanide 470
9 Sodium Hydroxide 439

A] REACTIONS:
Stage I: Chloromethylation
CH3
CH3

+ HCHO + HCl
Cl

n + H2O
CH3
CH3
p-Xylene,MW=106 p-formaldehyde,MW=30 2-(chloromethyl)-1,4-dimethylbenzene,MW=154.6 water,MW=18

Stage II : Cyanation

CH3 CH3

Cl CN
+ NaCl
+ NaCN
H2O,Toluene

CH3 CH3
2-(chloromethyl)-1,4-dimethylbenzene,MW=154.6 Sodium cyanide,MW=49 (2,5-dimethylphenyl)acetonitrile,MW=145 Sodium Chloride,MW=58.5

96
 Stage III: Hydrolysis

CH3 CH3

CN COONa
NaOH,H2O
+ NH3

CH3 CH3
(2,5-dimethylphenyl)acetonitrile,MW=145 (2,5-dimethylphenyl)acetic acid sodium,MW=186 Ammonia,MW=17

HCl,MW=36.5,Toluene

CH3

COOH

+ NaCl

CH3
(2,5-dimethylphenyl)acetic acid,MW=164 Sodium Chloride,MW=58.5

Stage IV: Chlorination

CH3 CH3

COOH COCl
SOCl2
+ HCl + SO2(g)

CH3 CH3
(2,5-dimethylphenyl)acetic acid,MW=164 (2,5-dimethylphenyl)acetyl chloride,MW=182.6 Hydrochloric acid,MW=36.5 Sulfur dioxide,MW=64

B] FLOW CHART:

97
 Stage I : Chloromethylation

4)Zinc chloride(45 Kg)

1)p-Xylene(1500 kg)
Condensation
2)Conc. HCl(4665 Kg)

3)p-Formaldehyde(1110 Kg)

5)Sodium carbonate(30 kg) 7)waste aqueous layer

Isolation
6)Water(300 Kg) 5630 kg

8)Recovered xylene
Organic layer
450 kg

9)Pitch
Crude stage I
145 kg

1425 kg
Pure stage I

98
Stage II : Cyanation

4)Sodium cyanide solution(470 Kg in 1425 Kg water)

1)Toluene(712 kg)
Cyanation
2)Stage I(1425 Kg)

3)Sodium carbonate (14 kg) 5)Sodium Hypochlorite

(10 %, 300 Kg)

Organic layer Aqueous waste
contains excess sodium
cyanide

Organic layer Aqueous waste after

hypo treatment

6)recovered toluene(676 Kg)

Crude
7)Pitch(150 Kg)

Pure Stage II 1254 Kg

99
Stage III : Hydrolysis

1)Water(1317 Kg) 4)Ammonia gas

Hydrolysis
2)Sodium Hydroxide(439 Kg) 125 Kg

3)stage II(1254 Kg)

5)HCl(1430 Kg)
Isolation

7) Waste aqueous layer

Filtration
3688 kg

Wet stage III Drying

Dried stage III 1254 Kg

100
Stage IV : Chlorination

1)Thionyl chloride(953 Kg)

Chlorination 3)Sulfur dioxide(489
2)Stage III(1254 Kg) Kg)

NaOH scrubber
Distillation

Sodium sulfite

Crude
HCl(275 Kg)

Pure 5)Pitch(140 Kg)

Packing
1300 kg

C] BRIEF PROCESS:
Stage I : Chloromethylation

P-xylene is chloromethylated using p-formaldehyde and concentrated hydrochloric acid and zinc
chloride as a catalyst.The product is isolated by separating organic layer, followed by sodium
carbonate washing to remove excess acidity.The organic layer is distilled out to remove p-xylene
followed by fractional distillation gives pure product stage I as 2-(chloromethyl)-1,4-dimethylbenzene
Stage II : Cyanation
Stage I 2-(chloromethyl)-1,4-dimethylbenzene is coverted into cyanide by suing sodium cyanide and
toluene as a solvent.The product is isolate by layer separation.The organic layer is distilled out to
recover toluene followed by fractional distillation gives pure product stage II as (2,5-
dimethylphenyl)acetonitrile

Stage III : Hydrolysis

Stage II is hydrolyzed to acid using sodium hydroxide as a hydrolyzing agent.The product is isolated
by acidifying with hydrochloric acid and it is isolated by filtration followed by water washing gives
wet product which on drying gives stage III as a 2,4-dimethyl phenyl acetic acid.

Stage IV : Chlorination:
Stage III i.e 2,4-dimethyl phenyl acetic acid is converted into acid chloride using thionyl chloride as a
chlorinating agent.the liberated sulphur dioxide gas and hydrochloric acid gas is scrubbed into
scrubber. The product is isolated by fractional distillation gives pure product as 2,5-dimethyl phenyl
acetyl chloride.

101
 17. INDOLINE

List of Raw materials:

Sr. Name of Raw Material Batch quantity

No. in Kg
1 2-chloro phenyl ethyl amine 2000
2 Ethanolamine 2800
3 Xylene 2800
4 Sodium Hydroxide 515

A] REACTION:

NH2

Cl NH2
+ HO
N
H
2-(2-chlorophenyl)ethanamine,MW=155.5 Ethanolamine,MW=61 2,3-dihydro-1H-indole,MW=119

CH4
NH2
HO
NH2 .HCl
+ NaOH HO + NaCl + H 2O

Ethanolamine hydrochloride,MW=97.5 sodium Hydroxide,MW=40 Ethanolamine,MW=61 Sodium chloride,MW=58.5 water,MW=18

102
 B] FLOW CHART:
3)Xylene(2800 Kg)

1) Ethanolamine(2800 Kg)
Cyclization
2)2-chloro phenylethylamine Sodium Hydroxide(515 kg)

(2000 kg)
Bottom layer

Upper Organic Layer

Recovered
ethanolamine
Pitch(81 kg) 2750 kg
Crude
Recovered Xylene(2660 kg)
Liquid aqueous waste
(421 Kg)
Fractional distillation

Pure(1450 kg)
95% of theory

C] BRIEF PROCESS:
Brief Process:2-chloro phenyl ethylamine is cyclised to 3-indoline by using ethanolamie as a base.
The product is isolated by extraction in xylene followed by solvent distillation gives crude product
which on fractional distillation gives pure product. The by-product ethanolamine hydrochloride is
basified with sodium hydroxide liberates free base which is used in the next reaction.

103
 18. ETHYL PHENYL GLYOXALATE (EPG)
List of Raw materials:

Sr. Name of Raw Material Batch quantity

No. in Kg
1 Mandelonitrile(MN) 1320 Kg
2 Ethyl alcohol 912 kg
3 Hydrochloric acid gas 362 Kg
4 Wtaer for reaction 357 Kg
5 Toluene 660 Kg
6 Water for dissolution 660

A] REACTION:
COOC2H5
CN
H OH
H OH

+ HCl(g) Ethyl alcohol,water + NH4Cl

Toluene

Mandelonitrile,MW=133 Hydrochloric acid,MW=36.5 Ethyl Mandalate,MW=180 Ammonium chloride,MW=53.5

NaOCl,MW=74.5

O
O
OC2H5

H2O + NaCl +
Water,MW=18 Sodium chloride,MW=58.5 Ethyl phenyl glyoxalate,MW=178

104
 B] FLOW CHART:

4)Hydrochloric acid gas(362 Kg)

1)Ethyl alcohol(912 kg) 5)recovered ethyl alcohol
2)Mandelonitrile(1320 Kg) Organic Layer (406 Kg)
3)Water(357 Kg)
6)Toluene(660 Kg)

7)water(660 kg) 8)Waste water(660 Kg)

Organic Layer
Toluene (660 Kg) 9) Ammonium chloride
(534 Kg) for sell

10) Sodium hypochlorite(8000 kg) Oxidation 11) Waste water (8824

Kg)

Organic layer 12)recoverd toluene

distillation (627 Kg)

Crude EPG
13)Pitch(83 Kg)

Pure EPG
1137 Kg

C] BRIEF PROCESS:
Mandelonitrile is reacted with hydrochloric acid and water and hydrolyzed to acid which is in-situ
esterfied with etyla alcohol to give ethyl mandalate. The excess ethyl alcohol is distilled out and re-
used in the next batchs. After that water and toluene is added ,water layer is separated which
contains ammonium chloride. Organic layer contains product is oxidized with sodium hypochlorite.
The organic layer is separated followed by tolune distillation gives crude ethyl phenyl glyoxalate
which on fractional distillation gives pure ethyl phenyl glyoxalate.

105
 19. ETHYL-1-HYDROXY CYCLOHEXANE CARBOXYLATE

List of Raw materials:

Sr. Name of Raw Material Batch quantity

No. in Kg
1 1-hydroxy cyclohexane carbonitrile 1000
2 Hydrochloric acid gas 292
3 Ethyl alcohol 736
4 Water for reaction 288
5 Toluene 500
6 Water for washing 500

A] REACTION:

EtOOC OH
NC OH

HCl,C2H5OH
water,Toluene + H2O + NH4Cl

1-hydroxycyclohexanecarbonitrile,MW=125 ethyl 1-hydroxycyclohexanecarboxylate,MW=172 water,MW=18 ammonium chloride,MW=53.5

106
 B] FLOW CHART:

4)1-hydroxy cyclopentane carbonitrile(1000 Kg)

1)Ethyl alcohol(736 kg) 5)recovered ethyl alcohol
2Hydrochloric acid (292 Kg) Hydrolysis and (332 Kg)
3)Water(288 Kg) Esterification

6)Toluene(500 Kg) 8)Waste water(644 Kg)

Organic Layer
7)water(500 kg) 9) Ammonium chloride
(428 Kg) for sell

10)Recovered toluene

Organic layer distillation

(475 kg)

Crude 11)Pitch( 117Kg)

Pure ethyl-1-hydroxy-
cyclohexane carboxylate
1320 Kg

C] BRIEF PROCESS:
1-hydroxy cyclohexane carbonitrile is hydrolyzed with hydrochloric acid and esterifies with ethanol
in-situ gives desired product. The formed product is isolated by adding water followed by toluene
extraction. The aqueous layer is separated contains ammonium chloride and organic layer contains
product. The solvent is distilled out gives crude product which on fractional distillation gives ethyl-1-
hydroxy cyclohexane carboxylate.

107
 20. ETHYL-1-HYDROXY CYCLOPENTANE CARBOXYLATE

List of Raw materials:

Sr. Name of Raw Material Batch quantity
No. in Kg
1 1-hydroxy cyclopentane carbonitrile 1000 Kg
2 Hydrochloric acid gas 329 kg
3 Ethyl alcohol 829 kg
4 Water for reaction 320 Kg
5 Toluene 500 Kg
6 Water for washing 500

A] REACTION:

NC OH
EtOOC OH

HCl,C 2 H 5 O H
Toluene + H 2O + NH 4 Cl

1-hydroxycyclopentanecarbonitrile,MW =111 ethyl 1-hydroxycyclopentanecarboxylate,MW -158 water,M W =18 am m onium chloride,MW =53.5

108
 B] FLOW CHART:

4)1-hydroxy cyclopentane carbonitrile(1000 Kg)

1)Ethyl alcohol(829 kg) 5)recovered ethyl alcohol
2Hydrochloric acid (329 Kg) Hydrolysis and
3)Water(320 Kg) Esterification (375 Kg)

6)Toluene(500 Kg) 8)Waste water(662 Kg)

7)water(500 kg) Organic Layer 9) Amonium chloride (482
Kg) for sell

Organic layer 9)Recovered toluene

10) Recovered toluene
distillation
(475 Kg)

Crude 11)Pitch( 74Kg)

Pure ethyl-1-hydroxy-
cyclopentane carboxylate
1410 Kg

C] BRIEF PROCESS:
1-hydroxy cyclopentane carbonitrile is hydrolyzed with hydrochloric acid and esterifies with ethanol
in-situ gives desired product. The formed product is isolated by adding water followed by toluene
extraction. The aqueous layer is separated contains ammonium chloride and organic layer contains
product. The solvent is distilled out gives crude product which on fractional distillation gives ethyl-1-
hydroxy cyclopentane carboxylate.

109
 21. 3-CHLORO-2-HYDRAZINYL PYRIDINE

List of Raw materials:

Sr. Name of Raw Material Batch quantity

No. in Kg
1 2,3-Dichloro pyridine 2000 Kg
2 Hydrazine hydrate (60% aqueous 3587 Kg
solution)
3 n- butanol 5000 Kg
4 Potassium carbonate 1840

A] REACTION:

Cl

2 +2 NH2NH2 + K2CO3
N Cl
2,3-dichloropyridine,MW=296 Hydrazine ,MW=64 Potassium carbonate,MW=138

n-Butanol

Cl

2 + 2KCl + CO2 + H2O

NH2
N NH

3-chloro-2-hydrazinylpyridine,MW=287 Potassium Chloride,MW=149 Carbon Dioxide,MW=44 Water,MW=18

110
 B] FLOW CHART:
3)Potassium carbonate(1840 Kg) 4)Hydrazine hydrate

1) n-Butanol (4000 Kg) (3587 Kg)

2)2,3-Dichloro pyridine
SSR CO2 gas (600 Kg)
(2000 kg)

Cooling,Filtration
5)n-butanol(1000 kg)
Wet Weight

Drying

Dry weight (1800 kg)

Mother Liquor

Layer separation
Aqueous layer (5127 Kg)
Organic layer
distillation to ETP

Recovered n- Pitch (50 Kg)

butanol(4850Kg) Incineration
For re-use

C] BRIEF PROCESS:
2, 3-Dichloro pyridine is reacted with hydrazine hydrate in presence of potassium carbonate
as a neutralizing agent and n-butanol as a solvent. The product is precipitated out during
course of reaction is isolated by filtration followed by n-butanol washing gives final product 3-
chloro-2-hydrazinyl pyridine as a solid. The biphasic mother liquor is separated by layer
separation method. Aqueous layer is sent to ETP for treatment and organic layer is taken for
n-butanol distillation and recovered n-butanol is re-used for next batch. The remaining pitch
after n-butanol distillation is sent for incineration.

111
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Ill!'USTRIES, ENERGY AND' LABOUR DEPARTL'YIENT

'> antralaya, Bombay 400 032, 'dated the 12th May 1988
MlsJL\.RJ.S·h 'RA lNOUSTRtAL DEYELOPMENT ACT, 196J.
, 229
f

No .. IDC+ 218(/(10514)"'IND~!4.-ln
exercise of powers eonferred ,by
sub-section (3) of section I of ·tile Maharashtra Industrial Development
A.c~ 1961 (Mah, of 1962) the <1overnment of Maharasbtra liereby appoints rre
17fh May.. 1988 to be the date from which Chapter
+~.;:: 'm"
VI.; __of
••••
the said Act shaH
~r<~-~,
'J I ij; • _

\Tl11'
 ¥~ ~ . i{tt~l~ ~ ~~, if ~~ l'~(./~ ~ .~ ;.\~O . [~~"!:l
• take effect in the area mentioned'. in the Schedule annexed hereto. and.
. declares the said area as industrial area under clause (g) of section 2 ,Q! tb~
said Act. '. ,
, .
The said area is more clearly defined in red in ·the maps deposited in. tho
Offi~ of the Chief Executive Officer" Mabarashtra InduStrial Developntent
Corporation. Bombay 400 093,. and the. Special .Land .-Acquisi.tion Offieer,
Solapur Division. Solapur, Dis' let Solapur, and is bounded by the: .~
"as indicated in the said Schedule.' ~
, Schedule
.
.District Solapur, taluka Mohol, vil~ge Ch~holL

Gat Area Gat

No. No.
- ------~--
H.Ar~s
~----------~---
H. AtC$
I pt. ? 36·0' so 10 33-1.
4 pc 5 92-0 51/1 2 61-Q
5 3 2-0 51/2
9 2 9;-0 ,",
........
10 5l-t
7 '61'
10 pt. 6· 56-0 53 10 93"9
II pt. 1 80·0 54/f1_ 3 75'e
12 pt. 1 92-0' 54/2• - 4 94/ •
-- 13 pt. 1 92-0 54/,3 '1 20"
14 2 40'0 55 8- 34·.
IS 2 19.0 56 6 80-'
16 2 28-0 -57 6 44-0
22 .4 60-0 58 13 1:7·trJ·
2 pt I to 3 3 40-0 5-9 1 9-0
25 pt. 7 16-0 60 4 - 11-t
26 1 '97-0 61 1 89-$
27 :? 29<l .; 62
3 46"G
28 p. o 80-0 63 4 81-9
29 pt.· J . o 80-0 64 :3 '63-0
38 l! .. ~\ 14 2-0 65 4 20,0
39! 1 +:i '~ .IS 37-{) 66 . .12 42--.
L!O l ,~;
-9 56'0
4 lA/I; 6~ 5 2S·.{
'IS 44-0 68/1.'
4'; /V 3 61{} 68i2 166·~·
6tH}
43 \.~.i.. 4 10-0 69 4 11·lJ
I, 44 5 77'0 70 pr.
45 3 59'0
12 61{J il pt . :3 9(}{):
46 -3 ~S:O 72 pt
47
9 39-0
3 85'0·, 73.pt. 11 0-0
5 - ~O.O . 74 8 97'0
49 5 19·0
 .. ,
.•
Area. Gat.
• H.. ~ . _ . No,

'3 84-0 lOff 1 ~1)

75'
o 41-{) 109 '0 '39-0
,76 no.·... ' ' 43<0
71. 0 .41-0.
III
. 01 , SQ-G
.·78 0 51-0· -:
- I' 44-0
7 49{) jJ2
1P 1 35~O
...
,80 9 68,0 lIS
0 25-0 1'14 2 12{)
81 l' '42»0.
82 1 23·0 115
116/1 0 4S{)
&3 1 15'0 45-0
14-0 .116/2 Q
84 1
0 4-0 117' .2 .17-0
.,.85/1 . 0 ,31-(/
8511. 1 49-0 -llS
86- - 5. 28-0, 1.19 " .si-o
. 1 _23>0
1.1-0 -120 . . 4
.81 2 ,

'88
,
7". 14'.0 124/1 3 48-0
3 67'(} 125 '0 241).
89 ;
126{1 2 99-{)
90 4 14·0. , -2' 0-0
91 2 SS-O 126/'"
4 61-{) 127 4 .62.0
. 92·
ss 3 51>0 .• , 12$/.1
l28ff),
,
,1 60'0
1 .83{)'
i
94, 2 691> .
128/3 4 4S'{)
95 10 "88-0 1l. S(rO
5-96/1 13 90,0' ]29/1
200 129/211, "
',1 14-0
~!,'96/2 .'
~
"\
2
.
:(- '4S~O - 129/2/2 1 14-(J
,:'97/t .~~ ~ .1. '.1400
I ~'
2''' 7'0 --"---:.12912./13 -'~'" ..," "
,
..
'97/2 ·t. 7,0 >

129'lgl4
r

1 .13i)
M\
}

. '2 ' ..[ r .

'91/3 129/21-S 1 ' 14-0
93 .1 ~, 9'·48-0 ; 1 .: 14';(}
l29-fZIl5 '
99
, 100
f~\ 3,64'0·
3 ·S-O
'"
129/211 1 14-0
130 s 14-{)
lOl
102
1 89-0
4 35'0 131 ·s 94~O'
"4"~"'5£1;3 -..~::'........, 13'2 '"7"
.4 93{)
103 1, 133": . :'··5~~54·O
104 2 .g-{)
.105 5 81N) 134 7 51-{)
lil5· 14. 40'{)
106/1 . 0 38{1 24~O
-0 34-0· 135 0
106/2 137 7 45{)
106/3 0' 3s.o. 1~ 4...•. . 50'\}
JO~/4 . 0 33-<J 139 f S{)
101 0 84~Q 140 11 7~
 .•. _'lit _ .••.
~.• _ ...•.
~' ' . ....:.
__ .. n ~-,---- ----.---
An.":!
~ .. -
( "'... - ~;l\..
Area . Gat
I • uat
'It..,.•••••
l'~( .•

.
.__ .- ......•.__ -_ .,
H.
.
Arcs
"
NIJ.
.
H, Arcs

(:'1 II 84-0 79. 3 10'T>

~.;, Us :,.10 j 5 40,0
2 pt. 14 75-0
7'2 10 75'0 81 2 3-0
i3
j.4
n 57'0 82 2
2..,
39-0
3·0.
7 J5'0 B3
34-0
,
75/ S
..•1.
..,~..,'
' _
":
2
1
~J5'O
75·0
84-
8S
~
4 30-f)
! .. 3 53-0 80 4 65-0
I ,'-11
~ ...•
it)'
...
1 0 S 1-0 a7 0 43'-0
76 2 ]8·0 tS 14 1'j'(1

77 2 9"'0 ~Q l~ t 3'0
'?~
-- _.-
3 6?'(J
" -.. .- •.. __ ~~.-
_ ....
..--.-- _.., - '" -"-"""'.

Ga~ Area G~tt j\ r-e:l

!'\. H. Arcs ~o. _______ ._ • __ • __
H.
•.•••• _ ~_
Ares:
••• , /'0 ••• _ •••• "_ •• -

2 I;l 26 soc 20c,: pL 5

--
QO.()()
--
21-4 ~ ~ 7d·~, .
. '")('in
.;.}7 pt.
. - ..• ]. -
. -- .•.
~ 14 .: 12 3'2'0
- - --,-...:..--,.,..,
.- ~ ~ --
-
- .--~
..•.
- ...• - P'!

- If,'HI' ,/,Pfrs-:.-
t tv: (he East by--Gnt Nos. !4,1 5. J 9. 20. 25. 56, 62. 64 pt.. 65 pl ..•
fl(~ rr.. 07 pt., 68 pt., 70 pr., 90. Q2. 94, 95. 98. 104. l05. "'06. of villagr
K~"ndi. -" J

On the West by-Oat Nos. 52,,14'8' pt., ISS, J56•. 151. (58. )83.. 1~
I is\!. J90. 230 pt., 231 Pt.1 233 pt ... of -<jiUage Cbincholi, and Bo,undZl1
l~f Village Sawleshawar.
d" the North by-Boundav of Villaaes Darfal and Akole,
I. .• ow
~ ,.~. '
0" fir S'ltith by-Gat Nos. 1 pt. 4 ft .. 6. 8. 10 pt.. ~I pt .. 12 'fK-.
fJ pt.. 1\.~ ~ pt:, 2~ pt., 25 pt., 28 pt. 29 .pt., J2, 37. 70 pf .. 71 p!.
72 pt., . d 73 pt.. of Village Chincholi and Pune-Solanur Nntion~1
H·I~\;\\'a
L..
:.
J'l
O. 7.
N' •

i :l!
'ByQrdct and in' the name of· the Governor0f Me harashtra, .:
M, D~.SARV!.' .•..."r.AR-
-oe~.... om cer.
 ; r

:q~l~q m~f~~~~, i; ;.:~, t\~':'j~itt<, ~J, ~{; -1I(, 9 0 r·~'~~l~<..;(

INDUSTRJEs: ENERG Y A..~D l:ABOlJR {)EPART~1ENT

. Muntralaya, Bombay 40i>v32. dated 13th May 1988
1tJ.f{AR.ASHTI{A :,,<;)L'S d::'iAL DE\ :-1 Ol'Ml.:Nl Al'T/ 196 II

No.. .rec. 2!~3f{4gSG)YIND.i4.--Iu exercise of powers conferred by Sub-

&cUm (3) of Section 1 of the Mah:JjJ~hl:a Industrial Development Act. 1!.!61.
(Mah. Tn l)( ;962). tit·.; Gcvcm.n 'n' o~ ;1I!:ih::f~S'htra hereby appoints 27th May
1988. to be the date from which Chapter VI of the'-snid Act shall take Clil.!Cl
in the area mentioned in the Schedule annexed hereto and declares the said
Area as industrial area under clause (g)o[ section 2 of the said Act.
The said Area is more clearly defined in red in the maps deposited in the
offices of the Chief Executive Officer, Mnharashtra : Industrial Development
Eorporation. Bombay 400 093~ and the Special Land Acquisition Officer.
Auraagabad, District Aurangabad; and is bounded by the areas as indicated
in tbe said .schcdule. e-

"
.
SCHI!DVLE
District
-- -' .,-~.-.-.--. -
Oat No.
Aurangabad,
.. _Area_---_
t~Juk;a .Atlrangatx'ld;: village
... ..... - ... "~ ---
Gat No.
WnIQdgaon.
Arca
Ares Ares
e! pt. 02·()
.... _-- -----
69 pt. 01·0
,J" -.-----.--.- -- - - - -_._.-
I .
B-owtdtUies. :
Orr the Nortli by'.-Part of.Gat Nos. 70. 71~ 16. 77.18.
CJr. the SOfith.~.~p~rt of Gal, N~s. 70. 11, 76. 17~78 ~nd 8I.
On {he East b. .~oundary of village Nakashtra wadi.
On tlu: lVestry. -Aurn~i$.d-Ahm.dnagar Road.
. 1 'i! •

District ~ranga.bad, taluka Aurangabad, village Patoda.:

--'-r-- -- --.-.- -'.. -_._._".
- ,.-.-.
Gat No. Area
Ares
16' pt.
- ....~------ _. ,' •.. _-,.-- ...__ .. ... - _-- ...• -._._ .. -"--."---'---
07'0

;J~s:
On lhe North by.-Part of Gat Nos. 18, 19. 20, 21 and 26.
On .he S~)u'h by.-Part of Gat No~. 18. 19. 20 and 22.
On the East by.~Bou(]dary of village Valadgnqn,
0,. the West bj.-Boundary village Valadgeon. of