Professional Documents
Culture Documents
c) Justification :-
Scale-up of Clothianidin manufacturing process from scale-up (3 Liter) to P2 Pilot plant 100 ltr) to validate process, data generation
for plant scale expansion, effluent treatibility study & solvent recovery/recycling validation.
Reviewed By Approved By
Signature
Name
Date
Copy To : a) HO b) Site
Page No. :- 02 of 02
N ASSETS
ata generation
Authorised By
NDG
Approved By
Mass Balance of CTZ Stage-1
Updated In reference
Admin: of provided BFD of step-1 Ver 03 from R&D Operating Condition
Don't change values other
FACTOR 9.0 Kg than ''B3'' to
of MNG get outputs.
(99.30% Purity) Temperature Pressure/
Sheet M.B. is linked with °C Vacuum
BCT sheet.
MNG 9.00
37% HCHO 13.51
Toluene 17.87
Water 0.48
Charging RT ATM
40.9
Dropwise Addition
40% MeNH2 6.234 at 35-46°C & 35-46°C ATM
Heating to 50°C
47.1
Cooking for 3 Hrs 1) Sample will be withdraw through bottom. 50±1°C ATM
47.1 Sample Analysis: MNG NMT 1.0%
Rxn Mass Nature : Creamish Slurry
18.3885
DMF 49.77 Bypass Circulation RT ATM
64.07
% of MNMTI 19.94
DMF+ MNMTI
RT ATM
solution
64.07 SP.GR : 0.97635
Toluene content? 65.62 LTR
DMF
23.85 Filtration 40±1°C ATM
Washing
131 Drying Dist.DMF 3 90-105°C Vacuum
21 B.D. loose: 0.7224
B.D. Pack:0.86
Filtrate ML
107.9 Waste to TSDF
Sp.Gr. 0.9669 111.58 17 B.D. loose: 0.6467
LTR B.D. Pack:0.8084
Dry CTMT
1.276
Residue 30°C ATM
5.164
Total Dry CTMT
19.048
CTMT 19.0
Water 91.95
Charging 30°C ATM
111
30-36°C ATM
35% HCl aq. 15.74 Dropwise addition After 30% HCl addition rxn mass become clear orange colur
127 solution
127
Water
67.45 Filtration Filtrate ML-1 102.69 10°C ATM
washing-01
Hot Water
24.50 218.69 Wash treatment yet to be decided
washing-2
Loose B.D.: 0.5090 Filtrate ML-2 89.29
Packed B.D.: 0.6207
Avg. B.D.: 0.56485 Wet CTZ
18.31
calculate time
calculate time
confirm time
Excel Crop Care Limited, Bhavnagar
New Pilot Plant
Equipment List for CTZ
Sr. Tag No. Operation MOC Capacity Location Available/ Maximum Cost of Remarks
No. New Batch Vol. new
(lit) equipme
nt
STEP-1
1 RB-801 Step-1 reaction vessel MSGL 100 ltr S.F Available 73 0 Minimum stirrable vol. : 10 lit
2 RB-801 Turbine agitator for MSGL 100 ltr vessel MSGL 100 ltr S.F Available - 0
3 P-802 Toluene transfer from drum to T-802 bx tank PP/PVDF 25 NB-AODD G.F. Available 0 PVDF is compatible with toluene
4 T-802 Toluene Batch tank SS-316 100 ltr T.F. Available 0 SS316 is compatible with toluene
5 H-1 Portable Hopper for MNG charging SS-316 80 NB-Dia S.F Available 0
6 P-817 Paristaltic pump for 37% HCHO addition SS-316 Body 100 ltr/Hr S.F Available 0
7 NEW Diaphragm pump for 40% MMA addition SS-316 Body 30 LPH S.F New 0.75 Addition time change to 20 min instead of
3 hours.
Exisiting Pump is of 5LPH capacity
whichneedsreplacement with 30LPH
Capacity. Addition qty. 7 Ltr in 20 Min.
8 T-811 Reflux pot for Dist Water separation SS-316 50 ltr S.F Available 0
9 T-1111 Ejector tank MS - G.F. Available 0
10 P-1111 Ejector pump CI - G.F. Available 0
11 T-1205 Buffer tank for ejector SS-316 - S.F Available 0
T-1204 Water pot SS-316 200 ltr S.F Available 0
P-803 For MNMTI DOM Filtration SS-316 25 NB-AODD F.F Available 0 Dom Batch
F-807 DOM filter for MNMTI Filtration SS-316 600 Dia T.F. Available 0 Wet Basis Cake Volm. is 23 Ltr 28 23
Working Capcity of Dom Filter is 28 Ltr
T-805 Filtrate Ml collection tank SS-316 200 ltr G.F. Available 47 0 Combine 3-4 Batches ML can be proceed to
distillation
P-804 Filtrate ml transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
T-807 MNMTI Solution collection tank SS-316 160 ltr G.F. Available 53 0
P-807 MNMTI Solution transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
- Load cell for DMF, MNMTI solution collection tank T- CI 1.5 Ton G.F. Available 0
807
STEP-2
R-802 Step-2 reaction vessel MSGL 250 ltr S.F Available 100 0 Min. Stirrable vol. 40 Ltr
Fresh DMF transfer from drum to R-802 SS-316 25 NB-AODD G.F. Available 0 Confirm Tag No.
pump
T-815 DMF Batch tank SS-316 200 ltr T.F. Available 40 0
- Reflux pot for cleaning to ensure moisture free SS-316 20 S.F Available 0
vessel
- Portable Hopper for K2CO3 & Cat-30149 charging SS-316 80 NB-Dia S.F Available 0
- CCMT + DMF Solution preparation tank Solution preparation to be decided with
R&D
Paristaltic pump for CCMT addition SS-316 Body S.F Available 0 Addition qty. 26 Ltr in 60 Min.
Required Capacity :- 433 ml/min
Existing Electrolab Pump will give required
capacity with Tube size of 5*8 with 100
RPM
Pump for waste solid DOM Filtration & MNMTI SS-316 25 NB-AODD F.F Available 0 Confirm Tag No. Dom Batch
solution circulation pump
F-1202 DOM filter for waste solid Filtration SS-316 900 Dia T.F. Available 0 Wet Basis Cake Volm. is 29 Ltr 64 29
Working Capcity of Dom Filter is 64 Ltr
T-809 Filtrate ml collection tank MSGL 160 ltr G.F. Available 112 0
P-808 Filtrate ml transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
ATFE for distillation (60% Concentration) Available 0 ATFE to be installed in plant 20
Vent Condenser of R-802 R-802 Vent Condenser can be used for
ATFE Vapour Condensation or Explore new.
R-802 Max. Operating Temp is 40 °C.
Solvent- DMF & Addition of CCMT
Vessel for concentrate mass collection 63 LIT F.F New 5 Vessel to be find out after 60% Concentration : ~40 lit 60
concentration mass transfer pump New 1 Pump to Find out
WFE for distillation(90% Concentration) SS-316 0.4 sq. mtr S.F Available 0 With Internal Condenser after 90% Concentration : ~24 lit
External Condenser of WFE SS-316
R-803 Vessel for concentrate mass collection SS-316 200 ltr F.F Available 63 0 Min. Stirrable vol. 35 Ltr, As per batch size
Min. operating vol. is 20 Ltr
Vent Condenser of R-803 Graphite F.F Available
29 P-816 Intal Vaccum pump for distillation SS-316 50 m3/hr G.F. Available 0
30 NA Buffer tank SS-316 100 ltr S.F Available 0
31 T-806 Dist DMF collection tank SS-316 100 ltr G.F. Available 80 0 Storage of 1 Batch volume
32 P-804 Dist.DMF transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
P-801 CMD-90 Transfering pump PP/PVDF 25 NB-AODD G.F. Available 0 Compatibility to be checked
T- CMD-90 Batch tank NEW
Confirm route for feeding with R&D
P- AODD PUMP for filter transfer NEW
F-801 ANFD filter for CTMT Filtration & Drying SS-316 0.25M2 G.F. Available 0
T-812 Filter ml collection tank SS-316 200 ltr G.F. Available 60 0 Combine 3 Batch vol. will proceed for crude
CTMT Recovery
P-810 Filter ml transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
STEP-2 Crude CTMT Recovery
R-803 Vessel for concentrate mass collection SS-316 200 ltr F.F Available 180 0 Chilled brine required
Condenser
P-816 Ital Vaccum pump for distillation SS-316 50 m3/hr G.F. Available 0
NA Buffer tank SS-316 100 ltr S.F Available 0
T-806 Dist CMD-90 collection tank SS-316 100 ltr G.F. Available 105 0
P-804 Dist.CMD-90 transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
P- AODD PUMP for filter transfer NEW
F-801 ANFD filter for CTMT Filtration & Drying SS-316 0.25M2 G.F. Available 0 Max. Batch Dry qty. 5 KGs
T-812 Filter ml collection tank SS-316 200 ltr G.F. Available 40 0
P-810 Filter ml transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
STEP-3
R-802 Step-3 reaction vessel MSGL 250 ltr S.F Available 122 0
Water batch tank Available 91
Portable Hopper for CTMT charging SS-316 S.F Available
R-801 Used as batch tank for HCl MSGL 63 ltr T.F. Available 15 0 Charging of HCL in R-801 discuss with R&D
NA Pump for crude CTZ DOM Filtration PP/PVDF 25 NB-AODD G.F. Available 0 Dom Batch
F-1201 Dom Filter for Crude CTZ Filtration Rubber Line 900 Dia T.F. Available 0 Wet Basis Cake Volm. is 30 Ltr 64 30
Working Capcity of Dom Filter is 64 Ltr
35 NA Filter ml collection tank MSGL 250 ltr G.F. Available 200 0
36 P-806 Filter ml transfering pump SS-316 1 m3/Hr F.F Available 0
Repulping of Crude CTZ
37 R-802 Repulping Vessel MSGL 250 ltr S.F Available 87 0
38 Water batch tank Available
39 Portable Hopper for CTMT charging SS-316 S.F Available
40 NA Pump for crude CTZ Filtration PP/PVDF 25 NB-AODD G.F. Available 0
41 F-801 ANFD filter for CTMT Filtration & Drying SS-316 0.25M2 G.F. Available 0 pH data to be checked.
Wet Basis Cake Volm. is 20 Ltr
Working Capcity of Dom Filter is 37 Ltr
T-812 Filter ml collection tank SS-316 200 ltr G.F. Available 80 0 Filtrate ML -1+2+3 Combine or Separate
store
P-810 Filter ml transfering pump PP/PVDF 1 m3/Hr G.F. Available 0
DMF Solvent recovery
V-108 with fractional distillation column setup
6.8 Rs. In Lakh
Basis:-
1. Crude recovery batches considered in CTMT Process Setup
2. Step-3 CTZ process consider after completion of CTMT campaing in same setp
3. Equipment Toluene & CMD-90 recovery not considered
4. DMF Fractionation/ Redistillation Facility to be explored
Excel Crop Care Ltd.
Projcet:CTZ
Admin:
Task: BCT (Option-5A)(Purification of Step-2 using CMD introduced) NO OF MONTHS FOR
PRODUCTION
Batch Output 1.000 TPB
Plant capacity Err:520 TPD
Admin:
Plant capacity Err:520 TPM 24HRS WORKING & 26
Plant capacity Err:520 50 TPA WORKING DAYS & 11
MONTHS WORKING.
Plant capacity Err:520 200 TPA
Stage-1
Batch input kg 9 Admin:
dont change value here
Batch Volume Equipment working Equipment
Sr.No. Activity (sheet linked with Time,Hrs
MB sheet) volume Occupancy %
Stage-2
Batch Volume
Equipment working Equipment
Sr.No. Activity (sheet linked with
MB sheet) volume Occupancy %
Stage -2 Salt Filtration & Drying (Dom Filter, SS-316, 900 Dia)
Filter Area Required 900.0 mm
1 Nos.
1 Innertisation with N2 0.25
2 Receiving of mass & Filtration 135 10
3 DMF washing & filtration 160 1.25
4 Wet Cake (B.D-0.7224, LOD-20%) 29 63.585 45 10
5 Scrapping & unloading, boxup 29 1.5
Cake volume 29 23
Capacity Per Filter, TPD 1.04
No. of Filters for the step,Nos. 1.0
Sectional Capacity, TPD 1.043
Capacity, TPM 29.2
Stage-2 Product Concentration & Dissolution Vessel (NEW/SS316/5KL) With FF Reboiler -500kg/hr X 01 Nos
Vessel Volume Required 112 Ltr
Vessel Considered with FF Reboiler 5KL/15m2 X 01 NOS
1 Innertisation with N2 0.25
2 Fitrate ml recieving lot-1 112 70 0.5
3 Heating to75 to 85°C 112 70 1.75
8 Cooling to RT 21 13 1
9 CMD-90 charging 42 26 0.5
10 Heat to 70C 42 26 1
Stirring for 30 min 42 26 0.5
Cool to 28C 42 26 1
11 Charge feeding for filtration 42 26 1
Maximum batch volume as per real 112 LTR 70 20.5
R&D density data
Capacity Per Reactor, TPD 1.17
No. of Vessels for the step,Nos. 1
Sectional Capacity, TPD 1.170
Capacity, TPM 32.8
Stage -2 CTMT Filtration & Drying (ANFD/0.25 M2)
Filter Area Required 4.4 m2
1 Nos.
1 Innertisation with N2 0.25
2 Receiving of mass & Filtration 42 8
3 CMD-90 washing & filtration 63 1.25
38
4 Wet Cake (B.D-0.7224, LOD-20%) 38 8
5 Scrapping & unloading, boxup 38 1.5
Cake volume 38 LTR 19
Capacity Per Filter, TPD 1.26
No. of Filters for the step,Nos. 1.0
Sectional Capacity, TPD 1.3
Capacity, TPM 35.4
Crude CTMT recovery (NEW/SS316/5KL) X 01NO
Vessel Volume Required 58 Ltr
Vessel Considered with FF Reboiler 5KL/15m2 X 01 NOS
1 Innertisation with N2 0.25
2 Fitrate ml recieving 58 23 0.5
3 Heating to70 to 80°C 58 23 1.75
CMD-90 Vacuum Distillation at 70 to
4 58 250 23 6
80°C
6 Cooling & Crystallization at 5-6°C 10 4 11
7 Charge feeding for filtration 10 4 1
Maximum batch volume as per real 58 LTR 23 20.5
R&D density data
Capacity Per Reactor, TPD 1.17
No. of Vessels for the step,Nos. 1
Sectional Capacity, TPD 1.2
Capacity, TPM 32.8
Crude CTMT Filtration & Drying (ANFD/NEW/1.5M2)
Filter Area Required 0.3 m2
1 Nos.
1 Innertisation with N2 0.25
2 Receiving of mass & Filtration 10 4
3 CMD-90 washing & filtration 13 1.25
38
4 Wet Cake (B.D-0.479, LOD-%) 3 7 4
5 Scrapping & unloading, boxup 3 1.5
Cake volume 3 11
Capacity Per Filter, TPD 2.18
No. of Filters for the step,Nos. 1.0
Sectional Capacity, TPD 2.2
Capacity, TPM 61.1
DMF Redistillation ( )
Batch volume 79 Kg
Volume per day to be distilled 79 Kg
1 Innertisation with N2 0.25
2 Dist. DMF Recieving 79 #DIV/0! 1
3 Heating to 95-105°C 79 #DIV/0! 1
Capacity of column,Kg/Hr 3
No. of columns for the step,Nos. 1
Sectional Capacity, TPD 2.0
Capacity, TPM 56.0
Stage-3
Batch Volume
Sr.No. Activity (sheet linked with Equipment working Equipment
MB sheet) volume Occupancy %
Note: 1) Filtrate ml of 3 no. of batches considered collectively for crude CTMT recovery.
2) One batch Equivalent wet cake quantity of crude CTMT will be make up with Step-3
Admin:
NO OF MONTHS FOR
PRODUCTION
Admin:
24HRS WORKING & 26
WORKING DAYS & 11
MONTHS WORKING.
Admin:
dont change value here
Excel Crop Care Limited., Bhavnagar 04.10.2018
Tentative Project costing for Pilot trials of CTZ in new Pilot Plant (P-2 Plant)
(Rs. Lakh)
2 Process side piping modification mtr Estimated cost. 100 mtr new piping, 200 mtr
re-route
3 Utility piping modification mtr Estimated for Hot water, CHW, N2 & LPS line
up considered.
4 Structural work 5 T Shed extension on T.F. for dom filter
installation.
5 Electrification & Instrumentation 0.5 Estimated cost.
4 Khalasi work, insulation and others - - 0.5
7 Civil Work 0.3
8 Contingency (10%) 0.1
Grand Total : In Lakh 1.4 Say Rs. 15.0 Lakh
Line List & Piping MTO
Line Duty Pipe, m Bend Stubend Flange Valve DW S.G
Stage-1
Process piping 25 NB SS
1 210 50 80 80 25 5
Unit Cost 600 120 60 85 3000 3000
Total Cost 126000 6000 4800 6800 75000 15000 233600
2 Utility piping 25 NB MS 85 20 30 30 10 2
Unit Cost 350 95 45 85 2000 2000
Total Cost 29750 1900 1350 2550 20000 4000 59550
Process piping 40 NB SS
3 65 15 25 25 10 3
Unit Cost 800 150 80 110 3500 3500
Total Cost 52000 2250 2000 2750 35000 10500 104500
397650
Details of Tentative Project costing for Pilot trials of CTZ in new Pilot Plant (P-2 Plant)
RB-801
1 Toluene charging line-up (25 NB SS) 15 mtr
2 CHW supply/return line-up (25 NB MS) 10 mtr
3 Utility hot water supply return line-up ( 25 NB MS) 20 mtr
4 Reflux pot line-up (25 NB SS) 10 mtr
5 DOM filter line-up (40 NB SS) 25 mtr
6 Filtrate ml circulation line-up (25 NB SS) 15 mtr
R-802
7 DMF Charging line-up (25 NB SS) 10 mtr
8 DMF circulation line-up throgh funda filter (25 NB SS) 15 mtr
9 Utility hot water supply/return line-up ( 25 NB MS) 15 mtr
10 Reflux pot line-up (25 NB SS) 15 mtr
11 DOM filter line-up (40 NB SS) 25 mtr
12 Filtrate ml line-up upto R-803 (25 NB SS) 15 mtr
R-803
13 Methanol Charging line-up (25 NB SS) 10 mtr
14 Conc. Mass transfering line-up (25 NB SS) 15 mtr
15 30%HCl line-up from R-801 to R-802 (25 NB SS) 10 mtr
16 CHW utility line-up ( 25 NB MS) 10 mtr
17 DOM filter line-up (25 NB SS) 20 mtr
18 Filtrate ml collection line-up (25 NB SS) 15 mtr
19 R-802 to ANFD line-up (40 NB SS) 15 mtr
20 ANFD ml transfering line-up (25 NB SS) 15 mtr
Misscellaneous
21 N2 Piping to vessel/tank (25 NB MS) 20 mtr
22 Piping for solvent recovery process (25 NB SS) 30 mtr
23 LPS Line modification if required. (25 NB MS) 10 mtr
24 Accessories like Scoop, measuring bucket (SS/Planstic) Mugs, - -
Carboys
25 SS-316 Hose pipe 2 EU
26 PTFE Hose pipe 2 EU
27 Safety accessories like safety guard, Earthing rod, earthing - -
wire, PPES
Hopper & Pot
1 Portable hopper without valve for MNG charging 1 EU
2 Portable hopper for K2CO3 1 EU
3 Reflux pot of 20 lit 1 EU
Total
1 25 NB SS Line 210 mtr
2 25 NB MS Line 85 mtr
3 40 NB SS Line 65 mtr
Excel Crop Care Limited, Bhavnagar
New Pilot Plant
Equipment List for CTZ
Sr. Tag No. Operation MOC Capacity Location Available/ Cost of Remarks
No. New new
equipme
nt
18 NEW Reflux pot for cleaning to ensure moisture free SS-316 20 lit S.F New 0.05
vessel R-802
19 NEW Paristaltic pump for CCMT addition SS-316 Body - S.F New 0.75 Capacity of pump will be
decided after finalised
addition time.
20 P-820 Pump for waste solid DOM Filtration & MNMTI SS-316 25 NB-Dozing F.F New 0.75
solution circulation pump
21 F-1202 DOM filter for waste solid Filtration SS-316 900 Dia T.F. Available 0
22 T-809 Filtrate ml collection tank MSGL 160 ltr G.F. Available 0
23 P-805 Filtrate ml transfering pump SS-316 1 m3/Hr G.F. Available 0
24 R-803 Vessel for Vacuum distillation SS-316 200 ltr F.F Available 0
25 P-816 Intal Vaccum pump for distillation SS-316 50 m3/hr G.F. Available 0
26 NA Buffer tank SS-316 100 ltr S.F Available 0
27 T-806 Dist DMF collection tank SS-316 100 ltr G.F. Available 0
28 P-812 Dist.DMF transfering pump SS-316 1 m3/Hr G.F. Available 0
29 P-802 Methanol Transfering pump PP/PVDF 25 NB-AODD G.F. Available 0
30 P-3 Concentrated CTMT solution transfering pump SS-316 1 m3/Hr G.F. Available 0
31 R-801 Used as batch tank for HCl MSGL 63 ltr T.F. Available 0
32 F-1201 Dom Filter for Crude CTZ Filtration Line 900 Dia T.F. Available 0
33 NA Filter ml collection tank MSGL 250 ltr G.F. Available 0
34 P-810 Filter ml transfering pump SS-316 1 m3/Hr F.F Available 0
35 F-801 ANFD filter for CTZ Filtration & Drying SS-316 0.25M2 G.F. Available 0
36 T-812 Filter ml collection tank SS-316 200 ltr G.F. Available 0
37 P-811 Filter ml transfering pump SS-316 1 m3/Hr G.F. Available 0
3.1 Rs. In Lakh
Tank Volume details for CTZ Campaign
Note : Calibration of all tank done. T-806 will be used for dist. DMF collection. Drum up will be done in between ope
Max volume on LI
lit
100
130
150
270
210
120
190
250
Stage-1
LMTD 3 °C
Stage-2 Part-1
Stage-2 Part-2
LMTD 3.04 °C