Method for preparing O,O-ethyl thioether substituted phosphorus oxychloride

Abstract

The invention relates to a method for preparing O,O-diethyl thiophosphoryl chloride (DETC), comprising the steps of reacting the raw material of phosphorus pentasulfide with anhydrous alcohol to obtain O,O-diethyl phosphorodithioate (referred to as ethyl sulfide); reacting with chlorine gas to obtain crude O,O-diethyl thiophosphoryl chloride; performing desulfuration of the crude O,O-diethyl thiophosphoryl chloride with ferric oxide desulfuration catalyst at room temperature to obtain desulfurized O,O-diethyl thiophosphoryl chloride and crystalline sulfur; and refining the desulfurized O,O-diethyl thiophosphoryl chloride by the steam distillation method to obtain O,O-diethyl thiophosphoryl chloride with high purity (over 99.5%). The method has the advantages of environmentally friendly production process, and high product purity.

Description

technical field

[0001] The invention belongs to the field of industrial preparation of organophosphorus fine chemicals, and in particular relates to a method for preparing O, O-diethylthiophosphoryl chloride (ethyl chloride for short). Background technique

[0002] The current industrial method is to use phosphorus pentasulfide and absolute ethanol as the main raw materials, obtain crude ethyl chloride through sulfidation and chlorination, then wash and separate with sodium sulfite solution and sodium sulfide solution to obtain the refined ethyl chloride intermediate. During the production process, the waste water produced has the characteristics of high concentration of organic matter, deep color, high toxicity, and difficult biodegradation. The production of 1 ton of product produces 9 tons of concentrated mother liquor and dilute waste water (of which 3 tons of concentrated mother liquor are produced per ton of product) . In 2002, Zheng Zhiming, Xu Zhifa, and Lin Hu repo...

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