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A kind of oxadiazone crystallization mother liquor catalytic method prepares the method for oxadiazone phenol

A technology for crystallizing mother liquor and oxadiazonol is applied in the field of resource utilization and treatment of production waste liquid, which can solve the problems of waste acid polluting the environment and long reaction time, and achieves the effect of speeding up the reaction rate and avoiding a large amount of waste acid

Active Publication Date: 2020-05-26
湖南兴同化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The present invention aims at resourceful utilization of the oxadiazone crystallization mother liquor, effectively recovering the residual oxadiazone therein, and at the same time solving the problems of long reaction time and the generation of a large amount of waste acid polluting the environment in the existing synthesis process of oxadiazone phenol, Provide a new process for the synthesis of oxadiasol with environmental friendliness, fast reaction speed and high reaction yield

Method used

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  • A kind of oxadiazone crystallization mother liquor catalytic method prepares the method for oxadiazone phenol
  • A kind of oxadiazone crystallization mother liquor catalytic method prepares the method for oxadiazone phenol
  • A kind of oxadiazone crystallization mother liquor catalytic method prepares the method for oxadiazone phenol

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Effect test

Embodiment 1

[0016] Take 189g of oxadiazone crystallization mother liquor, the content of oxadiazone is 25.6%, recover 116.7g of ethanol, add 100g of solvent dichloroethane and 18g of catalyst aluminum trichloride, start the mechanical stirring, react for 0.5h after dissolving, add dropwise 50g of water. Keep the temperature at about 30°C, let stand after 0.5h, separate the water phase, desolventize the organic phase and use 80g of xylene to recrystallize and purify oxadiazone, and dry the solid to obtain 39.7g of oxadiazone, with an HPLC purity of 97.6 %, the yield is 92.3%.

Embodiment 2

[0018] Take 220g of oxadiazone crystallization mother liquor, the content of oxadiazone is 25.6%. After recovering 126g of ethanol, add 110g of solvent dichloroethane and 20g of catalyst boron trifluoride, start the mechanical stirring, react for 1h after dissolution, and drop 60g of water into it . Keep the temperature at about 40°C, let stand after 0.5h, separate the water phase, desolventize the organic phase and recrystallize with 80g of xylene to purify oxadiazone, and dry the solid to obtain 47.1g of oxadiazone, with an HPLC purity of 98.8 %, the yield is 94.1%.

Embodiment 3

[0020] Take 220g of oxadiazone crystallization mother liquor, the content of oxadiazone is 25.6%. After recovering 122.6g of ethanol, add 110g of solvent dichloroethane and 20g of catalyst aluminum trichloride, start the mechanical stirring, react for 1h after dissolution, and add 55g of it dropwise water. Keep the temperature at about 40°C, let stand after 0.5h, separate the water phase, desolventize the organic phase and recrystallize with 80g of xylene to purify oxadiazone, and dry the solid to obtain 47.7g of oxadiazone, with an HPLC purity of 98.3 %, the yield is 95.3%.

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Abstract

The invention discloses a method for preparing oxadiazon phenol from oxadiazon crystal mother liquor by a catalytic process. With the crystal mother liquor containing 20-60% of oxadiazon as a raw material, the method comprises the following steps: in a series of Lewis acid catalytic hydrolysis conditions, reacting for 0.5-2h at 20-40 DEG C; performing desolvation and purification to obtain oxadiazon phenol. The liquid chromatogram content of the product oxadiazon phenol is over 95%, and the yield exceeds 92%. According to the method, the crystal residual mother liquor generated in the production of oxadiazon is subjected to resource utilization, and the residual active pesticide ingredient oxadiazon in the crystal mother liquor is recycled, thus the utilization rate of the oxadiazon is increased, and the influence of residual pesticide on the ecology is reduced; meanwhile, the oxadiazon is effectively converted into a product with high added value, the production cost of the product islowered indirectly, and relatively great economic benefits and environmental benefits are created.

Description

technical field [0001] The invention belongs to the field of resource utilization and treatment of production waste liquid, and particularly relates to a preparation method for synthesizing oxadiazone from oxadiazone crystallization mother liquor. Background technique [0002] In the production process of oxadiazone, about 20%-60% of oxadiazone will remain in the crystallization mother liquor of the recrystallization step of oxadiazone. They are all similar and difficult to recover by solvent extraction or rectification. Therefore, converting oxadiazone in the crystallization mother liquor into oxadiazone phenol has become an important means to effectively recover oxadiazone. At the same time, clomazoneol is an important derivative of oxadiazone herbicides with high efficiency, and is an important raw material for the synthesis of oxadiazone herbicides such as propargyl clomazone, and has great economic value. The current synthesis method of oxadiazone is mainly to obtain ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D271/113
CPCC07D271/113
Inventor 党东辉廖丽莎段正康李华轩王宇
Owner 湖南兴同化学科技有限公司