Crystallization method of azoxystrobin
A technology of azoxystrobin and crystallization, applied in the crystallization field of azoxystrobin, can solve the problems of difficult filtration, long filtration time and high purity, and achieve the effects of low moisture content, fast filtration speed and high purity of the product
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preparation example 1
[0051] Add 200 g of azoxystrobin in butyl acetate solution (the content of azoxystrobin is 30% by weight) in a 500ml reaction bottle, heat up to 70°C to completely dissolve; control the temperature to 66°C, slowly cool down to 45°C in 4 hours, and keep warm After 2 hours, the solid product obtained by filtration was used as a seed crystal (hereinafter also referred to as seed crystal A).
[0052] figure 1 It is the X-ray powder diffraction pattern measured by Cu-Kα radiation at 25° C. for seed crystal A in Preparation Example 1. Such as figure 1 As shown, the 2θ values of the X-ray powder diffraction pattern measured by Cu-Kα radiation of the seed crystal A at 25°C are at 7.5±0.2, 8.5±0.2, 13.3±0.2, 13.9,±0.2, 14.6±0.2, 18.2 ±0.2°, 18.5±0.2°, 19.0±0.2°, 20.6±0.2°, 21.4±0.2°, 22.5±0.2°, 22.7±0.2°, 24.4±0.2°, 26.3±0.2°, 26.8±0.2°, There are characteristic peaks at 28.8±0.2° and 30.8±0.2°.
[0053] Add 60 g of crude azoxystrobin and 200 ml of methanol into a 500 ml reaction...
Embodiment 1
[0056] Add 500 g of azoxystrobin butyl acetate solution (azoxystrobin content is 30% by weight) in a 1000 ml reaction bottle, heat up to 70° C. to completely dissolve, then cool down to 66° C., add 2 g of seed A, and keep stirring for 30 Minutes for the first stage of crystallization; then, take 5 hours to cool down to 45°C, keep warm for 2 hours to carry out the second stage of crystallization; then, take 5 hours to cool down to 5°C, keep warm for 30min for the third stage of crystallization; the third stage crystallization product Suction filtration was carried out, which took about 15 minutes, and the obtained crystals had an measured moisture content of 13% by weight. Sampling microscope shows as figure 2 As shown, the size of its crystals is 100-700um.
Embodiment 2
[0058] Add 500 g of butyl acetate solution of azoxystrobin (the content of azoxystrobin is 27% by weight) in a 1000 ml reaction bottle, heat up to 70° C. to completely dissolve, then cool down to 64° C., add 2 g of seed A, and keep stirring for 60 Minutes for the first stage of crystallization; then, take 5 hours to cool down to 45°C, keep warm for 1 hour to carry out the second stage of crystallization; then, take 5 hours to cool down to 5°C, keep warm for 30min to carry out the third stage of crystallization; the third stage crystallization product Suction filtration was carried out for about 15 minutes, and the moisture content of the obtained crystals was determined to be 13% by weight, and the crystal size was 150-800um.
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