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Method for synthesizing chlopyrifos in water medium

A kind of technology of chlorpyrifos and water medium, applied in the field of production of chlorpyrifos, can solve problems such as less than ideal, troublesome operation, difficult to control reaction, etc., and achieve the effect of easy operation, low production cost, and improved product yield and purity

Active Publication Date: 2006-11-08
SHANDONG TIANCHENG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is cumbersome to operate, difficult to control the reaction, 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

[0026] In a 250ml four-neck flask equipped with a stirring and thermometer, add 118.5g of water, 1g of Pingpingjia O-20, 0.5g of sodium dodecylbenzenesulfonate, 0.25g of a 30% aqueous solution of trimethylamine, 1g of trioctylmethyl ammonium chloride, 0.5g 4-dimethylaminopyridine, 20.7g O, O-diethylphosphoryl thiochloride, 22.0g 3,5,6-trichloropyridin-2-alcohol sodium, with 30% potassium carbonate solution and 20% sodium hydroxide solution to adjust PH=9.7, heat up to 55°C and react for 1 hour, cool down to 20°C to crystallize, filter with suction, wash with water, and dry to obtain white crystals of chlorpyrifos with a yield of 98.1% and a content of 99.0% (gas chromatography Law).

Embodiment 2

[0028] In a 2000L glass-lined reactor, add 1100kg of water, 4.5kg of octylphenol polyoxyethylene ether OP-10, 3.5kg of sodium lauryl sulfate, 5kg of trimethylamine 30% aqueous solution, 0.5kg of 4-dimethylaminopyridine, 5kg Polyethylene glycol 400, 207kg O, O-diethylphosphoryl thiochloride, 220kg 3,5,6-trichloropyridin-2-alcohol sodium, adjust pH=9.5 with 20% potassium carbonate solution and 10% potassium hydroxide solution , heated up to 50° C. for 1.5 hours, cooled to 20° C. to crystallize, discharged, suction filtered, washed with water, and dried to obtain white crystals of chlorpyrifos with a yield of 98.0% and a content of 98.2% (gas chromatography).

Embodiment 3

[0030] The potassium carbonate solution among the embodiment 1 is replaced with 20% sodium carbonate solution, and all the other remain unchanged. Yield 98.0%, content 98.0%.

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PUM

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Abstract

The method of synthesizing chlorpyrifos in water medium features that through adding water into reaction kettle, adding surfactant, 3,5,6-trichloro pyridyl -2-sodium alcoholate and O, O-diethyl thiophosphoryl chloride via stirring for emulsifying and dispersing in water, adding composite catalyst, adding pH regulator to regulate system pH value to 9-10, reaction at 25-65 deg.c, lowering temperature to crystallize, suction filtering, water washing and drying, chlorpyrifos is prepared. The present invention features using water as medium to form high dispersed reaction system, simple and reliable synthesis process, easy operation, high product yield and purify, low production cost and environment friendship.

Description

technical field [0001] The invention relates to a method for producing chlorpyrifos by using 3,5,6-trichloropyridin-2-alcohol sodium and O, O-diethylthiophosphoryl chloride as main raw materials. Background technique [0002] Chlorpyrifos, chemical name O, O-diethyl-O-(3,5,6-trichloro-2-pyridyl) phosphorothioate, is a highly efficient, broad-spectrum, medium and low toxicity organophosphorus insecticide Acaricide is a replacement product for the current pesticide structure adjustment in my country. [0003] The current industrial methods for synthesizing chlorpyrifos mainly include dual-solvent method and aqueous phase method. The main raw materials are 3,5,6-trichloropyridin-2-alcohol sodium and O, O-diethylthiophosphoryl chloride. The dual-solvent method is a dual-solvent system composed of water and an organic solvent (mostly dichloroethane), which can effectively inhibit the hydrolysis of O, O-diethylphosphorylthiochloride, and the yield can reach 95%. However, this me...

Claims

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Application Information

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IPC IPC(8): C07F9/58
Inventor 徐国庆
Owner SHANDONG TIANCHENG BIOTECH
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