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HOIST
ERECTIONBAY
POS-0141(N)
POS-0143(N)
POS-0141POS-0191
POS-0151
POS-0153
POS-0141(S)
POS-0143(O)
A'
A
B
C
D
E
F
HOIST
POS-AR106 POS-1172(S)
HOT/COLD OILPUMP
POS-1132 POS-1131 POS-1172
V-1600 V-20POS-1161(O) POS-1191 POS-1161(S) POS-1181
TETA-2167DIMER
2166(O)TETA-2108 DIMER
2166(S)
1234567891011121415
1234567891011121315
DRUM STORAGE AREA(EXISTING)12 m x 6 m
ENTR
Y PA
SSAG
E
SHEDFOR
DRUM STORAGE
ERECTIONBAY
POS
332
STEA
M E
JECT
OR
DRUM STORAGE AREA
LOCKER ROOM &TEA SERVING POINT
3 m x 6 m
WASH ROOM3 m x 3 m
TOILET3 m x 4 m
MCC ROOM9 m x 3 m
MEZZ. FLOOR
12
A
B
C
WATERCIRC.TANK
(AT 4 m ELE.)CONTROL&
PANEL ROOM
MCC ROOM(NEW)
MCC ROOM(NEW)
13
14
POS T-1133CARDANOL TANK
(TO BE RELOCATED)
SS TANK(TO BE RELOCATED)
G
H
G
H
13
Checked
Unauthorized disclosure to any third party or duplication is not permitted .This drawing is a property of Shroff And Associates (Engineers) Pvt. Ltd.
Title :
Rev Date
Project Name:
Drg. No.Scale
Plant:
Owner:
Description Name
Rev
Approved
Location:
Sheet
of
Project No:
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OPEN
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OPENING
OPENING
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ATUL LIMITED (Corporate SHE Dept.)
Division: Bulk Intermediate
Name of Product: Caustic soda lye
1. Lab Process details:
1.1
New Project – Lab Process Details
Date:
Brief process and flow diagram of process stage wise Salt & water is charged to prepare saturated brine solution, it is treated chemically with barium carbonate, sodium carbonate & NaOH in precipitation tank. It clarified by adding flocculent & suspended solids separated by filtration. Brine solution further purified in two steps of polishing filtration & ion exchange. Brine flows into anode chamber & weak caustic flows into cathode chamber. Chlorine is liberated at anode surface & hydrogen generated at cathode surface. Two phase mixture of NaOH & hydrogen gets separated at cathode header. 32% NaOH is further concentrated to 50% NaOH by evaporation. Depleted brine is dechlorinated. Chlorate destruction is done under influence of HCl. Chlorine is further treated with 98% sulfuric acid to get dry chlorine. Hydrogen is cooled & passed through filter for treatment.
1.2
Chemicals reactions with molecular weight stage wise
Brine Saturation NaCl
10% Barium carbonate solution Chemical Preparation
Clarification
Filtration
Sec. Brine Purification
Electrolysis
Catholyte system
Anolyte Dechlorination
Chlorate Destruction
Chlorine Treatment
Hydrogen Treatment
10% Sodium carbonate solution 32% NaOH solution
Flocculent
32% NaOH Hydrogen
Chlorine
32% HCl
98% H2SO4 78% H2SO4
Sodium Chloride
Mwt. 58.5
2NaCl(aq) + 2H2O(l) 2NaOH(aq) + Cl2(g) + H2(g)
Water Mwt. 18
Sodium Hydroxide Mwt. 40
Chlorine Mwt. 71
Hydrogen Mwt. 2
Caustic evaporation
32% CS Lye Dist. Water 50% CS Lye
Chlorine Chlorine
Sludge
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption Kg/kg of 100% NaOH
1 NaCl (100%) 1.5250 2 Barium carbonate (100%) 0.0157 3 Sodium Carbonate (100%) 0.0058 4 HCl (100%) 0.0180 5 NaOH(100%) 0.0150 6 NaHSO3 (100%) 0.0004 7 Flocculating agent 0.00004 8 Precoat alfa cellulose 0.00035 9 Water 3.3000
10 Sulfuric acid (100%) 0.0150
1.4
Sr. No.
List of co-product per kg Chemical name kg /kg
1 Chlorine 0.886
2 Hydrogen 0.0239
1.5
S.No.
Complete Mass balance per kg: Input kg Output kg
1 NaCl (100%) 1.5250 50% NaOH (100%) 1.000 2 Barium carbonate (100%) 0.0157 Chlorine 0.886 3 Sodium Carbonate (100%) 0.0058 Hydrogen 0.0239 4 HCl (100%) 0.0180 Solid waste 0.090 5 NaOH(100%) 0.0150 Liquid effluent 1.0862 6 NaHSO3 (100%) 0.0004 Water in 50% NaOH 1.000 7 Flocculating agent 0.00004 Distilled water 1.260 8 Precoat alfa cellulose 0.00035 Sulfuric acid (78%) 0.01923 9 Water 3.7700
10 Sulfuric acid (100%) 0.0150 Total 5.3653 Total 5.3653
1.6
Complete Molecular balance
2NaCl(aq) + 2H2O(l) 2NaOH(aq) + Cl2(g) + H2(g)
1.7 Sr. No.
Complete Water balance Input Quantity
kg Output Quantity
kg 1 Water 3.770 water 3.386
2. Gas Emission:
Gas emission stage wise per kg: 5mg/nm3 Cl2
Identification
3. Water discharges:
Raw water consumption details per kg Waste water quantity and quality generated i.e. pH, COD TDS acidity, alkalinity etc per kg Stream wise quality of the effluent (Analysis reports | experimental results) per kg Proposed treatment method developed if any: No
Quantity /kg of Product
COD PPM
BOD PPM
TDS PPM
Color
Liquid effluent 1.0862 250 - 125000 colorless
4. Waste generation:
Solid waste generated per kg: 0.090Kg/Kg Solid waste characteristics and its proposed treatment developed if any.
5. Details of Hazardous chemicals:
Hazardous chemicals used and method of handling & disposal. Normal precautions in handling chemicals are to be followed. 6. Other Consideration:
Recycle & Reuse options in process. Solvent recovery details stage wise per kg. Acetone used as solvent & it is recovered & reused in the process.
7. Any other relevant information:
You may want to share about the product\process
Date: Project In-Charge G.M R & D
SULFUR BLACK
POLYSULFIDE PREPARATION
32 % NaOH LYE 6937 KG SULFUR 2905 KG
PHENOLATION
32 % NaOH LYE 2984.3 KG 2:4 DNCB 2415 KG WATER 4100
REDUCTION/COUPLING
THIONATION
FILTRATION
MIXING
WATER WASH
DRYER
NH₃ GAS
H₂S GAS
ML + WATER WASH
OXIDATION
WATER SCRUBBER
ALKALI SCRUBBER
AIR
WATER
5 % AMMONIA
25 % NaOH
27 – 30 % Na₂S
SULFUR BLACK
SODA ASH
SODIUM SULFIDE
MULTIPLE EFFECT EVAPORATOR
CONDENSATECONC. Na₂S₂O₃
Na₂S₂O₃ CRYSTALSSODIUM CHLORIDE
ATUL LIMITED
Name of Product: Anethole (p-Propenylanisole)
Lab Process details:
New Project – Lab Process Details
i) Brief process and flow diagram of process stage wise-
Step 1: Friedel Crafts Acylation (F.C Reaction)
Brief Process: Charge Anisole & EDC in glass reactor. Under stirring cool the reaction mixture.
Charge Aluminum chloride in reaction mass by maintaining temperature. Charge Propionyl chloride
in 3-4h by maintaining temperature. Once addition over continue stirring at same temperature for 2h.
Reaction monitored on GC instrument. After that do the work up. Separate Aqueous and organic
layer. Do the recovery of solvent and fractional distillation of organic material.
(1) Anisole(2) Propionyl Chloride(3)AlCl3 anhyd.(4)EDC
(16) HCl gas evaluation
(6) Ice-Cold water (7) Organic 1:
INPUT(11) Aquous 2: *
(9) EDC (12) Organic 2: (10) Water
(15) Aqueous 3:(14) 13% NaCl (16) Organic 3:
(16) Organic 3: (18) Aqueous 4:(17) 10% NaHCO3 (19) Organic 4:
(20) Recovered EDC(19) Organic 4: (21) ForeCut (tops)
(22) Intercut (tops)(23) Maincut 1(24) Maincut 2(25) % EDC Rec Loss(26) Residue *
(13) Organic 1+ Organic 2
FLOW DIAGRAM 4-MPP (STEP - I)
FC REACTION TIMECYCLE : 6-7 hrs
Stirring for 0.5 hrs
(27) 4-Methoxy propio-phenone
DISTILLATION (4-MPP) TIMECYCLE : 25 hr
Quenching timecycle: by mainting temp. 5-20 deg C: 3-4 hrs
(5) Reaction Mass
(8) Aqueous 1
Washing of organic mass with pH= 7-7.5
Washing of organic mass
Organic Mass for rec. of solvent & Fr. Distillation
Step 2: Hydrogenation
Brief Process: Charge 4-methoxy propiophenone, methanol, tri ethyl amine & catalyst, purge nitrogen
1-2Kg/cm2 in autoclave. After complete H2 consumption takes the sample & checks the conversion of
reaction mass by GC. Cool the mass & release the pressure from autoclave. Filter the reaction mass &
recover the catalyst which is to be recycled in next batch. After 5 times recycle spent catalyst for sell
as by-product/send for regeneration.
(1) Distilled 4-MPP(2) Raney Ni(3) Triethyl amine(4) MethanolHydrogen gas
Filter (7) Filtrate 4-MPP alcohol(8) Rec. R-Ni
(7) 4-MPP alcohol
Flow diagram Hydrogenation 4-MPP alcohol (Step-2)
Autoclave(5) Flush with N2 two times then
H2 two times
.
Step 3: Dehydration
Brief Process: Charge paraffin & potassium hydrogen sulphate in R.B flask. Charge 1-(4-
Methoxy phenyl) propyl-1-ol in RBF drop by drop through addition funnel. Check GC % Area of
crude Anethole for complete conversion of 4-MPP alcohol to cis & trans-Anethole. Workup done
separating crude Anethole and water. Take crude Anethole for fractional distillation.
Note: The Apparatus must be completely clean and dry.
(1) 4-MPP alcohol (5) Crude Anethol(2) KHSO4 (6) Water(3) Paraffin(4) High Vacuum
(7) Residue
Dehydration Assembly
Flow diagram Dehydration : crude Anethole (step 3)
Step 4: Fractional distillation of crude Anethole
Fractional distillation using 3 meter long packed (ss net) column with reflux divider.
(1) Crude Anethol (3) Forecut (tops)(2) Vacuum 1-2 mbar (4) Intercut (tops)
(5) Maincut (t-Anethole)(6) H.B *
(7) Residue *
FLOW DIAGRAM FOR ANETHOLE (STEP - 4)
Distillation Assembly
ii) Chemicals reactions with molecular weight stage wise Step 1: Acylation
O
H3COH3CO Cl
OAlCl3
EDC92.5 164
Anisole Pr-chloride 4-MPP108MW-
(133)
(99)
Step 2: Hydrogenation
O
H3CO
OH
H3CO
H2
164
4-MPP
Methanol (32); R-Ni
1664-MPP alcohol
MW-
OH
H3CO H3CO H3CO
-H2O
t-Anethole cis-Anethole
Step 3: Dehydraation
166
4-MPP alcohol
KHSO4148 148MW- (136)
Step 4: Fraction distillation of Anethole isomer
H3CO H3CO
t-Anethole cis-Anethole148 148MW-
H3CO
t-Anethole148
iii) List of raw materials along with quantity per KG
1 Anisole 108 1.122 Propionyl chloride 92.5 1.0663 Aluminium Chloride (AlCl3) 133.5 1.374 Ethylene dichloride (EDC) 99.8 0.465 Sodium chloride 58.5 0.13
6Sodium bicarbonate (NaHCO3)
84 0.13
7 Ra-Ni- (Monarch ltd) 0.018 Methanol 32 0.1639 H2 gas 2 0.018910 N2 Gas 28 0.00211 Triethyl amine 101.5 0.001712 Paraffin Oil- Merck 0.07
13Potassium hydrogen sulphate (KHSO4)
120 0.04
Sr. No. Raw Materials MW (g)
Raw material consumption data for 1kg Anethole
Qty. req. kg/kg of product
.
iv) Complete Mass balance per KG
Material req. kg/kg Anethole Sr.No. Raw Materials Input Qty kg Sr.No Materials Output Qty kg
1 Anisole 1.04 1 Aqueous 2 6.790833 2 Propionyl Chloride 1.003 2 Aqueous 3 1.85956 3 AlCl3 1.34 3 Aqueous 4 1.299667 4 EDC 1.992 4 Recovered EDC 2.93455 5 Ice cold water 3.097 5 Tops step 1 0.075 6 EDC 1.097 6 Residue step 1 0.069922 7 Water 2.103 7 Rec. Methanol 1.125 8 13% NaCl 1.667 8 Rec. R-Ni 8030 0.034722 9 10% NaHCO3 0.764 9 Water 0.13944 10 Methanol 1.25 10 Residue 0.199556 11 R-Ni 8030 0.030889 11 Anethole 1 12 Tri ethyl amine 0.003089 Total output 15.52825 13 KHSO4 0.0125
14 Paraffin oil 0.054792
Mass balance: 98.73 %
Total input 15.728
v) Complete Molecular balance
Step 1: Acylation
O
H3COH3CO Cl
OAlCl3
EDC
92.5 164
Anisole Pr-chloride 4-MPP
108MW-
(133)(99)
HCl
36.5
Step 2: Hydrogenation
O
H3CO
OH
H3COH2
164
4-MPP
Methanol; R-Ni
166
4-MPP alcohol
M.W- 2
OH
H3CO H3CO-H2O
Crude Anethole
Step 3: Dehydraation
166
4-MPP alcohol
KHSO4
148MW-
(136)H2O
18Water
Step 4: Fraction distillation of Anethole isomer
H3CO H3CO
Crude - Anetholecis-Anethole148MW-
H3CO
t-Anethole148
&
ATUL LIMITED
Name of Product: Avobenzone
1. Lab Process details:
New Project – Lab Process Details
Brief process and flow diagram of process stage wise Stage-1: Process for 4-t-butylbenzoicacid to Ester
Charge 4-t-butylbenzoicacid and add Methanol and start stirring. Slowly add H2SO4 and heat the mass to reflux. Stir the mass at reflux till the desire conversion. Recover methanol and allow to separate the layers. The bottom aq layer is to be recycled in the next batch. Wash the organic layer with sodium bicarbonate solution to recover & recycle the unreacted acid. Purify the product by vacuum distillation.
Stage-2: Process for Avobenzone
Charge toluene and heat the solution to reflux temp. Distill out some toluene to remove moisture. Cool the mass to 60oC. Add sodium methoxide and mixture of methyl 4-tert-butylbenzoate, 4-methoxyacetophenone and toluene. Stir the reaction mass at same temp and monitor on GC. Cool the mass, acidify with dilute acid and separate the layers. Wash the organic phase with water. Collect aqueous layer & washings for p-tert-butylbenzoic acid recovery. Recover toluene from organic layer under vacuum. Add methanol and stir the mass at reflux temp. Gradually cool the mass and stir for 15 min. Filter the slurry under vacuum and dry the product in vacuum oven.
Flow diagram
Stage-1:
Reflux
Recovered methanol
4-t-butylbenzoicacid
Distillation
Residue
Product
Organic layer M.L
Recovered acid
Methanol 98% H 2 SO 4
Methanol recovery
5% Na 2 CO 3 wash H 2 SO 4
Organic layer Spent acid layer
Aq layer
To be recycled
To be recycled
To ETP
To be incinerated
Toluene
Stage-2:
4-MAP + Ester+Toluene
Distillation Toluene
Reaction Distillation Toluene+methanol
Recovered Toluene
1 st crystallisation
2 nd crystallization
Workup 10% H 2 SO 4
Organic layer Water wash
Recovered acid
Aq. layer
Product
H 2 SO 4
M.L
M.L
Residue Methanol recovery
Recovered methanol
Aq. layer
Mixing
Toluene recovery
Aq. layer
Cooling
Methanol
Methanol
Drying
To be recycled
To be recycled
To ETP
To be incinerated
To be recycled
To be recycled
NaOMe
Chemicals reactions with molecular weight stage wise
COOCH3
C12H16O2192.3
methyl 4-t-butylbenzoate
COOH
C11H14O2 178.2
4-t-butylbenzoicacid
+ CH3OH
Conc.H2SO4
CH4O32
Methanol
-H2O
Stage-1
COCH3
OCH3
+
COOCH3
CH3ONa
C9H10O2150.2
4-MAP
C12H16O2192.3
methyl 4-t-butylbenzoate
H3CO
O O
C20H22O3310.39
Avobenzone
Stage-2
List of raw materials along with quantity per KG
Complete Mass balance per KG
Input
Stage-1
g Output g
4-t-butylbenzoicacid 250 Aq. layer (spent acid) 53
Methanol 225.3 Recovered acid 3.2
98% H2SO4 30.6 Methyl-4-t-butylbenzoate 247
5% Na2CO3 100 Recovered methanol 158
Water 50 Aq.layer 142
Residue 8
Methanol loss 21
Water loss on drying 22
655.9 Total 654.2 Mass balance = 99.74%
Sr. No. Raw Materials Molecular weight
(g) Quantities
Practical kg/kg of Product 1 4-Methoxyacetophenone 150.2 0.730 2 4-tert-butylbenzoicacid 178.2 0.753 3 Sodium Methoxide 54 0.322 4 Toluene 92 0.454 5 Methanol 32 1.300 6 98% sulfuric acid 98 0.447 7 Sodium bicarbonate 84 0.019
Input
Stage-2
g Output g
4-methoxyacetophenone 112.5 Aq. layer 1157
Methyl-4-t-butylbenzoate 151.2 Recovered acid 35
Sodium methoxide 49.6 Recovered toluene 808
Toluene 850 Recovered methanol 675
Methanol 750 Avobenzone 154
10% H2SO4 504 Residue 52
Water 600 Methanol loss 75
Toluene loss 42
Water loss on drying 10
3017.3 Total 3008
Mass balance = 99.67%
ATUL LIMITED
Name of Product: Avobenzone
1. Lab Process details:
New Project – Lab Process Details
Brief process and flow diagram of process stage wise Stage-1: Process for 4-t-butylbenzoicacid to Ester
Charge 4-t-butylbenzoicacid and add Methanol and start stirring. Slowly add H2SO4 and heat the mass to reflux. Stir the mass at reflux till the desire conversion. Recover methanol and allow to separate the layers. The bottom aq layer is to be recycled in the next batch. Wash the organic layer with sodium bicarbonate solution to recover & recycle the unreacted acid. Purify the product by vacuum distillation.
Stage-2: Process for Avobenzone
Charge toluene and heat the solution to reflux temp. Distill out some toluene to remove moisture. Cool the mass to 60oC. Add sodium methoxide and mixture of methyl 4-tert-butylbenzoate, 4-methoxyacetophenone and toluene. Stir the reaction mass at same temp and monitor on GC. Cool the mass, acidify with dilute acid and separate the layers. Wash the organic phase with water. Collect aqueous layer & washings for p-tert-butylbenzoic acid recovery. Recover toluene from organic layer under vacuum. Add methanol and stir the mass at reflux temp. Gradually cool the mass and stir for 15 min. Filter the slurry under vacuum and dry the product in vacuum oven.
Flow diagram
Stage-1:
Reflux
Recovered methanol
4-t-butylbenzoicacid
Distillation
Residue
Product
Organic layer M.L
Recovered acid
Methanol 98% H 2 SO 4
Methanol recovery
5% Na 2 CO 3 wash H 2 SO 4
Organic layer Spent acid layer
Aq layer
To be recycled
To be recycled
To ETP
To be incinerated
Toluene
Stage-2:
4-MAP + Ester+Toluene
Distillation Toluene
Reaction Distillation Toluene+methanol
Recovered Toluene
1 st crystallisation
2 nd crystallization
Workup 10% H 2 SO 4
Organic layer Water wash
Recovered acid
Aq. layer
Product
H 2 SO 4
M.L
M.L
Residue Methanol recovery
Recovered methanol
Aq. layer
Mixing
Toluene recovery
Aq. layer
Cooling
Methanol
Methanol
Drying
To be recycled
To be recycled
To ETP
To be incinerated
To be recycled
To be recycled
NaOMe
Chemicals reactions with molecular weight stage wise
COOCH3
C12H16O2192.3
methyl 4-t-butylbenzoate
COOH
C11H14O2 178.2
4-t-butylbenzoicacid
+ CH3OH
Conc.H2SO4
CH4O32
Methanol
-H2O
Stage-1
COCH3
OCH3
+
COOCH3
CH3ONa
C9H10O2150.2
4-MAP
C12H16O2192.3
methyl 4-t-butylbenzoate
H3CO
O O
C20H22O3310.39
Avobenzone
Stage-2
List of raw materials along with quantity per KG
Complete Mass balance per KG
Input
Stage-1
g Output g
4-t-butylbenzoicacid 250 Aq. layer (spent acid) 53
Methanol 225.3 Recovered acid 3.2
98% H2SO4 30.6 Methyl-4-t-butylbenzoate 247
5% Na2CO3 100 Recovered methanol 158
Water 50 Aq.layer 142
Residue 8
Methanol loss 21
Water loss on drying 22
655.9 Total 654.2 Mass balance = 99.74%
Sr. No. Raw Materials Molecular weight
(g) Quantities
Practical kg/kg of Product 1 4-Methoxyacetophenone 150.2 0.730 2 4-tert-butylbenzoicacid 178.2 0.753 3 Sodium Methoxide 54 0.322 4 Toluene 92 0.454 5 Methanol 32 1.300 6 98% sulfuric acid 98 0.447 7 Sodium bicarbonate 84 0.019
Input
Stage-2
g Output g
4-methoxyacetophenone 112.5 Aq. layer 1157
Methyl-4-t-butylbenzoate 151.2 Recovered acid 35
Sodium methoxide 49.6 Recovered toluene 808
Toluene 850 Recovered methanol 675
Methanol 750 Avobenzone 154
10% H2SO4 504 Residue 52
Water 600 Methanol loss 75
Toluene loss 42
Water loss on drying 10
3017.3 Total 3008
Mass balance = 99.67%
ATUL LIMITED
Name of Product : OCTOCRYLENE
1. Lab Process details :
New Project – Lab Process Details
Brief process and flow diagram of process stage wise: In 1st step ester formed by the condensation of a Cyanoacetic acid with 2-ethylhexanol in presence of
PTSA as catalyst, which is worked up & fractionally distilled to get pure 2-Ehtyhexyl cyanoacetate (2-EHCA). In 2nd step 2-Ethylhexyl cyanoacetate (2-EHCA), Benzophenone (BP), ammonium acetate, acetic acid and Cyclohexane are mixed. The mixture is heated under stirring to reflux temperature and water is distilled out azeotropically. The reaction mass is cooled and worked up. Crude product is fractionally distilled to get pure Octacrylene.
2-ETHYLHEXYL-2-CYANOACETATE [2-EHCA] FLOW DIAGRAM OF STEP- I : OF OCTOCRYLENE
Fractional distillation
NITROGEN GAS
FLOW DIAGRAM OF STEP- II : OF OCTOCRYLENE
[OCR]
in 20 hrs.
Fractional distillation
Chemicals reactions with molecular weight stage wise:
R M for 1 kg OCTOCRYLENE
List of raw materials along with quantity per KG:
Sr. No. Raw Materials
Lab. Expt. Qty.
in (g)
Qty. for1 kg in (g)
Mol. wt Moles
1 Cyanoacetic acid 85 395 85 4.647 2 2-Ethylhexanol(consumed) 120 558 130.2 4.286 3 p-Toluene sulfonic acid 2.4 11 190 0.058 4 2-EHCA 176.3 820 197.3 4.156 5 Benzophenone(consumed) 120.2 559 182.2 3.068 6 Cyclohexane(consumed)in lit. 60 276 84.16 3.279 7 Glacial acetic acid 148 690 60.05 11.50 8 Ammonium acetate 43 200 77.08 2.595 9 Ground salt 15 70 58.5 11.97
10 Methanol (consumed) 77 360 32 11.25 11 Darco 16 75 - - 12 Hyflosupercell 4 19 - - 13 Anhydrous Glauber’s salt 4 19 - -
C C
C
C
O
N
O CH3
H3C
2-Propenoic acid, 2-cyano-3,3-diphenyl-, 2-ethylhexyl ester or Octocrylene CAS no.: 6197-30-4 M.Wt.:361
C=O
Ammonium acetate,Acetic acid & Cyclohexane , Heat to 94 - 105°C, distill mix. of water,
BenzophenoneCas no.:119-61-9M.wt. 182
HOC C N
O
Cyanoacetic acidCAS no.: 372-09-8M.wt.: 85
+
H3C OH
CH3
2-Ethylhexane-1-olCAS no.: 104-76-7M.Wt.: 130
H3C SO3H
Reflux for 3.5 hr., distill water,. at 104 - 125°C
2-Ethylhexyl -2-cyanoacetateCAS no.: 13361-34-7M.Wt.: 197
+
O
O
N
MATERIAL BALANCE FOR OCTOCRYLENE
Complete Mass balance per KG: (% Mass balance 99.856%)
Sr. no. INPUT Quantity
in (kg) OUTPUT Quantity in (kg)
1 Cyanoacetic acid 0.395 Middle cut of 2 - EHCA dist. 0.008
2 2 - Ethyl hexanol 0.678 Recovered Ethyl hexanol 0.125 3 p - Toluenesulfonic acid 0.013 Recoveed Cyclohexane 0.65 4 Water 3.098 Recovered Benzophenone 0.656 5 Benzophenone 1.218 Recovered 2 - EHCA 0.222 6 Acetic acid 0.853 Recovered MeOH 2.10 7 Ammonium acetate 0.247 Trap 0.11 8 Cyclohexane 0.685 Distillate 0.470 9 Methanol 2.340 Water wash 3.585
10 NaCl 0.085 Octocrylene 1.000 11 Darco 0.086 Darco sludge 0.149 12 Hyflowsupper cell 0.023 Organic solvent loss 0.500 13 Anhyd. Na2SO4 0.023 Handling loss 0.100 14
Residue 0.055
9.744
9.73
Molar calculation (2-EHCA)
Complete Molecular balance :
Sr. No. Raw Material Weight
in g M.wt. Moles Molar Ratio
1 2-Ethylhexanol 150 130.23 1.151808 1 2 Cyano acetic acid 85 85 1 0.8682 3 p-Toluene sulfonic acid.H2O 2.4 190 0.012632 0.010967 4 2-Ethylhexyl-2-cyanoacetate 176.3 197.3 0.893563 0.775791
Molar calculation (OCTOCRYLENE) Sr. No. Raw Material Weight
in g M.wt. Moles Molar Ratio
1 2-Ethylhexyl-2-cyanoacetate 177.8 197.3 0.901166 1 2 Benzophenone 213.3 182.2 1.170692 1.299086 3 Cyclohexane 117 84.16 1.390209 1.542679 4 Acetic acid (Glacial) 149.4 60.05 2.487927 2.760787 5 Ammonium acetate 43.2 77.08 0.560457 0.621924 6 Methanol 385 32 12.0312 13.3507 7 Darco 16 - - - 8 Hyflosuper cell 4 - - - 9 Anhydrous Na2SO4 4 142 - -
10 Salt 15 58.5 - -
Confidential & Restricted Circulation Page 1 of 5
ATUL LTD
Name of Product: Octyl Methoxy Cinnamate (OMC)
Lab Process details:
New Project – Lab Process Details
i) Brief process and flow diagram of process stage wise-
Step 1: Esterification
Brief Process: In 1st step ester formed by the condensation of P- Anisaldehyde (PAA) with
Ethyl acetate in presence of Sodium Methoxide powder as a catalyst, which is worked up and get
the mixture of 4-Methoxycinnamic acid ethylester (4-EMC) and 4-Methoxycinnamic acid
methylester (4-MMC).
Step 2: trans-esterification
Brief Process: In 2nd step, 4-Methoxycinnamic acid ethylester (4-EMC) and 4-Methoxycinnamic
acid methylester (4-MMC) react with 2-Ethyl hexanol in presence of liquid Sodium Methoxide.
The mixture heated under stirring at ambient temperature and vacuum to remove/distilled out
mixture of solvent. The reaction mass is cooled and worked up. Crude product fractionally
distilled to get pure Octyl Methoxy Cinnamate (OMC)
Confidential & Restricted Circulation Page 2 of 5
FLOW DIAGRAM- OMC
Confidential & Restricted Circulation Page 3 of 5
ii) Chemical Reactions with Molecular Weight Stage wise:
p-AnisaldehydeCAS 123-11-5C8H8O2MW 136
+
Ethyl acetateCAS 141-78-6C4H8O2MW 88
NaOMe+
4-Methoxycinnamic acidethylesterCAS no.: 1929-30-2MF : C12H14O3M.Wt.: 206
4-Methoxycinnamic acidmethylesterCAS no.: 832-01-9MF : C11H12O3M.Wt.: 192
OCH3
CHO
CH3COOC2H5
OC2H5
O
OCH3
OCH3
O
OCH3
Step – 1st
+
4-Methoxycinnamicacid ethylesterCAS no.: 1929-30-2MF : C12H14O3M.Wt.: 206
4-Methoxycinnamicacid methylesterCAS no.: 832-01-9MF : C11H12O3M.Wt.: 192
OH
-C2H5OH -CH3OH
2-Ethyl hexanolCAS 104-76-7C8H18OMW 130
2-Ethylhexyl-4-methoxycinnamateOctylmethoxy cinnamate (OMC)CAS no.: 5466-77-3MF : C18H26O3M.Wt.: 290
OC2H5
O
OCH3
OCH3
O
OCH3
NaOMe
OCH3
O
O
+
Step – 2nd
Confidential & Restricted Circulation Page 4 of 5
iii) List of Raw Materials along with quantity per Kg:
RAW MATERIALS CONSUMPTION FOR 1kg OMC
Sr./No. Raw Material Mol. Wt. Quantity (Kg)
1 P-Anisaldehyde 136.15 0.5913 2 Ethyl acetate 88.11 0.4391 3 Sodium Methoxide (98%) 54.02 0.2982 4 Phosphoric acid (85%) 98.00 0.0147 5 2-Ethylhexanol 130.23 0.6043 6 Sodium methoxide (30%) 54.02 0.0326 7 Formic acid 46.03 0.0097 8 Divyol 460 - 0.0815 9 Darco - 0.014
10 Hyflo supercell - 0.0059
iv) Mass Balance data for 1Kg OMC
Sr. no. INPUT Quantity
in (g) OUTPUT Quantity in (g)
1 p-Anisaldehyde 593 Recovered Ethyl acetate 1741 2 Ethyl acetate 2180 Recovered Ethyl hexanol 195 3 Ethyl hexanol 675 Ethanol/Methanol 270 4 Sodium methoxide powder 302 Aqueous for recovery 1620 5 Sodium methoxide solution 114 Water to be recycle 2000 6 Phosphoric acid 22.5 OMC 1000 7 Formic acid 6.5 OMC to be recycle (100%) 50 8 Divyol 460 108 Residue 152 9 Fresh Water 1620 Divyol 460 108
10 ml of OMC recycled 2000 Fraction-2 to be recycle 54 11 Fraction-2 54 Darco sludge 25 12 Darco 13 Distillate of MeOH/EtOH etc 320 13 Hyflo supercell 5.5 W/C of MMC/EMC recovered 65
7693.5 7600 Mass Balance – 99.00%
Confidential & Restricted Circulation Page 5 of 5
v) Complete Molecular Balance:
Sr.No. Raw Material M.Wt. Moles
1 P-Anisaldehyde 136.15 4.000
2 Ethyl acetate 88.11 22.87
3 Sodium Methoxide powder 54.02 5.083
4 Phosphoric acid 98.00 0.182
5 2 – Ethylhexanol 130.23 4.808
6 Sodium methoxide 54.02 0.583
7 Formic acid 46.03 0.128
8 Divyol 460 - -
9 Darco - -
ATUL LTD
New Project – Lab Process Details
Name of Product: p-Anisylpropanal
(1) Brief process and flow diagram of process stage wise
Step -1: Condensation of p-Anisaldehyde (PAA) & Propanaldehyde to form p-Anisylpropenal
(Step-1):
p-Anisaldehyde is condensed with propanaldehyde in presence of sodium hydroxide as a base and
Methanol as a solvent. Conversion is checked by GC analysis. reaction mass is neutralized with Sulfuric
acid followed by methanol recovery and extraction in toluene and organic layer is washed with water and
sodium bicarbonate. Toluene is recovered by distillation to generate crude. Finally product is obtained by
fractional distillation.
Step -2: Hydrogenation of p-Anisyl propenal (Step-1) to form p-Anisylpropanal (Step-2)
p-Anisyl propenal is hydrogenated with hydrogen gas in Autoclave in presence of 5% Pd/C as
catalyst and Sodium carbonate. Methanol is used as solvent. After hydrogenation, catalyst is recovered by
filtration followed by Methanol recovery. Finally the product is purified by fraction distillation. Note: The
autoclave must be completely clean and dry.
Process flow diagram of Step-1:
Process flow diagram of Step-2:
p-Anisaldehyde (PAA)Propionaldehyde Rec. Methanol Recycle
Methanol 35% NaOH solutionH2SO4
Water (1st wash) Toluene 5% NaHCO3 soln (2nd) Aq-3* (Recycle)Water (3rd wash)
Rec. Toluene Recycle
Rec.PAA Recycle
Divyol Oil (460) Intercut Recycle B.H.T.
Highers Recycle
Residue Co-product
Fractional distillation
p-Anisylpropenal
Washing and separation
Aq-1 & 2 (For effluent)
Toluene recovery
Reaction and Methanol recovery
p-Anisylpropenal (Step-1)Methanol Sodium CarboanteWater5% Palladium Carbon
Methanol Rec. Catalyst Recycle
Rec. Methanol Recycle
Forecut (Recycle)B.H.T.
Residue Co-productFractional distillation
p-Anisylpropanal
Hydrogen gas
Hydrogenation
Methanol recovery
Catalyst filtration
(2) Chemicals reactions with molecular weight stage wise:
Step-1: Condensation
H3CO
CHO
p-Anisaldehyde (PAA)
Mol.Wt=136 g/mol
+ CH3
O
Propanaldehyde
Mol.Wt=58 g/mol
NaOH (40 g/mol) Methanol (32 g/mol)
H3COCH3
O
p-Anisylpropenal (Step-1)
Mol.Wt=176 g/mol
+ H2O
Step-2: Hydrogenation
H3COCH3
O
p-Anisylpropanal (Step-2)
Mol.Wt=178 g/mol
H3COCH3
O
p-Anisylpropenal (Step-1)
Mol.Wt=176 g/mol
5% Pd/CMeOH (32 g/mol)
H2 gas
(3) List of raw materials along with quantity per KG
Raw materials consumption data for 1kg p-Anisyl propanal
Sr. No. Raw Materials Molecular
Weight (g) Quantities
kg/1kg of Product 1 p-Anisaldehyde* 136 1.0143 2 Propanaldehyde 58 0.5102 3 Sodium hydroxide 40 0.0154 4 Sodium bicarbonate 84 0.0220 5 Sodium carbonate 106 0.0224 6 Sulfuric acid 98 0.0132 7 Methanol* 32 0.2890 8 Toluene* 92 0.0788 9 5% Pd/C (5T 756) Dry Basis** 0.0002
10 Hydrogen gas 2 0.0159 11 Butylated Hydroxy Toluene 220 0.0045 12 Divyol Oil (460) 0.0220 13 Nitrogen gas 14 0.004
* All the quantity based on consumed Raw materials. **Actual consumption (1+5 recycle)
(4) Complete Mass balance per KG
Input Output Remarks
Sr. No. Charged Qty (Kg) Sr. No. Obtained Qty
(Kg) 1 p-Anisic aldehyde 1.79 1 Aq-1 0.495 2 Propanaldehyde 0.51 2 Aq-2 0.497 3 Sodium hydroxide 0.0154 3 Aq-3 0.501 Recycle in next batch 4 Methanol 4.62 4 Rec. PAA 0.78 Recycle in next batch 5 Sulfuric acid 0.0132 5 Rec. Methanol 4.6 Recycle in next batch 6 sodium bicarbonate 0.022 6 Recovered Toluene 1.49 Recycle in next batch 7 Sodium carbonate 0.0224 7 Rec. Pd/C 0.0122 Recycle in next batch 8 Toluene 1.5 8 Residue (Step-1) 0.214 Sold as Co-product 9 5% Palladium Carbon 0.0143 9 Residue (Step-2) 0.08 Sold as Co-product 10 Water 1.33 10 Canthoxal 1 11 Divyol Oil 0.022 11 12 BHT 0.0035 9.8628 9.6692 Mass balance 98.03707
(5) Complete Molecular balance
H3CO
CHO
p-Anisaldehyde (PAA)Mol.Wt=136 g/mol
+ CH3
O
PropanaldehydeMol.Wt=58 g/mol
NaOH (40 g/mol) Methanol (32 g/mol)
H3COCH3
O
p-Anisylpropenal (Step-1)Mol.Wt=176 g/mol
+ H2O
WaterMol.Wt=18 g/mol
Step-1: Condensation:
H3COCH3
O
p-Anisylpropanal (Step-2)
Mol.Wt=178 g/mol
H3COCH3
O
p-Anisylpropenal (Step-1)
Mol.Wt=176 g/mol
5% Pd/CMeOH (32 g/mol)
H2 (2 g/mol)
Step-2: Hydrogenation:
ATUL LTD
Name of Product: Raspberry Ketone
Lab Process details:-
New Project – Lab Process Details
1. Step-1 Oxidation and condensation :
Charge methanol, p-cresol, Cobalt acetate, cupric oxide, and sodium hydroxide in autoclave. Purge Oxygen
gas and complete the reaction. Filter the reaction mass followed by methanol recovery. Take the material
for condensation with acetone. Complete the reaction; the reaction mass take for neutralization with
Hydrochloric acid followed by filtration and water wash.
2. Step-2 Hydrogenation
Charge 4-Hydroxybenzyledene acetone, Ra-Ni, tri ethylamine & methanol in autoclave & start stirring.
Purge hydrogen gas and complete the reaction followed by filtration and methanol recovery. Crude
product is taken for flash vacuum distillation with paraffin oil followed by crystallization with methanol
and obtained the final product Raspberry ketone.
p-CresolMethanol
Sodium HydroxideCobalt acetateCopper oxide
Oxygen
Water Catalyst Methanol Recycle
Methanol Rec.Recycle
AcetoneWater
Hydrochloric acid
Water Filterate
Ra-NiTEA
MethanolHydrogen Ra-Ni
Recycle
Methanol Recycle
Crude RBK
Crude RB Rapid mainParaffin oil Residue*
Paraffin oil
Rapid Main Crop-lMethanol Crop-ll
Crop-IIIMethaol rec.
Condensation
Process flow digram of Raspberry Ketone
Oxidation
Filteration
Filterate
Reaction mass
Crystall ization
Neutralization
Hydroxy benzylidene acetone
Hydrogenation
Filteration
Metanol Recovery
Disti l lation
Chemicals reactions with molecular weight stage wise Step-1 Oxidation and condensation:
Step-2 Hydrogenation:
CHO
ONa.2H2O
CH3CH2OCH3(58)
CH=CHCOCH3
OH
p-Hydroxybanzaldehyde1-(4-hydroxyphenyl)-3-butanone
180 162
C7H9O4Na C10H10O2
-H2O(18)
CH3
OH
108
C7H8O
p-Cresol
Co(Ac)2(249)CuO(79)
O2
(40
(32)
CH=CHCOCH3
OH
CH2CH2COCH3
OH
Ra-NiH2
1-(4-hydroxyphenyl)-3-butanone Raspberry ketone162 164
C10H10O2C10H12O2
i) List of raw materials along with quantity per KG
p-cresol to Raspberry ketone
RM Consumption /Kg
sr. no. Raw materials Mw Ratio Kg/kg
1 p-cresol 108 1.3
2 NaOH (flaks) 40 1.68
3 Methanol 32 .03
4 Cobalt acetate 249 .02
5 Copper oxide 79 0.0048
6 oxygen 32 0.5
7 Acetone 58 1.05
8 HCl 36.5 2.75
9 Ra-Ni (1961) - 0.013
10 Hydrogen 2 0.03
11 water 18 4.5 12 Triethyl amine 101.19 0.0158
13 Divyol oil - .05
ii) Complete Mass balance per KG
Material req. kg/kg Raspberry Ketone
Sr.No. Raw Materials Input Qty kg Sr.No Materials Output Qty kg
1 p-cresol 1.3 1 Catalyst 0.48 2 NaOH (flaks) 1.68 2 Methanol 7.97 3 Methanol 8.08 3 Filtrate 13.43 4 Cobalt acetate 0.02 4 Ra-Ni 0.02 5 Copper oxide 0.0048 5 By-product 0.17 6 Oxygen 0.5 6 RBK Crop-I 0.42 7 Acetone 1.2 7 RBK Crop-II 0.384 8 30%HCl 2.75 8 RBK Crop-III 0.202
9 Ra-Ni (1961) 0.013 9 Recover acetone + water 0.7
10 Hydrogen 0.03 10 Divyol oil 0.05 11 Water 9
12 Triethyl amine 0.0158 Total output 23.83 13 Divyol oil 0.05
Total input 24.64 % Mass balance = 96.74
iii) Complete Molecular balance
Step-1 Oxidation and condensation:
Step-2 Hydrogeantion
CH3COCH3
CH=CHCOCH3
OH
1-(4-hydroxyphenyl)-3-butanone162
C10H10O2
CH3
OH
108
C7H8O
p-Cresol
O2
(32)
+ +
(58)
+ 2H2O
(18)
Oxygen Acetone Water
CH=CHCOCH3
OH
CH2CH2COCH3
OH
Ra-NiH2
1-(4-hydroxyphenyl)-3-butanoneRaspberry ketone162
164
C10H10O2C10H12O2
+
Hydrogen(2)
ATUL LIMITED
Name of Product: 1,3-Cyclohexanedione (1,3-CHD)
1. Lab Process details:
1.1
New Project – Lab Process Details
Brief process and flow diagram of process stage wise 1,3-CHD is manufactured by catalytic hydrogenation of Resorcinol in the presence of caustic soda in aqueous medium. Hydrogenated mass is acidified using Hydrochloric acid to get out 1,3-CHD.
Hydrogenation Catalyst
Resorcinol Hydrogen
Work-up
Filtration
1,3 CHD Drying
Filtration Catalyst
ML
Water Caustic soda flakes
HCl
1.2
1.3
Chemicals reactions with molecular weight stage wise
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption /kg
1 Resorcinol 1.056 2 Caustic soda flakes 0.384 3 Hydrogen 0.021 4 Catalyst 0.0093 5 HCl (36%) 1.056 6 Water 1.320
1.5
S.No.
Complete Mass balance per kg: Input
Input kg Output kg 1 Resorcinol 1.056 1,3-Cyclohexanedione 1.000 2 Caustic soda flakes 0.384 Mother Liquor 2.837 3 Hydrogen 0.021 Catalyst 0.0093 4 Catalyst 0.0093 5 HCl (36%) 1.056 6 Water 1.320 Total 3.846 Total 3.846
1.6
C6H6O2 + H2 + NaOH + HCl C6H8O2 + H2O + NaCl
Complete Molecular balance
ATUL LIMITED
Name of Product: Anisole
1. Lab Process details:
1.1
New Project – Lab Process Details
Brief process and flow diagram of process stage wise Anisole is manufactured by methylation of Phenol in the presence of caustic soda with Dimethyl sulfate. Crude Anisole is further purified by vacuum distillation.
1.2
Chemicals reactions with molecular weight stage wise
Methylation Reaction Phenol
Di-methyl Sulfate
Water CS Lye
Work-up Aq. Layer
Distillation Anisole
Residue
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption /kg
1 Phenol 0.91 2 Di-methyl Sulfate 0.83 3 CS Lye (48%) 0.98 4 Water 1.31
1.5
S.No.
Complete Mass balance per kg: Input
Input kg Output kg 1 Phenol 0.907 Anisole 1.000
Di-methyl Sulfate 0.834 Aq. Layer 2.993 3 CS Lye (48%) 0.979 Residue 0.036 4 Water 1.315 Distillation Loss 0.006 Total 4.034 Total 4.034
1.6
C6H6O +NaOH + ½ C2H6SO4 C7H8O + H2O+½ Na2SO4
Complete Molecular balance
CHEMICAL REACTION OF EPOXY RESIN (BLR)
HO C OH
CH3
CH3
2 CH2 CH CH2
O Cl
+ 2NaOH+
+ 2NaCl + 2H2O
Bisphenol A288
EPICHLOROHYDRINE
92.5 40
RESIN
340
BPA: 0.68 kg
ECH: 2.08 kg
DISTILLATION
Eff. To ETP: 4.51 kg
REACTION
Steam: 0.098 kg
ECH: 1.41 kg
DISTILLATION
FLOW DIAGRAM WITH MASS BALANCE OF EPOXY RESIN (BLR)
Caustic: 0.489 kg
IPA: 0.01 kg
Wash water: 3 kg
Wash water: 0.8 kg
ECH: 0.113 kg
Residue: 0.037 kg
Recycled water: 0.098 kg
PURIFICATION
Caustic: 0.011 kg
FILTRATION
Distilled water: 0.13 kg
RESIN: 0.978 kg
Water: 1 kg
Steam: 0.1 kgEff. To ETP: 1.01 kg
Filter cake: 0.009 kg
ATUL LIMITED
Name of Product: Thiamethoxam
New Project – Lab Process Details
1. Lab Process details:
Brief process and flow diagram of process stage wise
2-chloro-5-chloromethyl thiazole (CCMT) is reacted with 3-methyl-4-nitroimino perhydro-1,3,5-oxadiazine(NII)in presence of Dimethyl carbonate (DMC) as solvent and potassium hydroxide as base. After completion of reaction, DMC is recovered, water added and product is filtered, washed with water and purified in ethanol. Finally product dried at 60°c.
N
SCl
Cl HN N
O
NNO2
CH3
N
SCl
N N
O
NNO2
CH3
2-chloro-5-chloromethyl thiazole
M.W.-168 g/m3-methyl-4-nitroimino-perhydro-1,3,5-oxadiazine
M.W.-160 g/m
Thiamethoxam
M.W.-291.5 g/mM.F.-C8H10ClN5O3S
M.F.-C4H3Cl2NS M.F.-C4H8O3N4
KOH
DMC
MW:56 g/m
+ KCl + H2OMW:74.5 MW:18
Chemicals reactions with molecular weight stage wise
Sr. No.
List of raw materials along with quantity per KG
Chemical name Norms
1 2-chloro-5-chloro methyl thiazole
0.780
2 3-methyl-4-nitroimino perhydro-1,3,5-oxadiazine
0.760
3 Potassium hydroxide 0.200
4 DMC 0.200
5 Ethanol 0.340
Sr. No.
Complete Mass balance per KG Input
Input Quantity kg
Output Quantity in kg
1 2-chloro-5-chloro methyl thiazole
0.780 Thiamethoxam 1.0
2 3-methyl-4-nitroimino perhydro-1,3,5-oxadiazine
0.760 Aq layer 8.28
3 Potassium hydroxide 0.200
4 Dimethyl carbonate 0.200
5 Ethanol 0.340
6 Water 7
Total 9.28 9.28
C4H3NCl2S + C4H8N4O3 + KOH C8H10ClN5O3S + KCl + H2O
Complete Molecular balance
ATUL LIMITED
Name of Product: Quizalofop-ethyl
New Project – Lab Process Details
1. Lab Process details:
1.1 Brief process and flow diagram of process stage wise
2,6-Dichloro quinoxaline is reacted with ethyl-2-(4-hydroxy phenoxy)propionate in presence of Dimethyl formamide as solvent and potassium carbonate as base. After completion of reaction, DMF is recovered, water added and product is filtered, washed with water and purified in ethanol. Finally product dried at 60°c.
1.2
+
2,6-Dichloro quinoxaline Ethyl-2-(4-hydroxy phenoxy)-Propionate
OHC
CH3
C OC2H5
O
HON
N
Cl
Cl
N
NCl
OHCCH3
C OC2H5
OO
M.W.-199 g/mM.W.-210 g/m
R/S Quizalofop-ethyl
1/2
MW-138 g/m
potassium carbonate
1/21/2 H2O
Potassium chloride carbon dioxide
K2CO3
KCl CO2
M.W.-372.5 g/mM.W.-74.5 g/m
Chemicals reactions with molecular weight stage wise
1.3
Sr. No.
List of raw materials along with quantity per kg
Chemical name Norms kg
1 Ethyl-2-(4-hydroxy phenoxy) -propionate 0.602
2 2,6-dichloro quinoxaline 0.662
3 Potassium carbonate 0.45
4 DMF 0.606
5 Ethanol 0.5
1.5
Sr. No.
Complete Mass balance per kg
Input Quantity kg
Output Quantity kg
1 Ethyl-2-(4-hydroxy phenoxy) -propionate 0.602 Quizalafop ethyl 1.0
2 2,6-dichloro quinoxaline 0.662 CO2 0.13
3 Potassium carbonate 0.45 Aqueous layer 8.68
4 DMF 0.606
5 Ethanol 0.5
6 Water 7
Total 9.82 9.81
1.6
C8H4N2Cl2 + C11H14O4 + ½ K2CO3 C19H17N2O4Cl + KCl + ½ CO2 + ½ H2O
Complete Molecular balance
ATUL LIMITED
New Project – Lab Process Details
Name of Product: Pyrazosulfuron ethyl
1. Lab Process details:
1.1
Brief process and flow diagram of process stage wise
1-methyl-4-ethoxycarbonyl pyrazole sulfonamide is reacted with Phenyl-N-(4,6-dimethoxy)pyrimidine-2-carbamate n presence of acetonitrile as solvent and triethyl amine as base. After completion of reaction, water added and reaction mass acidified with HCl. Product is filtered, washed with water followed by methanol and dried.
1.2
NN
N
N
NN
N
N
COOC2H5
SO2NH2
CH3
+
OCH3
OCH3
HNC
O
O
Pyrimidine Carbamate
COOC2H5
CH3
SO2NH
OCH3
OCH3
HNC
O
ethyl 5-[(4,6-dimethoxypyrimidin-2-ylcarbamoyl)sulfamoyl]- 1-methylpyrazole-4-carboxylate
+
OH
Phenol
MW:233 g/m MW:275 g/m
MW:414 g/mMW:94 g/m
Chemicals reactions with molecular weight stage wise
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption /kg
1 Acetonitrile 2.941
2 Phenyl-N-(4,6-dimethoxy)pyrimidine-2-carbamate 0.694
3 1-methyl-4-ethoxycarbonyl pyrazole -5-sulfonamide.amide 0.588
4 Triethyl amine 0.388
5 Methanol 1.176
1.5
S.No.
Complete Mass balance per kg: Input
Input kg Output kg 1 Acetonitrile 2.941 Pyrazosulfuron ethyl 1.0 2 Pyrimidine carbamate 0.694 Aqueous layer 19.787
3 1-methyl-4-ethoxycarbonyl pyrazole -5-sulfonamide
0.588
4 TEA 0.388 5 Methanol 1.176 6 Water 15 Total 20.787 Total 20.787
1.6
C7H11N3O4S + C13H13N3O4 C14H18N6O7S + C6H6O
Complete Molecular balance
CHEMICAL REACTION OF DCDPS
+ SO3 CH3O SO2 OCH3SO2O + SO3
Pyrosulfate206
CH3O SO2 OCH3SO2O
Pyrosulfate206
Cl
+
MCB112.5
2
Cl ClSO2 + 2CH3O SO2 OH
DCDPS287
Methyl Hydrogen Sulfate112
+SO3
STAGE: 1
STAGE: 2
Cl
2 CH3O SO2 OH
Methyl Hydrogen Sulfate112
CH3O SO2 OCH3
Di Methyl Sulfate126
+ H2SO4
CH3O SO2 OCH3SO2O
Pyrosulfate206
Cl
+
MCB112.5
2 Cl SO2 + CH3O SO2 OH
Comp. 1206.5
Methyl Hydrogen Sulfate112
OCH3
DI METHYL SULFATE RECOVERY:
DMS: 1053 kg
SO3 : 1337 kg
CO2 (g): 298.15 kg
REACTIONMCB: 1881 kg
SO3 (g) to scrubber: 226.1 kg
Eff. To MEE: 12098.10 kg
Methanol recovered : 3380
REACTION
Water: 10273 kg
DMS: 855 kg
FILTRATION&
WASHING
FLOW DIAGRAM WITH MASS BALANCE OF DCDPS
Na2CO3: 1053 kg
DIGESTIONMethanol (fresh + recovered): 3670 kg
ML to Methanol recovery: 4007 kg DISTILLATION
Dist. Loss: 70 kg
Residue : 557 kgDRYING Drying loss: 204.2 kg
DCDPS: 1578.85 kg
ATUL LIMITED (Corporate SHE Dept.)
Division: CP R&D
Name of Product: Metribuzin
Lab Process details:
New Project – Lab Process Details
Date: 25/02/2015
i) Brief process and flow diagram of process stage wise-
Brief Process:
Brief process and flow diagram of process stage wise Charge 98% Sulfuric acid and 4-amino-6-tertiary-butyl-3-mercapto-1,2,4-triazinone in flask. Add Methanol in reaction mass and cook mass for 10 hrs at 55°c. Quench reaction mass in to water at 10°c. Stir mass for 2 hrs and neutralize reaction mass with 48% caustic lye to pH 7. Filter Metribuzin and wash with water. Dry Metribuzin at 75°c. Recover water from mother liquor, filter sodium sulfate and recycle water back in the process.
ii) Chemicals reactions with molecular weight stage wise
+ CH3OH + H2SO4 + 2NaOH + Na2SO4 + 3H2O
4-amino-6-tertiary butyl-3-mercapto-1,2,4-triazin-5-one
MW-200g/m
MW-32g/m MW-98g/m MW-40g/m
MW-214g/m
MW-18g/mMW-142g/m
N
CH3
SH
CH3
N
N SH
NH2
N
CH3
SH
CH3
N
NH2
N
SH
Metribuzin
iii) List of raw materials along with quantity per KG
Sr. No. Raw Materials Purity MW Norms
kg/kg
1
4-amino-6-tertiary-butyl-3-mercapto-1,2,4-triazinone
98% 200 1.05
2 98% Sulfuric acid 98% 98 1.68
3 Methanol 99% 0.21
4 48% Caustic lye 48% 40 2.95
iv) List of co-product per KG Sodium sulfate: 2.38
v) Complete Mass balance per KG
Sr. No. Input
Kg
%Purity Sr. No.
Output Kg %Purity
1
4-amino-6-tertiary-butyl-3-mercapto-1,2,4-triazinone
1.05 98 1 Metribuzin 1.04 97
2 98% Sulfuric acid 1.68 98 2 Aqueous-1 13.0 NA
3 Methanol 0.21 99 3 Aqueous-2 2.0 NA
4 48% Caustic lye 2.95 48
5 Water 10.52
Total
16.42 Total
16.04
vi) Complete Molecular balance C7H12OSN4 + CH3OH + H2SO4 + 2NaOH C8H14OSN4 + Na2SO4 + 3H2O
200 32 98 80 214 142 54
vii) Complete Water balance
Material req. kg/kg Metribuzin
Sr. No. Raw Materials Input
Qty kg
Sr. No Materials Output
Qty kg
1 98% Sulfuric acid 1.68
1 Aqueous 1 13.0
2 48% Caustic lye 2.95
2 Aqueous 2 2.0
3 Water 10.52
Total input 15.15 Total output 15.0
2. Gas Emission: Gas emission stage wise per KG: Nil 3. Water discharges: Water is recovered by distillation from aqueous -1 &2 and is to be recycled back in the process.
4. Waste generation: Solid waste generated per KG: Nil Solid waste characteristics and its proposed treatment developed if any.NA
5. Details of Hazardous chemicals: Hazardous chemicals used and method of handling & disposal.
1) 4-amino-6-tertiary-butyl-3-mercapto-1,2,4-triazinone: Refer MSDS. 2) 98% Sulfuric acid: Refer MSDS
6. Other Consideration:
Recycle & Reuse options in process.
1. Water: Recover from aqueous-1&2 and reuse in the next batch. 7. Any other relevant information:
You may want to share about the product\process: NA
Dr. Jayesh Parekh Dr Palaniappan. R
Date: 25/02/2015 Project In-Charge G.M R & D
CHEMICAL REACTION OF ISOPROTHIOLANESTAGE: 1
CS2
Di Isopropoyl MalonateDi Sodium salt of Di Iso propoxy
Carbonyl ketone mercaptide
188 308
+ + 2H2O
Carbon Disulfide76
CH2
COOCH(CH3)2
COOCH(CH3)2
2NaOHC
COOCH(CH3)2
COOCH(CH3)2
CNaS
NaS
STAGE: 2
Di Sodium salt of Di Iso propoxyCarbonyl ketone mercaptide
308
+ + 2NaBrCCOOCH(CH3)2
COOCH(CH3)2
CNaS
NaSCH2 CH2
Br Br
Ethylene Dibromide188
CCOOCH(CH3)2
COOCH(CH3)2
CS
S
CH2
CH2
ISOPROTHIOLANE290.4
Di Isopropyl Malonate: 0.95 kg
CS2: 0.46 kg
DISTILLATION
REACTION
Eff. To Incinerator: 1.58 kg
FLOW DIAGRAM WITH MASS BALANCE OF ISOPROTHIOLANE
ISOPROTHIOLANE: 1.04 kg
Acetone: 2.8 kg
NaOH: 1 kg
N-Hexane: 2.11 kg
Vapor loss: 0.25 kg
TBAB: 0.01 kg
Ethylene Dibromide: 0.88 kg
CS2 recovered : 0.18 kg
NaBr: 0.82 kg
N-Hexane recovered : 2 kg
Acetone recovered: 2.66 kg
CHEMICAL REACTION OF PYRIDINE BASED INSECTICIDES & HERBICIDES CHEMICAL IMIDACLOPRIDSTAGE: 1
STAGE: 2
STAGE: 3
H2SO4
Guanidine Nitrate Nitroguanidine122 104
C NHHNO3
NH2
NH2
C NH
NO2
NH2
NH
KOH
Nitroguanidine104
C NH
NO2
NH2
NH+
CH2 CH2
NH2 NH2
NH NO2
NH N + NH3
Ethylene Diamine60
2-[Nitroimino] imidazolidine130
Ammonia17
+
NH NO2
NH N
2-[Nitroimino] imidazolidine130
2-Chloro-5-Chloromethyl Pyridine162
CH2Cl
Cl N
NH NO2
N NCH2
Cl N
+ HCl
Imidacloprid
255.5
H2SO4: 50 kg
Guanidine Nitrate: 65 kg
REACTION
EDA: 131.4 kg
REACTION
FLOW DIAGRAM WITH MASS BALANCE OF PYRIDINE BASED INSECTICIDES & HERBICIDES CHEMICAL IMIDACLOPRID
IMIDACLOPRID: 100 kg
HCl: 800 kg
KOH: 500 kg
Effluent to ETP: 1847.36 kg
Residue: 13.32 kg
Water: 740 kg
Eff. To Incinerator: 675 kg
Water: 300 kg
NH3 (g) to scrubber: 13.21 kg
REACTION&
DISTILLATION
2-chloro-5-methylchloro-pyridine : 74.6 kg
Sodium Methoxide: 40 kg
DMF: 112.5 kg Effluent to ETP: 1167.37 kg
Water: 1125 kg
Distillation loss: 5.97 kg
Methanol recovered : 11.5 kg
DMF recovered : 104.7 kg
CHEMICAL REACTION OF GLYPHOSATE
Name: N-Phosphonomethyl iminodiacetic acid Hydrogen peroxide Glyphosate Carbon dioxide Formaldehyde Water
MW 227 34 169 44 30 18
(OH)2-P-CH2-N-(CH2COOH)2
O
(OH)2-P-CH2-NH-CH2COOH
O
+ H2O2 + CO2 + HCHO + H2O
Water: 1000 kg
PMIDA: 2000 kg
PRECIPITATION&
DRYING
CO2 (g) : 375.09 kg
REACTION
Eff. To Incinerator: 2347.95 kg
FLOW DIAGRAM WITH MASS BALANCE OF GLYPHOSATE
GLYPHOSATE: 1447.95 kg
Sodium tung state : 6 kg
H2O2: 700 kg
10% FeSO4 : 300 kg
Water: 300 kg
Vapor loss: 135 kg
STEP-1
Input Qty in Kg Output Qty in Kg
o-CRESOL 1389.096 SO2 815.00
SO2Cl2 1726.812 HCl 465.00
AlCl3 6.372
DPS 6.372
TOTAL 3128.652 FRACTIONAL DISTILLATION
CRUDE PCOC 1848 1ST CUT 142.30
1848.00 MIDCUT 60.98
PRODUCT 1459.92
RESIDUE 184.80
TOTAL 1848.00 OUTPUT 1848.00INPUT
STAGE-3
SO2 815.00 SO2Cl2 1719.14
Cl2 904.1406 wastecarbon 0.17
SULFURYL CHLORIDE PREPARATION
PREPARATION OF 4-CHLORO-2-METHYL PHENOL (PCOC)
Reaction stage-1
Chlorination of o-cresol
Reaction stage-2
FractionalDistillation
Reaction stage-3
Sulfuryl chloride preparation
Active carbon 0.171OUTPUT 1719.31
TOTAL 1719.31INPUT
Step-1
INPUT QTY PURITY REAL M.Wt MOLE % EXCESSo-CRESOL 1389.096 100% 1382.151 108.5 12.74 1
SO2Cl2 1726.812 100% 1726.812 135 12.7912 1.00AlCl3 6.372 100% 6.372 133 0.04791DPS 6.372 100% 6.372 186 0.034258Cl2 904.14 100% 904.1406 71 12.73438
Active Carbon 0.17 100% 0.171TOTAL 4032.964
OUTPUT Kg1st cut 142.302nd cut 60.98
PRODUCT 1459.92RESIDUE 184.80
HCl 465.00SO2Cl2 1719.14
waste carbon 0.17TOTAL 4032.31
4-Chloro-2-Methyl Phenol ( PCOC)
To be scrubbed in waterTo be used in process
RemarksTo be recycle in stage-1To be recycle in stage-2To be taken for MCPA preparationTo be sent for incineration
STEP-2
WT IN KG WT IN KG
WATER 345.244652MCA 1338.91
TOTAL 1684.15465
30% NaOH 1418.93PCOC 1459.9230%NaOH 2537.3
WATER 6081.69 13181.9947 AQ LAYER
TOTAL 13181.9947 13181.9947
STEP-2
WATER 101530%HCl 2129.37AQ LAYER 13181.9947
TOTAL 16326.3647
REAN MASS 2787 WET CAKEWATER WASH 6081.7 12989 6493.52 ML+WML
ML WMLTOTAL 22408.0647 22270
WET CAKE 2787 1952 DRY CAKE
TOTAL 2787 1952
ACIDIFICATION
PREPARATION OF MCPA
R-2
MS
R-3MSGL
BRIEF PROCESS OF 4-CHLORO-2-METHYL PHENOXY ACETIC ACID ( MCPA)
STEP-1 PREPARATION OF 4-CHLORO-2-METHYL PHENOL(PCOC)
Chlorination of o-cresol carried out using sulfuryl chloride as chlorinating agent and Aluminium chlorideand Diphenyl sulfide as catalyst. 4-chloro-2-methyl phenol was separated from crude mass by fractional distillationand used for MCPA preparation.
STEP-2 PREPARATION OF 4-CHLORO-2-METHYL PHENOXY ACETIC ACID
Condensation of PCOC carried out with chloroacetic acid in prsence of caustic lye to give sodium salt of MCPA.Which on acidification with 30%HCl give 4-chloro-2-methyl phenoxy acetic acid.
Step-3 Preparation of Sulfuryl chloride
Sulfur dioxide reacted with Chlorine gas in presence of active carbon as catalyst to give sulfuryl chloride.
GLYPHOSATE ( N-PHOSPHONOMETHYL GLYCINE)
INPUT OUTPUTKG KG
DM water 2700
PMIDA 2000 350 CO2
Sodium Tungstate 6
50%H2O2 700
TOTAL INPUT 5406
5056
Reaction mass 5056
10%FeSO4 300
TOTAL INPUT 5356
1000 1600 wet productDM water 3800 MLReaction mass 5356 956 WML
TOTAL INPUT 6356 6356 OUTPUT
Wet product 1500 1440 GLYPHOSATE
SN Name Qty Purity Real MW Mole1 DM water 3700 100% 3700 18 205.55562 PMIDA 2000 99% 1980 227 8.7224673 50%H2O2 700 50% 350 34 10.294124 Na-Tungstat 6 99% 5.94 330 0.0185 10%FeSO4 300 10% 30 152 0.197368
6706
SN Name Qty Purity Real MW Mole1 Na-Tungstat 6 90% 5.4 18 0.32 ML 3800
Reaction massSodium tungstate
7% HCHO,0.7%FeSO4,92% water
INPUT
OUTPUT
Stage-1
Main reaction
Filtration
Stage-2
Precipitation
Filtration
Drying
3 WML 9564 CO2 350
Glyphosate 14406552
98%water,0.5% max HCHO
99% Purity
GLYPHOSATE BRIEF PROCESS:
Oxidation of Phosphonomethyl iminodiaceticacid carried out with Hydrogen peroxide usingSodium tungstate as catalyst in water.Ferrous sulfate added and precipitated Glyphosate se filtration and washed water.Generated effluent was treated chemically to decompose formaldehyde before discharging t
eparated by
to ETP.
ATUL LIMITED (Corporate SHE Dept.)
Division: CP R&D
Name of Product: Diafenthiuron
Lab Process details:
New Project – Lab Process Details
Date: 25/02/2015
i) Brief process and flow diagram of process stage wise-
Brief Process:
Brief process and flow diagram of process stage wise Charge Toluene and 4-phenoxy-2, 6-diisopropyl phenyl isothiocyanate in the flask. Add Tertiary butyl amine in reaction mass and cook mass for 2 hrs. Recover toluene and add n-hexane to the reaction mass. Cool reaction mass to 10°C.Filter solid Diafenthiuron and wash with hexane. Recover n-hexane from ML and send residue for incineration.
ii) Chemicals reactions with molecular weight stage wise
iii) List of raw materials along with quantity per KG
Sr. No. Raw Materials
Purity MW Norms kg/kg
1
4-phenoxy-2, 6-diisopropyl phenyl isothiocyanate
96% 311 0.912
2 Tertiary butyl amine 99% 73 0.675
3 Toluene 99% 0.03
4 Hexane 99% 0.09
O
CH
CH
NH
CH3
CH3
CH3
CH3
NH
S CH3
CH3
CH3
CH
CH
N=C=S
CH3
CH3
CH3
CH3
ONH2
CH3
CH3
CH3+
Toluene
4-phenoxy-2,6-diisopropyl phenyl isothiocyanateTertiary butyl amine
M.W--311g/mM.W.-73.11g/m
DiafenthiuronM.W.-384g/m
iv) List of co-product per KG No co-product formed in Diafenthiuron process
v) Complete Mass balance per KG
Sr. No. Input
Kg
%Purity Sr. No.
Output Kg %Purity
1
4-phenoxy-2, 6-diisopropyl phenyl isothiocyanate
0.912 96
1
Diafenthiuron 1 98
2 Tertiary butyl amine 0.214 99
2 Rec. Toluene 0.68 99
3 Toluene 0.72 99
3 Rec. Hexane 1.73 99
4 Hexane 1.82 99
4 Residue 0.256 NA
Total
3.666 Total 3.666
vi) Complete Molecular balance C19H21ONS + C4H11N - C23H32ON2S
4-phenoxy-2, 6-diisopropyl phenyl isothiocyanate Tertiary butyamine Diafenthiuron
MW 311 73 384
vii) Complete Water balance Water is not used in Diafenthiuron process
2. Gas Emission: Gas emission stage wise per KG : Nil 3. Water discharges: Water is not used in Diafenthiuron process
4. Waste generation: Solid waste generated per KG : 0.256 Solid waste characteristics and its proposed treatment developed if any.NA
5. Details of Hazardous chemicals: Hazardous chemicals used and method of handling & disposal.
1) 4-phenoxy-2, 6-diisopropyl phenyl isothiocyanate: Refer MSDS. 2) Tertiary butyl amine: Refer MSDS
6. Other Consideration:
Recycle & Reuse options in process.
1. Toluene and n-hexane: Recover from process and use in next batch as a solvent. Solvent recovery details stage wise per KG.
Materials Output Qty kg (purity, % ) Recover toluene 0.68 99.5
Recover hexane 1.73 99.40 7. Any other relevant information:
You may want to share about the product\process: NA
Dr. Jayesh Parekh Dr Palaniappan. R
Date: 25/02/2015 Project In-Charge G.M R & D
ATUL LIMITED (Corporate SHE Dept.)
Division: Crop protection
Name of Product: Indoxacarb: ( (S)-methyl-7-chloro-2,5-dihydro-2-[[methoxycarbonyl)[4-(trifluoromethoxy)phenyl]amino]carbonyl]indenol[1,2-e][1,3,4]oxadiazine-4a(3H)-carboxylate
1. Lab Process details:
New Project – Lab Process Details
Date: 10-03-2015
Brief process and flow diagram of process stage wise
Synthetic scheme of Tech. Indoxacarb:
Part-A:
O
Cl
O
Cl
O
O O
Cl
O
OCinchonine & TBHP OH
Phenylmethyl hydrazine carboxalate
N
Cl
O
OOH
NHCO2CH2PhCelite/ P2O5
EDClCl
NN
O
CO2CH2Ph
O
O
Cl
NHN
O
O
O
(1) (2) (3)
(4) (5) (6)
5% Pd/C / H2
Methyl acetate
Toluene EDClToluene
NaOCH3
Part-B:
OCF3
NH2MCF /NaHCO3
H2O
OCF3
NHCO2CH3COCl2 / NaH / DME
DCM
OCF3
NCO2CH3
COCl
PART A +B
Cl
NHN
O
O
O
( 6)
+
OCF3
NCO2CH3
COCl
Methyl acetateCl
NN
O
O
O
NOCO2CH3
OCH3
( 9 ) ( 10 )
( 7 ) ( 8 ) ( 9 )
NaOH
5-chloro indanone (1) was carbomethoxylated with dimethylcarbonate in the presence of sodium methoxide and solvent toluene which afforded methyl-5-chloro-1-oxo-2, 3-dihydroindene-2-carboxtlate (2).
Enantioselective catalytically hydroxylation of (2) with chiral base (cinchonine) and t-butyl hydroperoxide to gave (+) hydroxyl indanone (3) in 42 % ee. Reaction of (3) with benzyl carbazate furnished Cbz-protected hydrazone (4) and which was condensed with methylal in the presence of phosphorus pentoxide to gave oxadiazine (5).
Debenzylation by hydrogenation using catalyst Pd/C was accompanied by decarboxylation and the resulting oxadiazine (6) was immediately coupled with carbonyl chloride (9) to afford the derived Indoxacarb (10)
The synthesis (9) from 4-(trifluoromethoxy) aniline (7) involves reaction with methylchloroformate in the presence of base followed by condensation of the sodium salt of its methyl carbamate(8) with excess phosgene gave (9).
Stage-A1:
flow diagram of process stage wise
Step-I
1) 778 g Toluene 4) 168 g Indanone 2) 83.4 g NaOMe + 520 g Toluene+ 180 g DMC 3) 90 g DMC
5) Distillation of MeOH+DMC+Toluene (365 g)
1) 1000 g Water 2)above 3) 160 g 35% HCl
Slurry 4) 150 g NaHCO3 Soln
5)2×200 g Waterwash
Distillation 1)aq.layer seaparation
(touene 370 g) Org layer (1275 g) Aq phase
i)1172 g ii) 195 g iii) 402 g
104˚C-109˚C
10˚C
922 g A1 Soln
Stage: A2:
Step-2
1)30.5 g Cinchonine 2) 116 g TBHP
25 g Toluen Filter
Dryed 150-151 g A2 !st Crop
1)872 g 35 % HCl ML 50˚C
2) 100 g Water
Separate layers
Distillation-Org lyr Aq.layer 125 g 32 % NaOH
656 g Toluene
0
10 g Toluene Filter 300 g Water filter
Dry at Dry at 28 g Cinchonine
50˚C 50˚C
28.0 g A2 2nd Cro 76.0 g Distilled Toulene
48.0 g Residue
922 g A1 Soln i)10-15˚C
ii)40-45˚C iii)0-5˚C
Wet Cake
25-30˚C
1038 g 0-5 ˚C
820 g
W.C. W.C.
ML
Stage: A3 &A4:
1)345 g EDcl 5) 5.5 g Water 2) 78.2 g A2 3) 58.0 g BCZ 4) 4.2 g PTSA
1)346 g EDcl 2) 111.6 g Hylfow 3) 111.6 g P2O5 5) A3 RM 4) 143.6 g
Methylal
3×63 g EDcl
Filter
1)235 g IPA Distillation 801 g EDcl
2×8 gm IPA Filter
Dry
50˚C
80˚C
65-70˚C
198 g Sludge
Filtrate 80-85˚C
Wet Cake 102 g A4
Stage: A5& A6 6) ZnBr2 3) DM Water
7)5% pd/C 4) Citric acid
2) A4 5)C.S.flaks
1) MA 8) H2
9) B2
Filter
NaHCO3 +H2O
Water
Separation
Organic layer Rec. of MA
Silica
Aq .Layer Hexane
Filter
Recycle ML
10-150C
5% pd/C
600C Org.layer 10-150c
Tech.Indoxacarb
Organic Layer
Indoxacarb
Step-I
Chemicals reactions with molecular weight stage wise
O
Cl
C OCH3
O
H3CO
Cl
O
CO2CH3
CH3OH CH3ONa
M.W: 224.5g/m
M.W:32 g/m M.W: 54g/m
M.W:166.6g/m
M.W:54g/m
M.W:90g/m
Sodium methoxide
5-Cl-1-indanoneDimethyl carbonate
CH3ONa
Toluene
A1
Step-II
Cl
O
CO2CH3
Cl
O
M.W: 240.5g/m
OH
CO2CH3
Tertiary butanol
M.W: 74g/m
A1
tertbutyl hydroperoxide
M.W: 224.5g/m
M.W: 90.0g/m
A2
Toluene
Cinchonine
(CH3)3COOH
(CH3)3COH
Step-III
Cl
O
M.W: 240.5g/m
OH
CO2CH3
HN
NH2
O
O
Benzyl carbazate
Cl
N
M.W: 388.5g/m
OH
CO2CH3
NHCO2CH2Ph
H2O
A3
A2
M.W: 18 g/m
M.W: 166.0g/mEDC
PTSA
Step-IV
Cl
N
M.W: 388.5g/m
CO2CH3
NHCO2CH2Ph
A3Cl
N
CO2CH3
A4
2CH3OHCH2
N
CH2(OCH3)2
Methylal
CO2CH2Ph
M.W: 400.5g/m2(32)
M.W: 76.0g/m
EDC
P2O5
OOH
If SOP followed there is no run away reaction
Step-V
M.W: 400.5g/m
H2
Cl
NO
CO2CH3
A5
CH2
N
H
M.W: 266.5g/mM.W: 44.0g/m M.W: 92.0g/m
Carbon dioxide
CH3
Toluene
C OOMethylacetate
Cl
NO
CO2CH3
A4
CH2
N
CO2CH2Ph
5% Pd/C
Hydrogen gas
M.W:2 g/m
714 g for 1kg indoxa78 g / 1kg of indoxa carb
Step-VI
Cl
N
CO2CH3
A5
N
H
M.W: 266.5g/m
O N
COCl
CO2CH3
B2
M.W: 297.5g/m
Cl
N
A6
N
M.W: 527.5g/m
OCF3N
H3CO2C
O
C
F
F
F
Methyl acetate
O
CO2CH3
HCl
M.W: 36.5g/m
O
Inndoxacarb
Indoxacarb B1
NH2
OCF3
O
OClCH3
Methyl chloroformatePTFMA
M.W. 177.0g/m
NHCOOCH3
OCF3
sodium bicarbonate
Sodium chloride Water
M.W. 58.5g/m M.W. 18.0g/m
B1
M.W. 235.0g/mM.W.:94.5 g/m
HO
HNaCl
NaHCO3
If SOP followed there is no run away reaction
Indoxacarb B2
NHCOOCH3
OCF3
B1
M.W. 235.0g/m
NaH
M.W. 24.0g/m
Sodium hydride
O
Cl
Cl
Carbonyl chloride
M.W. 99.0g/m
N
OCF3
B2
M.W. 297.6 g/m
COOCH3
Sodium chloride
M.W. 58.5 g/m
H2
M.W. 2.0g/m
NaCl
Hydrogen
DCM
Cl
O
Benzyl carbazate
Step-I
C O
C2H5O
C2H5O
2HO
Benzyl alcohol
OO
O
Dibenzyl carbonate
2C2H5OH
2(46)
Diethyl carbonate
M.W: 118 g/m 2(108)M.W: 242.4 g/m
Ethanol
Step-II
OO
O
Dibenzyl carbonate
M.W: 242.4 g/m
NH2NH2.OH
Hydrazine hydrate
M.W: 50.0 g/m
HN
NH2
O
O
Benzyl carbazate
M.W: 166.0 g/m
HO
Benzyl alcohol
M.W: 108.0 g/m
HO
Hwater
M.W: 18.0g/m
List of raw materials along with quantity per KG
No Name of raw material Quantity (Kg) Quantity (Kg) Consumption(Lab) Consumption(Plant)
1 5-chloro-1-indanone 0.515 0.74 2 Sodium methoxide 0.256 0.36 3 Dimethyl carbonate 0.622 0.91 4 Toluene 1.025 1.77 5 HCl(35 %) 0.705 1.34 6 Sodium bi carbonate 0.364 0.691 7 Cinchonine 0.0076 0.03 8 tert-butylhydrogenperoxide 0.356 0.47 9 Sodium hydroxide 0.3 0.647
10 Ethylene di chloride 0.948 1.43 11 Benzyl alcohol 0.58 0.803 12 Diethyl carbonate 0.455 0.63 13 Hydrazine hydrate(80%) 0.243 0.337 14 Chlorobenzene 0.373 0.518 15 P-toluene sulfonic acid 0.029 0.04 16 Hyflow 0.778 0.56 17 Phosphorous pentoxide 0.778 0.72 18 Dimethoxy methane 1.004 0.98 19 Isopropanol 0.349 0.72 20 Methylacetate 1.534 2.38 21 Citric acid 0.56 0.58 22 D. M water 2.14 2.14 23 Pd/ C( 5%) 0.0357 0.004 24 Zinc bromide 0.023 0.02 25 H2 gas 0.006 0.02
26 P-trifluoromethoxy aniline 0.318 0.42
27 Methyl chloroformate 0.266 0.26
28 Methylene di chloride NA 2.73 29 1,2-dimethoxy ethane(Monoglyme) NA 0.338 30 Phosgene 0.551 2.42 31 n-Hexane 1.7 1.74 32 Soda ash 0.038 0.62 33 Sodium hydride NA 0.105 34 Silica 0.176 0.177
List of co-product per KG
Stages In put Qty Co-product Qty Stage-A1 5-chloro-1-Indanone 515 g Methanol 197.89 g NaCl 180.8 g Stage-A2 A1 624.4 g Tert- butanol 205.8 g Stage- A3 A2 520 g Nil Nil Stage- A4 A3 756 g Methanol 124.5 g Stage-A5 A4 714 g Toluene 164 g Stage-A6 A5 475 g NaCl 104 g BCZ-1 Diethyl carbonate 630 g Ethanol 491 g BCZ Dibenzyl carbonate 1294 g Benzyl alcohol 576.6 g B1 PTFMA 318 g NaCl 105 g B2 B1 409 g NaCl 101 g
Complete Mass balance per KG
I
INPUT
N
OUTPUT
D Sr.No. Raw Materials Quantity[kg.] O Sr.No. Materials Quantity[kg.]
1 5-chloro-1-indanone 0.232 X 1 Indoxacarb S Isomer 0.3138 2 Sodium methoxide 0.113 A 2 Recovered Toluene 4.008 3 Dimethyl carbonate 0.676 C 3 Recovered Methanol 0.133 4 Toluene 4.76 A 4 Recovered Ethylene dichloride 1.387 5 HCl(35 %) 0.421 R 5 Recovered Isopropyl alcohol 0.687 6 Sodium bi carbonate 0.234 B 6 Recovered Dichloromethane 3.447 7 Cinchonine 0.037 7 Recovered Hexane 0.712 8 tert-butylhydrogenperoxide 0.147 T 8 Recovered Methyl acetate 1.2 9 Sodium hydroxide 0.099 E 8 Solvent Vapor loss 5.25
10 Ethylene di chloride 1.94 C 10 Recovered Cinchonine 0.0325 11 Benzyl alcohol 0.477 H 11 Organic/Aqueous phase effluents with 4.39 12 Diethyl carbonate 0.2 salts
13 Hydrazine hydrate(80%) 0.106
14 Chlorobenzene 0.679
15 P-toluene sulfonic acid 0.012 Total 21.5603 16 Hyflow 0.176
17 Phosphorous pentoxide 0.226 18 Dimethoxy methane 0.308 19 Isopropanol 0.968 20 Methylacetate 1.89 21 Citric acid 0.18 22 D. M water 0.672 23 Pd/ C( 5%) 0.004 24 Zinc bromide 0.006 25 H2 gas 0.006 26 N2 gas 0.003 27 P-trifluoromethoxy aniline 0.132 28 Methyl chloroformate 0.081 29 Methylene di chloride 5.03 30 Sodium hydride 0.0341 31 1,2-Dimethoxy ethane 0.11 32 Phosgene 0.194 33 n-Hexane 1.575 34 Silica 0.053
21.78
Complete Molecular balance
Already given in above schemes
Complete Water balance Stage-1: A1: Water input for work up: 8.189 kg Water out put as a effluent: 8.227 kg A2: Input: 7.286 kg Out put: 7.348 kg Stage: 2: A3: Input: Nil Out put from reaction: 0.046 kg A4: Input for work up: 3.432 kg Out put as a effluent: 3.582 kg Stage: 3: A5: Input for buffer solution: 2.14 kg Out put as a effluent or recycle: 3.5 kg A6: Input: 0.204 kg Out put: 0.250 kg Stage: 4
M.W: 400.5g/m
H2
Cl
NO
CO2CH3
A5
CH2
N
H
M.W: 266.5g/mM.W: 44.0g/m M.W: 92.0g/m
Carbon dioxide
CH3
Toluene
C OOMethylacetate
Cl
NO
CO2CH3
A4
CH2
N
CO2CH2Ph
5% Pd/C
Hydrogen gas
M.W:2 g/m
714 g for 1kg indoxa78 g / 1kg of indoxa carb
: B1: Input as a reaction water: 15.94 kg Out put as a effluent: 16.22 kg B2: Input for B1 recovery: 1.1 kg Output as a effluent: 1.15 kg
2. Gas Emission:
Gas emission stage wise per KG
Reaction scheme for B2: Gas emission per kg of indoxacarb
177 g/mole94.5 g/mole 84 g/mole 235 g/mole
58.5 g/ mole 44 g/ mole 18 g/mole398 g 99 g/ 1 kg indoxa
235 g/mole 24 g/mole 297. 5 g/mole
58.5 2 g/mole511 g
4.3 g/1 kg indoxa
3. Water discharges:
Raw water consumption details per KG Waste water quantity and quality generated i.e. pH, COD TDS acidity, alkalinity etc per KG Stream wise quality of the effluent (Analysis reports | experimental results) per KG Proposed treatment method developed if any.
4. Waste generation:
Solid waste generated per KG Solid waste characteristics and its proposed treatment developed if any.
Pl. refer As per given above table
As per above requirement we mentioned in below table as per stage wise of 1 kg tech. Indoxa carb Effluent / solid waste generated stage wise for 1 kg tech. Indoxacarb
Sr Stage Effluent Solid waste
Qty / kg of Indoxacarb
pH COD BOD TDS Remark
1 Step-1(A1)
Aqueous - 3.583 2.3 24000 7142.8 80430 To be treated in ETP as current practice
Step-1(A1)
Aqueous 1.726 8.1 5680 1200 11540
2 Step-2(A2)
Aqueous 4.01 12.1 4570 800 52470
Step-2(A2)
- Organic residue
0.147 - - - - To be incenerated
3 Step-3&4(A3 & A4)
Aqueous 3.188 8.1 ETP
Step-3&4 )A3 &A4)
Hyflow sludge
1.381 To be incenerated
Step-3&4(A3 &A4)
Organic residue
0.419 To be incenerated
4 Step-5&6 (A5&A6)
Aqueous 1.7 2.8 166536 88500 To be recycle and use in next batch
Step-5&6 (A5&A6
Aqueous 0.9 ETP
5 B1 Aqueous 0.29 8 17881.6 108510 ETP Aqueous 1.276 7 5852 22410 ETP B2 Aqueous 1.31 6 8388.5 18100 ETP Aqueous 1.31 6 58390.4 12300 ETP
5. Details of Hazardous chemicals:
Hazardous chemicals used and method of handling & disposal.
Pl. refer below table for above requirement
6. Other Consideration:
Recycle & Reuse options in process.—Most of the solvent we recover and reuse Solvent recovery details stage wise per KG. Pl. refer below table for solvent details
Solvent consumption for 1Kg Tech. Indoxacarb-
Stagewise R&D Plant
No Stages Name of solvents Consume qty(Kg)
Usages qty(Kg)
Recovery (%)
Consume qty(Kg)
Usages qty(Kg)
Recovery (%)
1 A1 & A2 Toluene (NEW TTD) 0.366 4.025 91 2.39
15.14 kg 84.22
2 Dimethyl carbonate (NEW TTD) 0.303 0.819 66 1.305 2.15 39.24
3 A3 & A4 Ethylene di chloride(NEW TTD) 0.948 6.355 85 1.97 6.91 71.53
4 Isopropanol (NEW TTD) 0.349 1.757 80 0.89 3.08 71
5 A5 & A6 Methylacetate -Normal 1.534 6.334 75 2.22 6.02 63.51
6 Hexane-Normal 1.63 3.35 51 1.44 2.61 45.16
7 B1 & B2 Dichhloro methane-OLD 1.51 7.55 80 5 16 69.13
8 Hexane-OLD 0.236 0.786 70 1.4 2.4 42
9 BCZ Benzyl alcohol-OLD 0.298 1.023 71 0.27 on DBC 1.52 on DBC
82 On DBC
10 Mono chloro benzene-OLD 0.245 0.816 70 1.05 2.16 51.65
Sr. No Hazrdous chemical Handling Disposal 1
NaOCH3(Sodium methoxide
Use PPE and use nitrogen while charging .In detail please refer MSDS
In detail please refer MSDS
2 Phosphorous pentoxide(P2O5)
Use PPE and use nitrogen while charging .In detail please refer MSDS
In detail please refer MSDS
3 5% palladium on carbon Use PPE and use nitrogen while charging .In detail please refer MSDS
In detail please refer MSDS
4 Methyl chloroformate Use PPE .In detail please refer MSDS
In detail please refer MSDS
5 Phosgene Use PPE .In detail please refer MSDS
In detail please refer MSDS
7. Any other relevant information:
You may want to share about the product\process
Date: 10/03/2015 Project In-Charge G.M R & D
RJP / UBP R. Pallaniappan
ATUL LIMITED
Name of Product: Bispyribac sodium
1. Lab Process details:
1.1
New Project – Lab Process Details
Brief process and flow diagram of process stage wise
2, 6-Dihydroxy benzoic acid is reacted (2,6-DHBA) with 4,6-dimethoxy-2- methylsulfonyl pyrimidine (4,6-DMMSP) in presence of THF as solvent and sodium hydride as base. After completion of reaction, THF is recovered, water added and product is filtered, washed with water and dried.
1.2
COOH
OHHO3NaH
COONa
ONaNaO3H2
COONa
ONaNaON
N SO2CH3
OCH3
H3COCOONa
OO
N
N
H3CO
H3CO
N
N
OCH3
OCH3
2SO2CH3Na
2,6-DHBAMW-154 g/m MW-220 g/m
MW-218 g/m
2
MW-102 g/m
MW-452 g/m
Bispyribac-sodium
MW-24 g/m
MW-220 g/m
Chemicals reactions with molecular weight stage wise
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Kg/kg 1 THF 2.1 2 2,6-Dihydroxy benzoic acid (2,6-DHBA) 0.486 3 4,6-Dimethoxy 2-methylsulfonyl pyrimidine (4,6-DMMSP) 0.973 4 Sodium hydride 0.413
1.5
S.N.
Complete Mass balance per kg:
Input kg Output kg 1 THF 2.1 Bispyribac sodium 1.0 2 2,6-DHBA 0.486 Sodium methane sulfonate 0.900 3 4,6-DMMSP 0.973 Aqueous layer 22.06 4 Sodium hydride 0.413 Hydrogen 0.019 5 Water 20
Total 23.972 Total 23.972 1.6
C7H6O4 + 3NaH C7H3Na3O4 + 3H2
Complete Molecular balance
C7H3Na3O4 + 2C7H10N2O4S C19H17N4NaO8 + 2SO2CH3Na
ATUL LIMITED
Name of Product: Azoxystrobin
1. Lab Process details:
1.1 Brief process and flow diagram of process stage wise: (E)-Methyl 2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxyacrylate is reacted with 2-cyanophenol in presence of base potassium carbonate and catalyst DABCO in DMF and toluene mixture at 80°c. Once reaction completed, crude product is isolated. The crude product obtained is purified with methanol to get technical Azoxystrobin.
Process flow diagram:
Project – Lab Process Details
Preparation of Azoxystrobin (MW: 403.4)
(1) 135g. Toluene (2)
97.1 g. CPOPMA
(3) 44 g. 2-Cyanophenol
(6) 0.7 g. DABCO in 10 g DMF
Layer separation
Recovery
105 g. Methanol
Filter
Distill 138 g. Methanol
(5) 62.8 g. K2CO3
Toluene layer
Recovered Toluene 299 g
Azoxystrobin 108.1 g
Methanol ML
Crude product
2x 30 g Methanol wash
Product wet cake Drying
20 g. DMF
(4)
Reaction mass
(7) 350 ml water
100 ml water
1.2 Chemicals reactions with molecular weight stage wise:
Cl O
N N
CO2CH3
+
CN
OH
DABCO in DMF
(E)-methyl 2-[2-(6-chloropyrimidin-4-yloxy)phenyl]-3-methoxyacrylate
2-cyanophenol
Anhy. K2CO3
TolueneDMF
M.W: 320.5M.W: 119
[CPOPMA]
H3CO
N N
O
CH3OCH CO2CH3CN
O
Methyl (E)-2-{2-[6-(2-cyanophenoxy)pyrimidin-4-yloxy]phenyl}-3-methoxyacrylate
AZOXYSTROBIN][
M.W: 403.4 1.3 List of raw materials along with quantity per kg: (consumption norms per kg of product)
Sr.No. Raw materials Consumption kg/kg
1. CPOPMA 0.898
2. 2-Cyanophenol 0.407
3. Toluene 0.333
4. Anhydrous K2CO3 0.581
5. Dimethylformamide 0.277
6. Methanol 0.250
7. 1,4-Diazabicyclo[2.2.2]octane (DABCO) 0.007
1.5 Complete Mass balance per kg Sr. no.
Raw materials Input(kg) Sr. no.
Raw materials Output(kg)
1 Toluene 3.238 1 Recovered Toluene 2.766
2 DMF 0.277 2 Recovered methanol 1.276
3 CPOPMA 0.898 3 Azoxystrobin technical 1.000
4 2-Cyanophenol 0. 407 4 Aqueous ML 5.187
5 K2CO3 0.581 5 Toluene distillation loss 0.472
6 DABCO 0.006 6 Methanol loss during distillation & drying 0.250
7 Methanol 1.526 7 Residue after toluene distillation 0.145
8 Water 4.163
Total 11.096 11.096
1.6 Complete Molecular balance C15H13ClN2O4 + C7H5ON --- C22H17N3O5 + HCl
ATUL LIMITED
Name of Product: Trans-4-MCHI
1. Lab Process details:
Brief process and flow diagram of process stage wise Step-1: Brief process: p-Cresol was hydrogenated in presence of Raney-Ni at 115-125°C and 10-12 kg pressure.
New Project – Lab Process Details
Flow diagram: Chemicals reactions with molecular weight:
OH
CH3 CH3
OH
MW: 108.14 MW: 114.19
Para Cresol 4-Methyl cyclohexanol
+ 3H2Ra-Ni catalyst
List of raw materials along with quantity per KG:
Sr. No.
Raw Material Qty (kg)
1. Para Cresol 1.081 2. Raney-Ni catalyst (Monarch Kalcat-3063) 0.06486
p-Cresol
Reaction
Filtration
4-Methyl cyclohexanol
Ra-Ni catalyst, H2
Catalyst recovery
Complete Mass balance per KG: Step: I
Input Kg Output Kg P-Cresol 1.081 Pure 4-Methyl cyclohexyanol 1.0 Ra-Ni catalyst [MONARCH KALCAT-3063]
0.06486
Ra-Ni catalyst wet cake 0.08648
Hydrogen gas -- Water from distillation of crude 4-Methyl cyclohexanol
0.054
Total Input 1.145 Total Output 1.140 Input – Output = 1.145 – 1.140 = 0.005 Kg loss
Step-2: Brief process: 4-Methyl cyclohexanol reacted with sodium hypochlorite and acetic acid at <0°C. Flow diagram: Chemicals reactions with molecular weight:
CH3
OH
MW: 114.19
4-Methyl cyclohexanol
+
CH3
O
MW: 112.17
4-Methyl cyclohexanone
NaOCl + +NaCl H2OCH3COOH
MW 74.5 MW 58.5 MW 18
4-Methyl cyclohexanol
Reaction
Isolation
4-Methyl cyclohexanone
NaOCl, AcOH
List of raw materials along with quantity per KG:
Sr. No.
Raw Material Qty (kg)
1. 4-Methyl cyclohexanol 1.06 2. Acetic acid 0.85 3. Sodium hypochlorite solution (~14.3% w/w) 5.69 4. Sodium bisulphite solution (5%) 0.85 5. Caustic lye (48%) 0.765 6. 10% Brine solution 1.06
Complete Mass balance per KG: Step:II
Input Kg Output Kg 4-Methyl cyclohexanol 1.063 Crude 4-Methyl cyclohexanone 1.00 Glacial acetic acid 0.853 Aqueous layer 9.11 Sodium hypochlorite 14.3w/w solution 5.690 Sodium bisulphate 5% solution 0.851 Caustic lye 48%w/w 0.765 10% Brine solution 1.063 Total Input 10.27 Total Output 10.11
Input – Output = 10.27 – 10.11 = 0.17 kg loss Step-3: Brief process: 4-Methyl cyclohexanone reacted with hydroxylamine hydro chloride in presence of caustic lye at 70-75°C. Flow diagram:
Reaction
Isolation
4-Methyl cyclohexanone oxime
NH2OH.HCl, NaOH
4-Methyl cyclohexanone
Chemicals reactions with molecular weight:
CH3
NOH
MW: 127.18
4-Methyl cyclohexanone oxime
NaOH + +NaCl
CH3
O
MW: 112.17
4-Methyl cyclohexanone
+ NH2OH.HCl
MW 69.5
MW 58.5 2 H2O
MW 18MW 40
List of raw materials along with quantity per KG:
Sr. No.
Raw Material Qty (kg)
1. 4-Methyl cyclohexanone 1.054 2. Sodium hydroxide 0.801 3. Hydroxyl amine.HCl 0.784 4. Water 6.320
Complete Mass balance per KG: Step:III Input Kg Output Kg 4-Methyl cyclohexanone 1.054 4-Methyl cyclohexanone oxime 1.0 Sodium hydroxide 0.801 Aqueous layer 7.65 Hydroxyl amine.HCl 0.784 Water 6.320 Total Input 8.95 Total Output 8.65
Input – Output = 8.95 – 8.65 = 0.3 kg loss
Step-4: Brief process: 4-Methyl cyclohexanone oxime reacted with sodium metal in n-Butanol followed with con.HCl. Flow diagram:
4-Methyl cyclohexanone oxime
Reactor
Pure 4-MCHA.HCl
n-Butanol
Acetone
Sodium metal
Separation
4-MCHA in Butanol
30% HCl
Butanol Distillation
Crude 4-MCHA.HCl
Acetone
Water Aq. ML
Chemicals reactions with molecular weight:
CH3
NH2.HCl
MW: 149.66
4-Methyl cyclohexylamine.HCl
Butanol MW 74 + +NaOH Butanol
CH3
NOH
MW: 127.18
4-Methyl cyclohexanone oxime
+ HCl MW 36.5
Na
MW 23MW 40 MW 74
List of raw materials along with quantity per KG:
Sr. No.
Raw Material Qty (kg)
1. 4-Methyl cyclohexanone oxime 1.26 2. Sodium metal 1.37 3. n- Butanol 20.5 4. Water 6.35 5. 30 % HCl 1.06 6. Acetone 10.6
Complete Mass balance per KG: Step:IV Input Kg Output Kg 4-Methyl cyclohexanone oxime 1.26 trans 4-methyl Cyclohexyl
Amine 1.0
Sodium metal 1.37 Aqueous layer 6.26 n- Butanol 20.5 Recover Butanol 14.35 Water 6.35 Residue 2.6 30 % HCl 1.06 Recovered Acetone 7.0 Acetone 10.6 Water -butanol 1.94 Total 41.14 Total 33.15
Input – Output = 41.14 – 33.15 = 7.99 kg loss
Step-5: Brief process: Trans -4- MCHA .HCl was taken in solvent (Toluene) and phosgene gas was
passed up to solution become clear at 80-85 o C, followed by distillation of toluene at reduced
pressure to get crude product which was further distilled to get pure T-4-MCHI.
Flow diagram:
T-4-MCHA.HCl Reaction Phosgen
Reaction Mass HCl gas/ Excess of Phosgene
Scrubbed in 10 % Caustic scrubber.
High Vaccum Distillation
Nitrogen Reaction Mass Remove Excess of Phosgene gas
Scrubbed in 10 % Caustic scrubber.
Crude Product
Residue Send to incineration
Toluene
Toluene Recovery To be used in next batch
High Vaccum Distillation
Product
Chemicals reactions with molecular weight:
List of raw materials along with quantity per KG:
Sr. No.
Raw Material Qty (kg)
1. Trans-4-MCHA.HCl 1.162
2. Phosgene 1.744
3. Toluene 4.302
Input kg Output kg
Trans-4-MCHA.HCl 1.162 Trans-4-MCHI 1.00
Phosgene 1.744 Rec. Toluene 4.135
Toluene 4.302 Residue 0.0465
Total 7.208 5.181
Loss:508 gm ( 0.8488 kg HCl and 0.969gm phosgene gas and 0.128 gm toluene)
NH2.HCl
+
NCO
Trans-4-MethylcyclohexylisocyanateC8H13NO
Mol. Wt.: 139.19CAS No:35258-74-1
Trans-4-Methylcyclohexylamine.Hydrochloride
C7H16ClNMol. Wt.: 149.66
CAS No:33483-65-7
COCl2
PhosgeneCCl2O
Mol. Wt.: 99CAS No:75-44-5
+ 3HCl
ATUL LIMITED
Name of Product: RF Resin (Resoform P-20)
1. Lab Process details:
1.1
New Project – Lab Process Details
Brief process and flow diagram of process stage wise
Resorcinol Tar is purified in Acetone. Resorcinol is polymerised with Styrene and purified Tar is added. Which is further polymerised with Formaldehyde in presence of Ethanol and CS Lye. Product is dehydrated by distillation and powerflex oil is added. Finished product is obtained by pastillation.
Purification Hyflo
Resorcinol
Acetone Reso-Tar
Distillation Acetone
Polymerization Water
Pastillation
37% Formaldehyde
Resoform P-20
Ethanol
Styrene Para Toluene Sulfonic Acid
CS Lye
1.2 Chemicals reactions with molecular weight stage wise -
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption /kg
1 Acetone 0.005 2 Reso - Tar 0.045 3 Hyflo 0.008 4 Resorcinol 0.554 5 Formaldehyde 0.241 6 Powerflex Oil 0.010 7 Para toluene sulfonic acid 0.002 8 Styrene 0.352 9 Ethanol 0.015
10 CS Lye 0.001
1.5
S.No.
Complete Mass balance per kg: Input
Input kg Output kg 1 Acetone 0.134 Resoform P-19 1.000 2 Reso - Tar 0.045 Acetone 0.129 3 Hyflo 0.008 Water 0.195 4 Resorcinol 0.554 Acetone loss in Distillation 0.005 5 Formaldehyde 0.241 Water loss in Distillation 0.025 6 Powerflex Oil 0.010 Hyflo 0.008 7 Para toluene sulfonic acid 0.002 8 Styrene 0.352 9 Ethanol 0.015
10 CS Lye 0.001 Total 1.362 Total 1.362
1.6 Complete Molecular balance -
ATUL LIMITED
Name of Product: RF Resin (Resoform P-19)
1. Lab Process details:
1.1
New Project – Lab Process Details
Brief process and flow diagram of process stage wise
Resorcinol Tar is purified in Acetone and Resorcinol is added to Tar and further polymerized with Formaldehyde to get Resoform P-19. Which is dehydrated by distillation and power flex oil is added. Finished product is obtained by Pastillation.
Purification Hyflo
Resorcinol
Acetone Reso-Tar
Distillation Acetone
Polymerization Water
Pastillation
37%Formaldehyde
Resoform P-19
1.2 Chemicals reactions with molecular weight stage wise
-
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption /kg
1 Acetone 0.035 2 Reso - Tar 0.357 3 Hyflo 0.008 4 Resorcinol 0.589 5 37% Formaldehyde 0.292 6 Powerflex Oil 0.010
1.5
S.No.
Complete Mass balance per kg: Input
Input kg Output kg 1 Acetone 0.874 Resoform P-19 1.000 2 Reso - Tar 0.357 Acetone 0.839 3 Hyflo 0.008 Water 0.237 4 Resorcinol 0.589 Acetone loss in Distillation 0.035 5 37% Formaldehyde 0.292 Water loss in Distillation 0.012 6 Powerflex Oil 0.010 Hyflo 0.008 Total 2.131 Total 2.131
1.6 Complete Molecular balance -
ATUL LIMITED
Name of Product: RF Resin (Resoform P-18)
1. Lab Process details:
1.1
New Project – Lab Process Details
Brief process and flow diagram of process stage wise
Resorcinol Tar is purified in Acetone and Resorcinol is added to Tar and further polymerized with Formaldehyde to get Resoform P-18. Which is dehydrated by distillation and power flex oil is added. Finished product is obtained by Pastillation.
1.2 Chemicals reactions with molecular weight stage wise -
Purification Hyflo
Resorcinol
Acetone Reso-Tar
Distillation Acetone
Polymerization Water
Pastillation
Formaldehyde
Resoform P-18
1.3
S.N.
List of raw materials along with quantity per kg
Chemical name Consumption /kg
1 Acetone 0.018 2 Reso - Tar 0.177 3 Hyflo 0.008 4 Resorcinol 0.760 5 Formaldehyde 0.356 6 Powerflex Oil 0.010
1.5
S.No.
Complete Mass balance per kg: Input
Input kg Output kg 1 Acetone 0.442 Resoform P-18 1.000 2 Reso - Tar 0.177 Acetone 0.424 3 Hyflo 0.008 Water 0.288 4 Resorcinol 0.760 Acetone loss in Distillation 0.018 5 Formaldehyde 0.356 Water loss in Distillation 0.015 6 Powerflex Oil 0.010 Hyflo 0.008 Total 1.752 Total 1.752
1.6 Complete Molecular balance -
ATUL LIMITED
New Project – Lab Process Details
Name of Product: 4-Methoxybenzyl chloroformate
1. Lab Process details:
Brief process and flow diagram of process stage wise Brief process: 4-Methoxybenzyl alcohol is added to a mixture of phosgene and methylene chloride and stirred till the reaction is completed. The product is isolated after solvent recovery. Flow diagram:
MDC
Reactor
Reaction mass
Phosgene
4-Methoxybenzyl chloroformate
4-Methoxybenzyl alcohol
MDC recovery
Chemical reaction with molecular weight:
OH
OCH3
4-Methoxybenzyl alcohol 4-Methoxybenzyl chloroformate
MDC
O
OCH3
Cl
O
M. Wt. 138.16 M. Wt. 200.61
Cl Cl
O
+ HCl+Phosgene
M. Wt. 98.9
M. Wt. 36.5
List of raw materials along with quantity per KG
Sr. No.
Raw Material Qty (g)
1. 4-Methoxybenzyl alcohol 0.725 2. Phosgene 0.65 3. MDC 0.24
Complete Mass balance per KG:
Input Kg Output Kg 4-Methoxybenzyl alcohol 0.725 4-Methoxybenzyl chloroformate 1.0 Phosgene 0.65 Recovered MDC 1.36 MDC 1.6 MDC vapor loss 0.24 HCl gas 0.19 Excess phosgene 0.13 Product loss 0.055 Total Input 2.975 Total Output 2.975
Complete Molecular balance: Input Output
4-Methoxybenzyl
alcohol
Phosgene 4-Methoxybenzyl
chloroformate
HCl
gas
Excess
phosgene
Loss (as
4-Methoxybenzyl
chloroformate)
Moles 0.353 0.441 0.335 0.353 0.088 0.018
Mole
Ratio
1.00 1.25 0.949 1.00 0.25 0.051
ATUL LIMITED
Name of Product: N, N- Disuccinimidyl Carnonate
1. Lab Process details:
Brief process and flow diagram of process stage wise : N-Hydroxy Succinimide is reacted with Phosgene in presence of tributyl amine in THF at 0-5°C to give the product. Mass Balance:
New Project – Lab Process Details
N-Hydroxy Succinimide
Phosgene
Tributyl amine
THF
Filter
N,N-Disuccinimidyl Carbonate Recoveries Gases
THF HCl trapped with
Tributyl Amine Tributyl amine
Reaction vessel
0-5°C
Chemicals reactions with molecular weight stage wise. Synthetic Scheme:
N
O
O
OH + Cl
O
Cl + N
CH3
CH3
CH3
Tributyl AmineMol. wt-185.35
PhosgeneMol wt-99
N-Hydroxy SuccinimideMol wt-115.08
THF
0-5 °C
N
O
O
O N
O
O
O
O
N
CH3
CH3
CH3
+ .HCl
N,N-Disuccinimidyl Carbonate
Mol wt-256.17
Tributyl Amine HCl
Mol wt-221.81 List of raw materials along with quantity per KG Raw Materials Quantity (Kg) Recoveries (%) N- Hydroxy Succinimide 1.01 Nil Tributyl Amine 0.19 90 Phosgene 0.55 Nil THF 2.00 80 Complete Mass balance per KG Input Quantities
(kg) Out Put Quantities
(kg) N- Hydroxy Succinimide 1.01 N,N-Disuccinimidyl Carbonate 1.00 Tribtyl Amine 1.875 Tributyl Amine 1.69 Phosgene 0.55 HCl 0.23 THF 10.00 Rec. THF 8.00 Total Input 13.43 Total Output 10.92
Complete Molecular balance - Two moles of N-Hydroxy Succinimide reactes with one mole of Phosgene in presence of two moles of tributyl amine to give one mole of N,N – Disuccinimidyl Carbonate and two moles of tributyl amine HCl.
ATUL LIMITED
Name of Product: HX-13059
1.Lab Process details:
Brief process and flow diagram of process stage wise Step 1: Synthesis of 1-(2,4-dichlorophenyl)-2,4-tiazole-5-one (intermediate A): 2,4-Dichloroaniline is converted to diazonium salt solution which is reduced to 2,4-dichlorophenylhydrazine. This hydrazine on reaction with formaldehyde forms corresponding hydrazone which is cyclized and then oxidized to afford 1-(2,4-dichlorophenyl)-2,4-tiazole-5-one (intermediate A) . Step 2. Synthesis of N-(2,4-difluorophenyl)-N-isopropycarbamoyl chloride (Intermediate B): 2,4-Difluoroaniline reacted with isopropyl bromide to prepare the N-isopropyl -2,4-difluoroaniline. This is further reacted with triphosgene to afford the product N-(2,4-difluorophenyl)-N-isopropycarbamoyl chloride (intermediate-B).
Step 3. (HX-13059) [1-(2,4-dichlorophenyl)-2',4'-difluoro-1,5-dihydro-N-isopropyl-5-oxo-4H-1,2,4-triazole-4-carboxanilide: 1-(2,4-Dichlorophenyl)-1,2,4-traizol-5-one (Intermediate A) is reacted with N-(2,4-difluorophenyl)-N-isopropyl carbamoyl chloride (Intermediate B) in presence of NaOH and TBAB at 95-100 oC. Further purification with Toluene, Hexane and Methanol gives pure [1-(2,4-dichlorophenyl)-2',4'-difluoro-1,5-dihydro-N-isopropyl-5-oxo-4H-1,2,4-triazole-4-carboxanilide (HX-13059). Flow diagram for Int A :
New Project – Lab Process Details
Flow diagram for Int B:
Flow diagram for final HX-13059:
Balanced Chemical Equation:
INTERMEDIATE-A
NH2
Cl
Cl
+
2,4-dichloroaniline
2 HCl NaNO2+
N+
Cl
Cl
N
2,4-dichlorobenzenediazonium chloride
Cl-
+ +NaCl 2 H2O
MW=162.01
MW=72.84 MW=68.99
MW=209.45
MW=58.44 MW=36.02
N+
Cl
Cl
N
2,4-dichlorobenzenediazonium chloride
Cl-
+ 2 NaHSO3
N
Cl
Cl
NH
SO3Na
SO3Na
disodium 1-(2,4-dichlorophenyl)hydrazine-1,2-disulfonate
+ HCl
MW=209.45
MW=208.12
MW=381.12
MW=36.46
N
Cl
Cl
NH
SO3Na
SO3Na
disodium 1-(2,4-dichlorophenyl)hydrazine-1,2-disulfonate
+ 2 H2ONH
Cl
Cl
NH2
(2,4-dichlorophenyl)hydrazine
Na2SO4 H2SO4+ +
MW=381.12
MW=36.02
MW=177.03
MW=142.04 MW=98.07
NH
Cl
Cl
NH2
(2,4-dichlorophenyl)hydrazine
+ H H
O
formaldehyde
NH
Cl
Cl
N CH2
formaldehyde (2,4-dichlorophenyl)hydrazone
H2O+
MW= 177.03
MW=30.02
MW=189.04
MW= 18.01
NH
Cl
Cl
N CH2
+
MW=189.04
formaldehyde (2,4-dichlorophenyl)hydrazone
NaOCN
N
Cl
Cl
NH
NH
O
2-(2,4-dichlorophenyl)-1,2,4-triazolidin-3-one
NaCN+MW=65.00
MW=232.06
MW=49.00
N
Cl
Cl
NH
NH
O
2-(2,4-dichlorophenyl)-1,2,4-triazolidin-3-one
+
MW=232.06
NaOCl
N
Cl
Cl
N
NH
O
2-(2,4-dichlorophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one
MW=74.44+ +
MW=18.01 MW=58.44
MW=230.05
H2O NaCl
INTERMEDIATE-B
NH2
F
F
+CH3
CH3 Br
2-bromopropane
2,4-difluoroaniline
NH
F
F
CH3
CH3
+ HBr
2,4-difluoro-N-(propan-2-yl)anilineMW=129.10
MW=122.99
MW=171.18
MW=80.91
NH
F
F
CH3
CH3
+
2,4-difluoro-N-(propan-2-yl)aniline
MW=171.18
(Cl3CO)2CO
N
F
F
CH3
CH3 Cl
O
(2,4-difluorophenyl)propan-2-ylcarbamic chloride
2 COCl2+ + HCl
MW=233.64
MW=197.82MW=296.74
Triphosgene MW=36.46
FINAL STEP
N
F
F
CH3
CH3 Cl
O
(2,4-difluorophenyl)propan-2-ylcarbamic chloride
MW=233.64
N
Cl
Cl
N
NH
O
2-(2,4-dichlorophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one
+
MW=230.05
Intermediate - A Intermediate - B
N
Cl
Cl
N
N
O
N
F
F
CH3
CH3
O
1-(2,4-dichlorophenyl)-N-(2,4-difluorophenyl)-5-oxo-N-(propan-2-yl)-1,5-dihydro-4H-
1,2,4-triazole-4-carboxamideOR [HX-13059]
+ HCl
MW=427.23
MW=36.46
List of raw materials along with quantity per KG
Sr No Raw Materials Consumption / 1Kg 1 2,4 Dichloroaniline 1.29 2 Toluene 1.29 3 35% HCl 13.875 4 H2O 7.31 5 NaNO2 (98.5%) 0.59 6 Na2SO3 (97%) 2.59 7 H2SO4 (95%) 0.08 8 48%NaOH 9.62 9 t-BUOH 7.96 10 37%HCHO 0.65 11 AcONa 0.03 12 AcOH 0.76 13 90%NaOCN 0.8 14 13%NaClO 3.75 15 Dichloroethane 7.32 Int A first step 1 2,4 Difluro aniline 0.97 2 IPBr 1.02 3 H2O 4 48%NaOH 0.69 5 Hexane 1.28 Int B Second step 1 2,4 Difluro aniline 0.62 2 N-Ipr-2,4 difluro aniline 0.18 3 IPBr 0.72 4 H2O 0.99 5 48%NaOH 0.51 6 Toluene 3.18 7 Triphosgene 0.60 Final HX-13059 step 1 Int A 0.76 2 Toluene 5.70 3 NaOH (96%) 0.13 4 nBu4NBr (98%) 0.20 5 int B 0.76 6 H2O 8.82 7 n-Hexane 0.13 8 MeOH 4.03
List of co-product per KG Complete Mass balance per KG Intermediate A
Process Input Kgs OutPut Kgs DI AZONIUM SALT PREPERATION - 2-4 Di chloro Aniline 1.1 Toln+product layer 10.2 NaNO2 0.5 Water 0.9 toluene 0.5 HCL 2.0 Water 5.1 10.2 Water 8.5 Toluene Layer 0.5 Na2SO3 2.1 Aquous Layer 20.9 H2SO4 0.1 Di Azo Salt 10.2 Total 20.9 Acid Hydrolysis / Product Isolation- aq layer 20.9 HCl (35%) 6.8 Reaction Mass 34.3 Caustic Solution (48%) 6.6 Total 34.3 filteration Reaction Mass 34.3 water wash 8.6 Wet Cake 1.3 Effluent 41.6 Slurry Wash to cake - Water 5.8 Cake 1.3 Cake 1.3 Water waste 9.5 Hydrazone Preperation Cyclization- Cake 1.3 Tert - Butanol 5.8 Water 6.4 Reaction Mass 20.6 37%HCHO 0.5 Sodium Acetate Acetic Acid Water 0.1 Sodium Cynate 0.7 Acetic Acid 0.6 Water 0.6 Cyclization 13% Hypochlorite Solution 3.4 NaOH flakes 0.5 Water 0.5
20.6 EDC Wash - Product Slurry 20.6 Tert Butanol Rec Tert Butanol 5.8 Distillation Residue 14.8 EDC extraction Distillation Residue 14.8 Aquous Layer 14.8 EDC Wash 1 3.0 EDC Wash 6.1 Intermediate A - Isolation - Aqueous Layer 14.8 HCl 2.6 Product Slurry 19.9 Water 2.6 Total 19.9 Product Slurry 19.9 Intermediate A 1 Water wash 1.3 Water 20.9
Intermediate B
Steps Reactants Kgs Output Kgs
Isopropylation 2,4-difluro aniline 0.57 Aq Layer 1.56
N-isopropyl -2,4-difluroaniline (91.75%)
0.17 Toluene layer 2.98
IPrBr 0.65 H2O 0.90 50% NaOH 0.46 Toluene 1.80 4.55 H2O 0.90 Aq layer 0.91 H2O 0.90 Aq layer 0.91 Toluene layer 2.96 Azeotropic distillation
Toluene laye r 887 H20 0.01
Phosgenation Triphosgene solution
Toluene rec 2.72 Triphosgene 0.55 Toluene 1.09 Toluene laye r 2.94 Distillation Product 1.00
HX-13059
Input Kgs OutPut Kgs
Toluene 3.810 Toln+product layer 4.833
1-(2-4-Dichlorophenyl) -5-one 0.694 Water(Azeotropic
Distillation) 0.129
Catlyst 0.189 96% NaOH 0.129 Water 0.129 4.961 Toluene 0.365 Int B solution 1.099 Int B 0.732 Toluene+ Int A 4.549 Reaction mass 5.647
N-(2,4-difluorophenyl)- chloride 1.099
Total 5.647 Reaction Mass 5.647 Toluene layer 5.427 water wash 5.139 water wash 5.138 Product 1.243 Slurry 8.090 Methanol 6.347 Toluene 0.250 Hexane 0.250 Slurry 8.090 Wet Cake 9.534
Water wash from R-201 2.550 Filtrate +Wash ML 6.847
Wet Cake 1.110 HX 13059 1.000 water Recovery 0.110
ATUL LIMITED (Corporate SHE Dept.)
Division: R & D -PI
Name of Product: Di-t-butyl dicrbonate
1. Lab Process details:
Brief process: Solid Sodium-t-butoxide is reacted with gaseous carbon dioxide in a gas-solid phase reaction to obtain the corresponding carbonate salt. This carbonate salt is treated with phosgene and then triethyl amine to obtain the final product DIBOC or Boc. anhydride.
DI-TERT-BUTYL DICARBONATE (Boc. anhydride)
Date:
Flow diagram:
STAGE-I: Carbonylation of t-Butoxide (NaTBC)
STAGE-II: Di-t-butyl carbonate from NaT
5. Addition Time: 2h
4. Ethyl acetate (130 ml)
1. Ethyl acetate (200 ml)
2. Phosgene (35 g)
3. Na TBC (100 g)
1. Na-t-butoxide (100 g)
2. CO2 gas (45.88 g) 10L/min
6. Triethyl amine (130 ml)
11. Ethyl acetate (25 ml x 4)
8. Hyflo ( 100 ml)
Autoclave <50°C
19-20 hPress: 2 Kg/cm2
Na-TBC (Yield: 96.5 %)
PhosgenationTemp: -5-0°C
Time: 1 h
16. Crude (52.5 g)
PhosgenationTemp: -5-0°CTime: 30 min7. 25-30°CTime: 1 h
9. Filtration10. Org layer12. Washing ML
14. DistillationVac: 80-90 mmHg
Mass Temp: 40-45°CBath Temp: 50°C
13. Residue
15. Recovered Ethyl acetate (54 %)
17. Distillation18. Vac: 15 mmHgMass Temp: 40-45°C
Bath Temp: 50°C20. Vac: 1.2 mBarBath Temp: 75°C
19. Recovered Ethyl acetate
21. Distillate (As DIBOC)39 gYield: 50 % from NaTBCOverall Yield: 48.2 %
22. Residue (< 1 g)
Chemicals reactions:
Stage-I
+ CO2O O
Na
O
ONa
M.Wt 96 44 140
Stage-II
O ONa
O+ COCl2
O O
O
O O
O O+ 2 NaCl
M.Wt 140 99 262
O O
O
O O
O O
O O
O
O
O
TEA + CO2
M.Wt 262 218
Raw Material: Sr. No Raw Material Qty/Kg
1 Sodium-t-butoxide 1.82 2 Carbon dioxide gas 0.835 3 Ethyl acetate 2.05 4 Phosgene 0.89 5 Triethyl amine 0.34 6 Hyflo supercel 0.256
Complete Mass balance per KG: Input Kg Output Kg Stage-I Sodium-t-butoxide 1.82 Sodium-t-butyl carbonate 2.58 Carbon dioxide gas 0.835 Total 2.655 2.58 Stage-II Sodium-t-butyl carbonate 2.58 Crude DIBOC 0.955 Phosgene 0.89 Recovered ethyl acetate 5.23 Kg Ethyl acetate 9.87 Triethyl amine 0.33 Dist. DIBOC 1 Hyflo 0.258 Total 13.93 7.18
Annexure – 3 Google map of ATUL LTD.
Annexure – 3 Google map of ATUL LTD.
Annexure – 4 Location map of ATUL LTD.
WATER (KL/DAY) BALANCE DIAGRAM (EXISTING)
RAW WATER 22569
DOMESTIC 937
INDUSTRIAL 21632
PROCESS16376
BOILER1170
COOLING2735
WASHING1351
PROCESS17403
BOILER805
WASHING1305
COOLING1944
Treated effluent discharged through Closed 4 km length pipeline
to tidal zone of river par
EFFLUENT21377
NORMALEFFLUENT
17283
High COD eff. To Incinerator
23
LOSS 791
TO EFFLUENT TREATMENT
PLANT
GARDEN 0
Septic tank/Soak pit
937
LOSS 365 LOSS 46
High TDS effluent to MEE
97
Water with Chemical 1027
WATER (KL/DAY) BALANCE DIAGRAM (PROPOSED)
RAW WATER 5788.70
DOMESTIC 2
INDUSTRIAL 5786.70
PROCESS1281.70
BOILER1958
COOLING2047
WASHING500
PROCESS1515.03
BOILER626
WASHING500
COOLING400
EFFLUENT1684.51
NORMALEFFLUENT
158.51
High COD eff. To Incinerator
57.57
LOSS 1647
TO EFFLUENT TREATMENT
PLANT
GARDEN 0
Septic tank/Soak pit
2
Water with Chemical 233.33 LOSS 1332 LOSS 0
High COD eff. To MEE
1298.95
Treated effluent discharged through Closed 4 km length pipeline
to tidal zone of river par
CHEMICAL SLUDGE
SUPERNATE RECYCLE
WASTE WATER FROM ATUL BIOSCIENCE LTD.
SLUDGE
GUARD POND
BIO-REACTORS (2 NOS.)
SURFACE AERATORS
WASTE WATER FROM ATUL PLANTS
MIXING CHAMBER (Hook Up Chamber)
ON LINE LIME SLURRY IN CHANNEL EQUALIZATION TANKS
(Pond No. 1, 3, 4) FLOCCULANTS /COAGGULANTS
HOLDING TANK
RECYCLE
CLARIFIER TANKS
TREATED EFFLUENT DISCHARGED TO PAR ESTUARY THROUGH 4 km PIPELINE
BLOCK DIAGRAM OF EFFLUENT TREATMENT PLANT
SLUDGE THIKENER
DISPOSAL / LANDFILL
PRIMARY CLARIFIER
NUTRIENTS
SLUDE DEWATERING BELT PRESS/
SLUDGE DRYING BEDS FILTRATE RECYCLE
PULSATOR (POLISHING TANK)
Annexure – 6 SCHEMATIC FLOW DIAGRAM OF EXISTING ETP
Annexure – 7 LOCATION OF FINAL DISCHARGE POINT OF TREATED EFFLUENT THROUGH PIPELINE IN RIVER PAR
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