Method for synthesizing chlorpyrifos by using ultrasonic catalysis

A chlorpyrifos and ultrasonic technology, applied in chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of many by-products, cumbersome operation, different temperature requirements, etc., to save production Cost, low equipment requirements, and the effect of saving reaction time

Inactive Publication Date: 2019-02-22
CHONGQING HUAGE BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the temperature requirements of the two stages in the prior art are different, and the operation is relatively cumbersome
On the other hand, the heat preservation time needs 3-3.5 hours, and the whole reaction takes 5.5-6 hours. The reaction cycle is longer, more by-products are produced, and the energy consumption is higher.

Method used

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  • Method for synthesizing chlorpyrifos by using ultrasonic catalysis

Examples

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Comparison scheme
Effect test

Embodiment 1

[0028] The present embodiment provides a method for ultrasonic catalytic synthesis of chlorpyrifos, the specific steps are as follows:

[0029] S1. Put the reaction flask into the ultrasonic generator and set the ultrasonic frequency to 20KHz.

[0030] S2. Put 200g of sodium triclopyridinate and 400g of water into the reaction flask, start stirring, put in 1.11g of composite catalyst (triethanolamine+tetrabutylammonium bromide), and heat up to 65°C.

[0031] S3. Slowly add 181.2g of O,O-diethylphosphorylthiochloride dropwise into the reaction flask within 55 minutes, and control the pH of the solution to 7-8 during the dropwise addition.

[0032] S4. After the addition is finished, separate the liquid to obtain the crude product of chlorpyrifos; the crude product of chlorpyrifos is processed successively through alkali washing, pickling, and dehydration to obtain 340.0g of chlorpyrifos, which is detected by HPLC quantitative analysis. The yield is 96.2%, and the purity is 97.2...

Embodiment 2

[0034] The present embodiment provides a method for ultrasonic catalytic synthesis of chlorpyrifos, the specific steps are as follows:

[0035] S1. Put the reaction flask into the ultrasonic generator and set the ultrasonic frequency to 30KHz.

[0036] S2. Put 200g of sodium clopyridinate and 400g of water into the reaction bottle, start stirring, put in 0.99g of composite catalyst (triethylenediamine+dispersant DAS), and heat up to 65°C.

[0037] S3. Slowly add 178.0 g of O,O-diethylphosphorylthiochloride dropwise into the reaction flask within 43 minutes, and control the pH of the solution to 7-8 during the dropwise addition.

[0038] S4. After the addition is finished, separate the liquid to obtain the crude product of chlorpyrifos; the crude product of chlorpyrifos is subjected to alkali washing, pickling, and dehydration post-treatment successively to obtain 330.0 g of chlorpyrifos, which is detected by HPLC quantitative analysis and has a yield of 98.0% and a purity of 9...

Embodiment 3

[0040] The present embodiment provides a method for ultrasonic catalytic synthesis of chlorpyrifos, the specific steps are as follows:

[0041] S1. Put the reaction flask into the ultrasonic generator and set the ultrasonic frequency to 50KHz.

[0042] S2. Put 200g of sodium triclopyridinate and 400g of water into the reaction bottle, start stirring, put in 1.00g of composite catalyst (dimethylcyclohexylamine+dispersant WA+tetrabutylammonium iodide), and heat up to 70°C.

[0043] S3. Slowly add 177.8g of O,O-diethylphosphorothiochloride dropwise into the reaction flask within 37 minutes, and control the pH of the solution to 7-8 during the dropwise addition.

[0044] S4. After the addition is finished, separate the liquids to obtain the crude product of chlorpyrifos; the crude product of chlorpyrifos is processed successively through alkali washing, pickling, and dehydration to obtain 339.6g of chlorpyrifos, which is detected by HPLC quantitative analysis and has a yield of 96...

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Abstract

The invention provides a method for synthesizing chlorpyrifos by using ultrasonic catalysis and relates to the field of chemical synthesis. In the process of dripping O, O-diethyl thiophosphoryl chloride, an ultrasonic wave with the frequency of 20-60 kHz is adopted to carry out auxiliary reaction, so that the reaction of sodium trichloro pyridinol and the O, O-diethyl thiophosphoryl chloride canbe finished in the dripping process. Therefore, a follow-up heat insulation condensation reaction stage is eliminated. Complicated operation caused by temperature change is avoided, and a lot of reaction time is also saved. The method for synthesizing the chlorpyrifos by using ultrasonic catalysis, provided by the invention, has the advantages that the operation is simple, requirements on equipment are low, the reaction time is greatly reduced after a reaction condition is improved, the production period is greatly shortened, the production efficiency is enhanced, the production cost is greatly reduced, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing chlorpyrifos by ultrasonic catalysis. Background technique [0002] Chlorpyrifos, also known as chlorpyrifos, chemical name O, O’-di and -O(3,5,6-trichloro-2-pyridyl) phosphorothioate, chemical structure formula is [0003] [0004] 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. [0005] The existing synthetic route of chlorpyrifos is obtained by condensation of 3,5,6-trichloropyridinate sodium and O,O-diethylthiophosphoryl chloride in the water phase under catalyst conditions. The reaction process includes two main stages: 1. O, O-diethyl thiophosphoryl chloride dropwise addition stage; 2. Insulation condensation reaction stage. Among them, the O, O-diethylthiop...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07F9/58
Inventor蒲桃蔡玉华吴承丽沈琼何小强
OwnerCHONGQING HUAGE BIOCHEM