Method for preparing O,O-diethylthiophosphorylchloride

A technology of diethyl phosphorothioate and diethyl phosphorodithioate, which is applied in the field of industrial preparation of organophosphorus fine chemicals, can solve the problems of high production cost, heavy pollution, complicated process, etc., and achieve the reduction of chlorination and the effect of perchlorinated impurities

Inactive Publication Date: 2016-11-09
JIANGSU XINNONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a new preparation method of O,O-diethylphosphoryl thiochloride, to effectively...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: Put 400 parts of phosphorus pentasulfide into 300 parts of O, O-diethyl phosphorodithioate, control the temperature at 5-50°C, add 4 parts of catalyst hydroxymethylpyridine, dropwise add 300 parts of absolute ethanol , kept warm for 30 minutes to obtain O, O-diethyl phosphorodithioate, content 95%, 900 parts of O, O-diethyl phosphorodithioate was dropped into the chlorination kettle, and the temperature was controlled at 30- Inject 300 parts of chlorine gas at 60°C, and the flow rate of chlorine gas is controlled at 1.3-1.5g / min. When the density of the reaction liquid reaches 1.275-1.285g / cm 3 , the reaction ends and the crude product of ethyl chloride is obtained; Transfer the material into the crystallization kettle, and start centrifugation when the temperature drops below 10°C, transfer the ethyl chloride after centrifugation into a thin-film evaporator, and collect distillate under the conditions of air pressure 10-30mmHg and temperature 90-110°C The pr...

Embodiment 2

[0013] Example 2: Put 500 parts of phosphorus pentasulfide into 400 parts of O, O-diethyl phosphorodithioate, control the temperature at 5-50°C, stir and add 5 parts of catalyst hydroxymethylpyridine, add dropwise 400 parts of absolute ethanol , and kept warm for 50 minutes to obtain O, O-diethyl phosphorodithioate with a content of 95%. 1000 parts of O, O-diethyl phosphorodithioate were put into the chlorination kettle, and the temperature was controlled at 30- Inject 400 parts of chlorine gas at 60°C, and the flow rate of chlorine gas is controlled at 1.3-1.5g / min. When the density of the reaction liquid reaches 1.275-1.285g / cm 3 , the reaction ends and the crude product of ethyl chloride is obtained; Transfer the material into the crystallization kettle, and start centrifugation when the temperature drops below 10°C, transfer the ethyl chloride after centrifugation into a thin-film evaporator, and collect distillate under the conditions of air pressure 10-30mmHg and temperat...

Embodiment 3

[0014] Example 3: Put 600 parts of phosphorus pentasulfide into 500 parts of O, O-diethyl phosphorodithioate, control the temperature at 5-50°C, add 6 parts of catalyst hydroxymethylpyridine, dropwise add 450 parts of absolute ethanol , and kept warm for 60 minutes to obtain O, O-diethyl phosphorodithioate with a content of 95%. 1000 parts of O, O-diethyl phosphorodithioate were put into the chlorination kettle, and the temperature was controlled at 30- Inject 420 parts of chlorine gas between 60°C and control the flow rate of chlorine gas at 1.3-1.5g / min. When the density of the reaction liquid reaches 1.275-1.285g / cm 3 , the reaction ends and the crude product of ethyl chloride is obtained; Transfer the material into the crystallization kettle, and start centrifugation when the temperature drops below 10°C, transfer the ethyl chloride after centrifugation into a thin-film evaporator, and collect distillate under the conditions of air pressure 10-30mmHg and temperature 90-110°...

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PUM

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Abstract

The present invention discloses a method for preparing O,O-diethylthiophosphorylchloride, including the steps: a, preparing an intermediate by reaction of phosphorus pentasulfide with ethanol; b, synthesizing crude ethyl chloride by reaction of sulfides with chlorine; c, subjecting the crude ethyl chloride to the procedures such as crystallizing, centrifuging and distillation to obtain the required product. The invention has the advantages that esterification is carried out in the presence of a phase transfer catalyst without a solvent; chlorination byproduct S2Cl2 and an esterification product are subjected to in-situ reductive chlorination through optimal selection of chlorination catalysts and chloride depth control so that there is no byproduct S2Cl2 produced at a chlorination end point, thereby reducing chlorination and superchlorination impurities; the target product has a purity of higher than 99.5% and can meet the requirements of high-grade products for production and exporting.

Description

technical field [0001] The invention belongs to the field of industrial preparation of organic phosphorus fine chemicals, and in particular relates to a method for preparing O, O-diethylthiophosphoryl chloride (ethyl chloride for short). Background technique [0002] Diethoxythiophosphoryl chloride is an important pesticide intermediate, and the production of pesticides such as chlorpyrifos, triazophos, diazinon and phoxim requires the key intermediate ethyl chloride. At home and abroad, mainly use phosphorus pentasulfide and ethanol as starting materials to synthesize ethyl chloride through reaction steps such as esterification and chlorination. Since the by-product S2Cl2 is unstable, easy to decompose, and miscible with ethyl chloride, it is now widely used. Alkali sulfide or sodium sulfite is used as a reducing agent to reduce S2Cl2 to sulfur, and then dissolve the generated sodium chloride or sodium sulfate with water and wash and purify the target compound ethyl chlorid...

Claims

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Application Information

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IPC IPC(8): C07F9/20
CPCC07F9/20
Inventor 徐群辉
Owner JIANGSU XINNONG CHEM
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