Metamifop crystallization purification method
A technology of fenpyramid and purification method, which is applied in the field of chemical raw materials, can solve the problems of high energy consumption, high cost, and large product loss, and achieve the effects of saving purification process, removing impurities, and reducing loss
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[0034] Example 1
[0035] Add 120g of crude oxadifen (content 79.6%) to a 1000mL reactor, then add 360g of isopropanol, heat and stir, control the temperature of the material at 80℃, stir for 1.5h to dissolve, after dissolving, heat to 0.5℃ Stir slowly at a cooling rate per minute to -5°C, keep for 1h, adjust the stirring speed to 45rpm, and slowly add 72g of water to the system at a uniform speed. The addition time should be longer than 1h. After the addition is complete, stir for 0.5h before adding 1.2 g oxadifen seed crystals, then stir for 0.5h, then continue to slowly add 144g of water to the reactor at a constant speed for 3h, after the addition, stir for 3h, filter, and rinse the filter cake twice with 72g of water, set Dry in an oven at 50°C to obtain a powdered solid of oxadifen. The purity is 99.57%, the content is 99.37%, and the crystallization yield is 98.67% by conventional methods. 1HNMR (400MHz, dmso-d6) δ 7.624-7.279 (m, 9H), 6.858-6.737 (m, 2H), 4.752-4.674 (m...
Example Embodiment
[0040] Example 2
[0041] Add 120g of crude oxadifen (content 79.6%) to a 1000mL reaction kettle, then add 460g of ethanol, heat and stir, control the temperature of the material at 50-70℃, stir for 1.5h to dissolve, after dissolving, heat to 0.5℃ Stir slowly at a cooling rate per minute to -3°C, keep for 1h, adjust the stirring speed to 45rpm, and add 72g of water to the system slowly and uniformly. The addition time should be longer than 1h. After the addition is complete, stir for 0.5h and then add 1.2 g oxadifen seed crystals, then stir for 0.5h, then continue to slowly add 144g of water to the reactor at a constant speed for 3h, after the addition, stir for 3h, filter, and rinse the filter cake twice with 72g of water, set Dry in an oven at 45°C to obtain a powdered solid of oxadifen. The purity is 99.13%, the content is 99.26%, and the crystallization yield is 95.37% by conventional methods.
Example Embodiment
[0042] Example 3
[0043] Add 120g of crude oxadifen (content 79.6%) to a 1000mL reactor, then add 360g of methanol, heat and stir, control the temperature of the material at 50-60℃, stir for 1.5h to dissolve, after dissolving, heat to 0.5℃ Stir slowly at a cooling rate per minute to -5°C, keep for 1h, adjust the stirring speed to 45rpm, and slowly add 72g of water to the system at a uniform speed. The addition time should be longer than 1h. After the addition is complete, stir for 0.5h before adding 1.2 g oxfenacet seed crystals, and then stir for 0.5h, then continue to slowly add 144g of water to the reactor at a constant speed for 3h, after the addition, stir for 3h, filter, and rinse the filter cake twice with 72g water, set Dry in an oven at 55°C to obtain oxadifen in powder form. By conventional methods, the purity is 99.42%, the content is 99.35%, and the crystallization yield is 97.34%.
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