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Method for synthesizing chlorpyrifos by adopting microreactor

A technology of microreactor and chlorpyrifos, which is applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, chemical/physical/physicochemical processes, etc., can solve problems such as difficulty in controlling the quality of finished products, and achieve improved product quality. quality, shorten the reaction time, and improve the effect of reaction yield

Pending Publication Date: 2022-04-01
CHONGQING HUAGE BIOCHEM
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Problems solved by technology

[0005] The present invention intends to provide a method for synthesizing chlorpyrifos using a microreactor to solve the technical problem that the quality of the finished product is difficult to control using the existing synthesis process

Method used

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  • Method for synthesizing chlorpyrifos by adopting microreactor
  • Method for synthesizing chlorpyrifos by adopting microreactor
  • Method for synthesizing chlorpyrifos by adopting microreactor

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Embodiment

[0025] A method for synthesizing chlorpyrifos using a microreactor (Shandong Jinde New Material Co., Ltd. model C0-4 can be selected), the process is as follows:

[0026] Put 100 g of sodium clopyridinate raw material into a four-necked bottle, wherein the sodium clopyridinate sodium in the raw material has a mass percentage of sodium clopyridinate greater than 85.5%, and the structural formula of sodium clopyridinate is shown in formula (1). Add the solvent acetonitrile whose weight is 1.7-2.5 times of the raw material of sodium clopyridinate and the water whose weight is 2.0-2.4 times of the raw material of sodium clopyridinate. Then, add catalysts A1, A2 and A3, stir to form a solution for later use, and obtain a sodium alkoxide solution. The mass percentages of A1, A2 and A3 in the sodium alkoxide solution are 0.2-0.3%, 0.25-0.35% and 0.1-0.15% respectively. Wherein, A1 is one of 2-methylcyclohexylamine, 4-dimethylaminopyridine and 4-methylaminopyridine; A2 is 4-butylammo...

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Abstract

The invention relates to the technical field of pesticide synthesis methods, in particular to a method for synthesizing chlorpyrifos by adopting a microreactor. The technical process of the scheme comprises the following steps: respectively inputting a sodium alkoxide solution, an alkali solution and ethyl chloride into a microchannel of a microreactor, synthesizing chlorpyrifos under the reaction conditions that the pH is 9-10, the temperature is 92-95 DEG C and the retention time is 50-70 seconds, and continuously collecting reaction effluent. According to the scheme, the technical problem that the quality of a finished product obtained through an existing synthesis process is difficult to control can be solved, and the chlorpyrifos synthesis process is efficient, continuous and low in cost.

Description

technical field [0001] The invention relates to the technical field of pesticide synthesis methods, in particular to a method for synthesizing chlorpyrifos using a microreactor. Background technique [0002] Chlorpyrifos is an organophosphorus insecticide with contact, stomach poisoning and fumigation effects. It is used in corn, cotton, rice, soybean, peanut, sugar beet, fruit trees and vegetables to control various soil and foliar pests. The existing synthesis route of chlorpyrifos is: 3,5,6-trichloropyridinate sodium and O,O-diethylthiophosphoryl chloride are condensed in water phase under catalyst conditions. [0003] Chinese patent CN102775443A (synthetic method of chlorpyrifos) reports that the finished product of potassium triclopyridinate is put into a reaction kettle, water, boric acid and catalyst are added, the temperature is stirred to 75-80°C, the pH is maintained at 9-10, and ethyl chloride is added dropwise. , maintain for 3-5 hours, stand still and separate ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/58B01J19/00
Inventor 陈志忠何小强林军崔红洋冯如平
Owner CHONGQING HUAGE BIOCHEM
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