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Synthesizing method of active compound of chlorpyrifos

A synthesis method and technology of chlorpyrifos are applied in the synthesis field of producing chlorpyrifos original drug, can solve problems such as low crude oil content of chlorpyrifos, high toxicity of organic solvent, long process route, etc., achieve less harm to human, improve yield and purity, and simple process Effect

Inactive Publication Date: 2013-03-27
HUBEI XIANLONG CHEM IND
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention mainly solves the existing technologies of high toxicity, large pollution, dangerous operation, unenvironmental protection, long process route, low yield and high production cost of organic solvents existing in the prior art; low crude oil content and low yield of chlorpyrifos synthesized by aqueous phase method, etc. problem

Method used

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  • Synthesizing method of active compound of chlorpyrifos

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Example 1: In a reaction kettle, add 200g of 2,3,5,6-tetrachloropyridine, 200g of water, 300g of 30% NaOH, slowly raise the temperature to between 145°C and 150°C for 5 hours, then cool down to room temperature and discharge to obtain 210g of sodium 3,5,6-triclopyridinate (tested content 88.30%) is set aside, put 150g of water and 0.1g of emulsifier into another reaction kettle (the composition of the emulsifier is 32.5% of calcium dodecylbenzenesulfonate, Alkylaryl polyoxyethylene polyoxypropylene ether 25.5%, nonylphenol polyoxyethylene ether 22%, toluene 20%), 0.1g catalyst 4-dimethylaminopyridine, stir for 15 minutes, and then add 3,5,6 - Sodium triclopyridinate 60g, warm up to 30°C, and stir for 30 minutes, add 47.8g of O, O-diethylthiophosphoryl chloride (content 99.1%) dropwise at 30-40°C, and use during the reaction Soda ash adjusts the pH value of the system between 8.5 and 9.0, then heats up to 43 to 48°C for 3 hours and keeps warm for 3 hours at 55 to 60°C fo...

Embodiment 2

[0010] Example 2: In the reaction kettle, add 1000g 2,3,5,6-tetrachloropyridine, 1000g water, 1540g 30% NaOH, slowly raise the temperature to between 145°C and 150°C and keep it warm for 5 hours, then cool down to room temperature and discharge to obtain 1010g3,5, Sodium 6-trichloropyridinate (tested content 86.575%) is used for later use, and 1.5L of water and 1g of emulsifier are put into another reaction kettle (the composition of the emulsifier is 32.5% of calcium dodecylbenzenesulfonate, alkyl aryl Polyoxyethylene polyoxypropylene ether 25.5%, nonylphenol polyoxyethylene ether 22%, toluene 20%), 1g catalyst 4-dimethylaminopyridine, stir for 15 minutes, and then add 3,5,6-trichloropyridinol Sodium 612.5g, heat up to 30°C, and stir for 30 minutes, drop O, O-diethylthiophosphoryl chloride (content 99.1%) 480g between 30°C and 40°C, adjust the pH value of the system with soda ash during the reaction Between 8.5 and 9.0, then heat up to 43-48°C for 3 hours and 55-60°C for 2 ...

Embodiment 3

[0011] Example 3: In the reaction kettle, add 1000g 2,3,5,6-tetrachloropyridine, 1000g water, 1540g 30% NaOH, slowly raise the temperature to 150°C-155°C and keep it warm for 5 hours, then cool down to room temperature and discharge to obtain 1000g3,5, Sodium 6-trichloropyridinate (tested content 87.50%) is used for later use, put 1.5L water and 1g emulsifier into another reaction kettle (the emulsifier composition is calcium dodecylbenzenesulfonate 32.5%, alkylaryl Polyoxyethylene polyoxypropylene ether 25.5%, nonylphenol polyoxyethylene ether 22%, toluene 20%), 1g catalyst 4-dimethylaminopyridine, stir for 15 minutes, and then add 3,5,6-trichloropyridinol Sodium 612.0g, heat up to 30°C, and stir for 30 minutes, add O, O-diethylthiophosphoryl chloride (content 99.1%) 480g dropwise between 30°C and 40°C, adjust the pH value of the system with soda ash during the reaction Between 8.5 and 9.0, then heat up to 43-48°C for 3 hours and 55-60°C for 2 hours, filter to the washing k...

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Abstract

The invention provides a synthesizing method of chlorpyrifos primary drugs. The method comprises the following steps of: dosing 2,3,5,6-tetrachloropyridine and NaOH with the volume concentration of 30% into a high-pressure autoclave in one time, insulating the reacting materials at a temperature of between 145 and 155 DEG C for 5 hours, and cooling and crystallizing to obtain a 3,5,6-trichloropyridin-2-ol sodium; injecting water into another reaction kettle, and dosing an emulsifier which accounts for 0.1 to 0.15 percent of the mass of the water, and catalyst 4-dimethylaminopyridine which accounts for 0.1 percent of the mass of the water into the water, stirring for 15 minutes, dosing the 3,5,6-trichloropyridin-2-ol sodium which is in a ratio of 1:(2.8-3.0) with the water mass into the reaction kettle, and dripping O,O-diethyl thiophosphoryl chloride until the reaction is completed. The synthesizing method has the advantages of simple process, small hurt to human, small environment pollution, high yield and purity, and the like, the technical problems of low content and low yield of a traditional aqueous phase process for synthesizing chlorpyrifos crude oil can be solved, and the environment can be effectively protected.

Description

technical field [0001] The present invention relates to a kind of chlorpyrifos technical material, especially relate to a kind of 2,3,5,6-tetrachloropyridine, water, 30% sodium hydroxide and O, O-diethyl thiophosphoryl chloride as starting raw material production Synthetic method of chlorpyrifos technical substance. Background technique [0002] Chlorpyrifos, chemical name O, O-diethyl-O-(3,5,6-trichloro-2-pyridyl) phosphorothioate, is a highly efficient, broad-spectrum, low-to-medium toxicity organophosphorus insecticide It is an anti-acaricide, which has contact killing, stomach poisoning and fumigation effects, and can effectively control pests and mites in rice, wheat, corn, cotton, sugarcane and other crops. It is an important product for the current pesticide structure adjustment in my country. There are many methods for synthesizing chlorpyrifos in the industry at present, and there are mainly four methods for the preparation of 3,5,6-trichloropyridinol sodium: pyridi...

Claims

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Application Information

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IPC IPC(8): C07F9/58
Inventor 翟专张业祥刘志新
Owner HUBEI XIANLONG CHEM IND
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