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Recrystallization method for improving trans-fluorochloridone content

A flurotrione and recrystallization technology, applied in the directions of solution crystallization, botanical equipment and methods, herbicides and algicides, etc. Efficient weeding and other problems, to achieve the effect of convenient operation, improving market competitiveness, and uniform crystal particle size

Active Publication Date: 2012-12-05
SUZHOU JIAHUI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the technical fluromidone synthesized from m-aminotrifluorotoluene and dichloroacetyl chloride has a low transcis ratio of fluromidone, which cannot meet the requirements of high-efficiency weed control and lacks market competitiveness.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] (1) 500 kg of fluroxazone technical material and 150 kg of dichloromethane are placed in the crystallization kettle, and the stirring device is started to stir;

[0015] (2) Control the temperature of the crystallization kettle to 30°C, and continue to stir for 2 hours, and then the original drug of fluroxazone is completely dissolved;

[0016] (3) After the original drug of fluroxazone is completely dissolved, the temperature is slowly lowered to crystallize, and after 3 hours of crystallization, the temperature of the crystallization kettle drops to 5°C;

[0017] (4) After the crystallization was completed, the obtained sample was placed in a centrifuge and filtered to obtain the technical product of fluroxazone. After analyzing the obtained sample, it was found that the anti-cis ratio of the technical product of fluroxazone increased by 1.5 times.

Embodiment 2

[0019] (1) 580 kg of fluroxazone technical substance and 200 kg of dichloromethane are placed in the crystallization kettle, and the stirring device is started to stir;

[0020] (2) Control the temperature of the crystallization tank to 38°C, and continue to stir for 2.5 hours to completely dissolve the original drug of fluroxazone;

[0021] (3) After the dissolution of the original drug of fluroxazone is completed, the temperature is slowly lowered to crystallize, and after 4 hours of crystallization, the temperature of the crystallization kettle drops to 10°C;

[0022] (4) After the crystallization was completed, the obtained sample was placed in a centrifuge and filtered to obtain the technical product of fluroxazone. After analyzing the obtained sample, it was found that the anti-cis ratio of the technical product of fluroxazone increased by 1.1 times.

Embodiment 3

[0024] (1) 700 kg of fluroxidone technical substance and 240 kg of dichloromethane are placed in the crystallization kettle, and the stirring device is started to stir;

[0025] (2) Control the temperature of the crystallization kettle to 45° C., and continue to stir for 3 hours, and then the original drug of fluroxazone is completely dissolved;

[0026] (3) After the dissolution of the original drug of fluroxazone is completed, the temperature is slowly lowered to crystallize, and after 4 hours of crystallization, the temperature of the crystallization kettle drops to 8°C;

[0027] (4) After the crystallization was completed, the obtained sample was placed in a centrifuge and filtered to obtain the technical product of fluroxazone. After analyzing the obtained sample, it was found that the anti-cis ratio of the technical product of fluroxazone increased by 1.8 times.

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Abstract

The invention relates to a recrystallization method for improving trans-fluorochloridone content. The method comprises the following steps: placing a fluorochloridone technical material and a solvent into a crystallization kettle, and starting a stirring device for stirring; controlling the temperature of the crystallization kettle to be between 30 and 45 DEG C, and continuing stirring to dissolve the fluorochloridone technical material; after the dissolution of the fluorochloridone technical material is finished, performing the cooling crystallization of the solvent with crystallization timefor 3 to 4 h, at the crystallization temperature between 5 and 10 DEG C; and after the crystallization is finished, spinning and filtering the obtained sample in a centrifuge to obtain a product. Compared with the prior art, the recrystallization method improves the ratio of trans form to cis form of the fluorochloridone technical material by 1 to 2 times, is favorable for obtaining the fluorochloridone technical material with high trans form content, and has crystalline particles with uniform size and convenient operation.

Description

technical field [0001] The invention relates to a recrystallization method, in particular to a recrystallization method for increasing the content of trans-fluroxazone. Background technique [0002] Fluroxetone technical is mainly used for pre-emergence treatment of winter wheat, rye, cotton, potato and other crops to control broad-leaved weeds. Its herbicidal effect is mainly based on the trans content of fluroxidone, and the higher the trans content of fluroxidone, the better the herbicidal effect. At present, the technical fluromidone synthesized from m-aminotrifluorotoluene and dichloroacetyl chloride has a low transcis ratio of fluromidone, which cannot meet the requirements of high-efficiency weed control and lacks market competitiveness. Therefore, it is necessary to recrystallize the original drug of fluroxazone to increase its trans content. Contents of the invention [0003] The object of the present invention is to provide a recrystallization method for increa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/273A01N43/36B01D9/02A01P13/00
Inventor 田晓宏李维华周忠良熊德兴
Owner SUZHOU JIAHUI CHEM
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