Demo Expt Summary

EXCEL CROP CARE LIMITED ,BHAVNAGAR

AZOXYSTROBIN DEVELOPMENT ACTIVITY

Azoxystrobin synthesis ( Water quenching and Crystallization without use of methanol)

Experiment No. UNIT 183 185 188 193 195

Date 13/06/16 16/06/16 20/06/16 25/06/16 27/06/16
CHARGE SIZE Kmol 0.312 0.78 0.78 0.78 0.312
MCPPMA gms 100 250 250 250 100
%PURITY BY AREA % 98.51 98.51 98.51 98.51 98.51
100% MCPPMA gms 98.51 246.3 246.3 246.3 98.5
Moles 0.31 0.77 0.77 0.77 0.31
Molar ratio 1 1 1 1 1
OCP gms 38.12 95.3 95.3 95.3 38.12
%PURITY BY AREA % 99.66 99.66 99.66 99.66 99.66
100% OCP gms 37.99 94.98 94.98 94.98 37.99
Moles 0.32 0.80 0.80 0.80 0.32
Molar ratio 1.039 1.039 1.039 1.039 1.039
Potassium Carbonate (PC) gms 65.35 163.37 163.37 163.37 65.35
Purity % 98 98 98 98 98
100% PC gms 64.043 160.1026 160.1026 160.1026 64.043
Moles 0.464 1.160 1.160 1.160 0.464
Molar ratio 1.510 1.510 1.510 1.510 1.510
Catalyst-4030 gms 1 2.5 2.5 2.5 1
% Catalyst base on MCPPMA %
DMA gms 150 375 375 375 150
%MOIST % -- -- -- 0.4 --
100% Azoxystrobin ( Weight Base ) gms 125.74 314.35 314.35 314.35 125.74
100% Azoxystrobin ( Purity Base ) gms 123.87 309.67 309.67 309.67 123.87
ALL RAW MATERIAL INITIALLY
REACTION PARAMETERS
Reaction Temp. °C 100 100 100 100 100
Reaction Time HRS 6 6 6 6 6
RESULT OF REACTION MASS
After 6.0 hrs
MCPPMA % 0.13 0.06 0.11 0.16 0.12
OCP % Nd 0.24 0.87 0.27 ND
AZOXY % 96.76 96.83 96.14 95.98 96.42
Other % 0.91 0.87 0.92 -- --
Salt filtration
Reaction mass 351.5 882 883 878.5 351.5
DMF wash to salt gms 161 402.5 402.5 402.5 161
Filtrate organic mass gms 412.5 1005 1038.5 1051 407
Wet salt gms 77.66 255 215 206 85.4
Water Quenching and Recrystallization
Filtrate organic mass gms 412.5 1005 1038.5 1051 407
DM water gms 311 777.5 777.5 777.5 311
DM water addition Temperature °C 70 75 70 70 70
DM water addition Time HRS 2 2.5 2 2 2
Time For Atmoshpheric from 70°C to 48°C HRS 2.15 2 2 2 2
Time For Temerature decrease from 48°C to 1.5 1.5 1 1 1
HRS
15°C
Filtration of Azoxy Crystal Sluury
DM Water used for Washing gms 100 500 500 500 200
Filtrate ML after Filtration gms 544 1332 1421 563
1700
1st Water Washing ML after washing gms 96 264 114.5
503.24
2nd Water Washing ML after washing gms -- 244.5 244 101
Wet Azopxystrobin 125 324.5 323.5 361.5 130
Dry Azoxystrobin 109 268 275.5 274.5 107.5
WEIGHT OF RC AZOXY (WET) gms
Result of Dry Azoxystrobin gms 109 268 275.5 274.5 107.5
MOISTURE % 0.25 0.04 0.07 -- --

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PURITY w/w % 98.84 98.49 98.53 97.5 97.2

100% Azoxystrobin (Purity Base ) gms
YIELD CALCULATION
Weight baseYIeld % 86.69 85.25 87.64 87.32 85.49
Purity Base yield % 88.00 86.54 88.97 88.64 86.79
DMA and Aq.mass Distillation
Filtrate ML For Distillation gms -- 1332 1685 -- --
Ist CUT ( Distilled water ) gms -- 641.68 830.19 -- --
SPGR of Ist CUT (Distilled water) -- 0.9985 0.9982 -- --
IIND CUT( Distilled Water & DMA) gms -- 71.99 60 -- --
MOISTURE % -- 13.54 16 -- --
IIRD CUT( DMA ) gms -- 467.26 574.41 -- --
% Purity % -- 99.81 99.88 -- --
% Moisture % -- 0.35 0.4 -- --
Residue gms -- 40 45 -- --

NOTE:1. Recover DMA used in Charge No:193

2. Distilled Water cut used in Charge No: 195 for Quenching step.

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