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O, O-dialkylphosphoryl thiochloride preparation method without waste residue

A technology of alkyl thiophosphoryl and ethyl thiophosphoryl, which is applied in the field of O,O-dialkyl thiophosphoryl chloride free-slag preparation, can solve the problem that it is difficult to deal with sticky sulfur waste residues, the reaction heat is large, and the treatment It is difficult to solve problems such as high difficulty, and achieves the effects of easy industrialization, high yield and low production cost.

Inactive Publication Date: 2016-03-09
秦小林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The phosphorus pentasulfide method that generally adopts at home and abroad has a serious deficiency in conversion rate and content at present, produces a large amount of sticky sulfur waste residues that are difficult to handle, and the pollution is serious, and the treatment difficulty is large (referring to US5278331; CN101130554); Thiophosphoryl chloride developed by Bayer The method reacts under a large amount of alkyl alcohol, the heat of reaction is large, and the reaction must be maintained at about 0°C, the energy consumption is large, and the product content is low (see US5948930)

Method used

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  • O, O-dialkylphosphoryl thiochloride preparation method without waste residue
  • O, O-dialkylphosphoryl thiochloride preparation method without waste residue
  • O, O-dialkylphosphoryl thiochloride preparation method without waste residue

Examples

Experimental program
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Effect test

Embodiment 1

[0025] In a 1000ml four-neck flask with an air duct, a cooling device, and a thermometer, 310g of diethyl chlorophosphite, 372g of O, O-diethyl phosphorodithioate, and 2g of aluminum chloride were successively put in; Slowly raise the temperature to 35°C, feed 164g of chlorine gas within 4 hours, keep it warm for 4 hours, use nitrogen to drive away the excess chlorine and hydrogen chloride gas; stir intermittently, quickly cool down to 25°C; filter at 25°C to obtain O,O- Diethyl thiophosphoryl chloride 735g, the content is 98%; Calculated with diethyl chlorophosphite, the yield is 96%.

Embodiment 2

[0027] In a 1000ml four-neck flask with an air duct, a cooling device, and a thermometer, 310g of diethyl chlorophosphite, 372g of O, O-diethyl phosphorodithioate, and 2g of aluminum chloride were successively put in; Slowly raise the temperature to 35°C, feed 164g of chlorine gas within 4 hours, keep it warm for 4 hours, use nitrogen to drive away the excess chlorine and hydrogen chloride gas; cool down to 25°C; filter at 25°C, wash the filtrate with water, and separate to obtain O,O -Diethylphosphorylthiochloride 715g, content is 99.5%; Calculated yield is 95% with diethyl chlorophosphite.

Embodiment 3

[0029] Into a 1000ml four-neck flask with air duct, cooling device and thermometer, put 310g of diethyl chlorophosphite, 372g of O,O-diethyl phosphorodithioate and 0.5g of aluminum chloride in sequence. and the last batch of filter residue 2.5g; slowly warm up to 35°C, feed 164g of chlorine gas within 4 hours, keep warm for 4 hours, use nitrogen to drive away the excess chlorine and hydrogen chloride gas; intermittently stir, quickly cool down to 25°C; at 25°C O, O-diethylphosphorothiochloride 735g was obtained by filtration at a lower temperature, with a content of 98%; the yield was 96% based on diethyl chlorophosphite.

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Abstract

The invention discloses a method for preparing O, O-dialkylthiophosphoryl chloride without waste residue, which is characterized in that: the method comprises using dialkyl chlorophosphite as an intermediate, and reacting with a strong Lewis acid metal chloride under the action of a strong Lewis acid metal chloride O, O-dialkyl phosphorothioate is chlorinated to prepare O, O-dialkylphosphorothiochloride of the following general structure: the chemical reaction equation is as follows: the invention provides a simple process route, reaction Mild conditions, simple post-treatment, low production cost, and a process method for preparing high-content O, O-dialkylphosphoryl thiochloride, which is convenient for industrial transformation; the method eliminates or reduces pollution, strictly controls the process and eliminates post-treatment Generation of sticky sulfur residues.

Description

technical field [0001] The invention relates to a method for preparing O, O-dialkylphosphoryl thiochloride without waste residue. Background technique [0002] O, O-dialkylphosphoryl thiochloride is an important intermediate in the production of organophosphorus pesticides and cephalosporins. [0003] At present, the phosphorus pentasulfide method generally adopted at home and abroad has a serious deficiency in conversion rate and content, and produces a large amount of difficult-to-handle viscous sulfur waste residue, and the pollution is serious, and the treatment difficulty is large (referring to US5278331; CN101130554); Thiophosphoryl chloride developed by Bayer The method reacts under a large amount of alkyl alcohol, and the heat of reaction is large, and must be maintained at about 0°C for reaction, with high energy consumption and low product content (referring to US5948930). Contents of the invention [0004] The purpose of the present invention is to overcome the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/20
Inventor 赵雪松陈巧玲
Owner 秦小林
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