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Aqueous phase method for synthesis of chlorpyrifos

A chlorpyrifos, water-phase technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. The effect of improved product yield and purity and low production cost

Pending Publication Date: 2013-12-25
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 invention relates to an aqueous phase method for synthesis of chlorpyrifos. The method is characterized by: adding water into a reaction kettle, adding a surfactant under stirring to make 3, 5, 6-trichloropyridine-2-sodium alkoxide and O, O-diethyl thiophosphoryl chloride emulsified and dispersed in water, then adding a compound catalyst, and a pH regulator to make the pH value of the system reach 9-10, then leaving the materials to react fully at 25-65DEG C, carrying out cooling crystallization, pumping filtration, washing, and drying, thus obtaining a chlorpyrifos original drug product. The main technical features of the invention lie in that: water is adopted as a solution, reactants are added in one time, and by means of the action of the surfactant, a highly dispersed system is formed to undergo reaction. The synthesis method is simple and reliable, and is easy to operate, the product yield and purity are both improved and both can reach over 98%. The production cost is low, and the environment is improved.

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 pre-industrial methods for synthesizing chlorpyrifos mainly include two-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 method ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/58
Inventor 姬文龙
Owner SHANDONG TIANCHENG BIOTECH
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