Waste residue-free preparation method of O,O-dialkyl thiophosphoryl chloride

A technology of alkyl phosphorothioate and dialkyl phosphorodithioate, which is applied in the field of waste-free preparation of O,O-dialkyl phosphorothioate chloride, which can solve the problem of difficult to handle viscous sulfur waste residue and large reaction heat generation , low product content and other problems, to achieve the effect of easy industrial transformation, high yield and simple post-processing

Inactive Publication Date: 2013-09-18
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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  • Waste residue-free preparation method of O,O-dialkyl thiophosphoryl chloride
  • Waste residue-free preparation method of O,O-dialkyl thiophosphoryl chloride
  • Waste residue-free preparation method of O,O-dialkyl thiophosphoryl chloride

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 waste residue-free preparation method of O,O-dialkyl thiophosphoryl chloride, which is characterized by comprising the following steps: by taking dialkyl chlorophosphite as an intermediate, performing chlorination with O,O-dialkyl phosphorodithioate under the effect of strong Lewis acid metal chloride to prepare O,O-dialkyl thiophosphoryl chloride with the structural general formula shown in the specification, wherein the chemical equation is shown in the specification. The method for preparing high-content O,O-dialkyl thiophosphoryl chloride, disclosed by the invention, has the advantages of simple process route, mild reaction conditions, simple after-treatment and low production cost, and is convenient for industrial transformation; and the method avoids or reduces pollution, strictly controls the process, saves after-treatment and prevents the generation of viscose waste 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 Applications(China)
IPC IPC(8): C07F9/20
Inventor 秦小林
Owner 秦小林
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