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Purification method of chlorpyrifos

A purification method, chlorpyrifos technology, applied in the field of chlorpyrifos purification, can solve problems such as unsatisfactory, inconvenient operation, cumbersome recrystallization operation, etc., and achieve the effects of easy operation, improved product yield and purity, and omission of recrystallization steps

Inactive Publication Date: 2013-03-20
ANHUI COSTAR BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The recrystallization operation in this method is cumbersome and inconvenient to operate, and the yield is 92%~95%, which is not ideal

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 3000L enamel glass reaction kettle, add 1100Kg water and 220Kg 3,5,6-trichloropyridin-2-alcohol sodium, stir well, then add 5Kg trimethylamine 30% aqueous solution, 0.5Kg 4-dimethylaminopyridine and 207Kg O, O-diethylthiophosphoryl chloride, add 10% sodium hydroxide solution dropwise to adjust pH=9~10, raise the temperature to 60°C for 1.5h, transfer the reaction liquid into the separatory tank, add 0.25 Kg Alkyl phenolic resin, polyoxyethylene polyoxypropylene ether, stirred at 60°C for 1 hour, let stand to separate the water layer, washed the organic phase once with 500L of 60°C water, then acid-washed once with 500LPH=3 sulfuric acid aqueous solution, and dried to obtain Chlorpyrifos technical, yield 98.2%, content 98.3% (liquid chromatography).

Embodiment 2

[0023] In a 3000L enamel glass reaction kettle, add 1100Kg water and 220Kg 3,5,6-trichloropyridin-2-alcohol sodium, stir well, then add 5Kg trimethylamine 30% aqueous solution, 0.5Kg 4-dimethylaminopyridine and 207Kg O, O-diethylthiophosphoryl chloride, add 10% sodium hydroxide solution dropwise to adjust pH=9~10, raise the temperature to 60°C for 1.5h, transfer the reaction liquid into the separatory tank, add 0.25 Kg Alkyl phenolic resin, polyoxyethylene polyoxypropylene ether, stirred at 60°C for 1 hour, let stand to separate the water layer, washed the organic phase once with 500L of 60°C water, then acid-washed once with 500LPH=6 sulfuric acid aqueous solution, and dried Chlorpyrifos technical, yield 98.0%, content 98.1% (liquid chromatography).

Embodiment 3

[0025] In a 3000L enamel glass reaction kettle, add 1100Kg water and 220Kg 3,5,6-trichloropyridin-2-alcohol sodium, stir well, then add 5Kg trimethylamine 30% aqueous solution, 0.5Kg 4-dimethylaminopyridine and 207Kg O,O-diethylthiophosphoryl chloride, add dropwise 10% sodium hydroxide solution to adjust pH=9~10, raise the temperature to 60°C for 1.5h, and transfer the reaction solution into the separatory tank, add 0.3 Kg Polysiloxane Polyoxyethylene Polyoxypropylene Ether Stir at 60°C for 1 hour, let stand to separate the water layer, wash the organic phase with 500L 80°C water once, then pickle once with 500LPH=3 sulfuric acid aqueous solution, and dry it Chlorpyrifos technical, yield 98.3%, content 98.4% (liquid chromatography).

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PUM

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Abstract

The present invention discloses a purification method of chlorpyrifos. According to the method, a demulsifier is added into an oil-water system obtained by condensation of an aqueous phase method for water demulsification. The separated oil phase is firstly washed with water of a suitable temperature, then acid of an appropriate temperature is used for pickling, and last the separated crude oil is dehydrated and dried to obtain finished chlorpyrifos with a content of more than 98%. The traditional separation process is improved and optimized by the present invention, a cumbersome recrystallization operation step is eliminated, and the demulsification and pickling steps are added. The purification method is simple and reliable, and easy to operate, and the product yield and purity can be increased to above 98%.

Description

technical field [0001] The invention relates to the field of chemical purification, in particular to a method for purifying chlorpyrifos. Background technique [0002] Chlorpyrifos, chemical name O,O-diethyl-O-(3,5,6-trichloro-2-pyridyl) phosphorothioate, its molecular formula is C 9 h 11 Cl 3 NO 3 PS. As an organophosphorus insecticide, chlorpyrifos has high efficiency, broad spectrum and low toxicity. It is the first choice for replacing highly toxic organophosphorus insecticides such as methamidophos and parathion in my country's current pesticide structure adjustment. Its mechanism of action is to inhibit acetylcholinesterase. It has three modes of action: contact killing, stomach poisoning and fumigation. It can effectively control more than 100 kinds of pests and mites. The synthetic method of chlorpyrifos is mainly two-solvent method and aqueous phase method according to different solvents of the reaction. The dual-solvent method uses water and an organic solve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/58
Inventor 葛九敢李健刘善和强金凤王红明
Owner ANHUI COSTAR BIOCHEM CO LTD
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