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

A technology of ethylphosphorothioate and diethylphosphorodithioate, which is applied in the field of industrial preparation of organophosphorus fine chemicals, can solve the problem of not fundamentally achieving no sulfur-containing wastewater discharge, and achieve desulfurization conditions mild effect

Inactive Publication Date: 2010-12-22
湖北蕲农化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Although the above-mentioned schemes have reduced the content of harmful components such as sulfur in sulfur-containing wastewater to a certain extent, they have not fundamentally achieved no discharge of sulfur-containing wastewater

Method used

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] A kind of preparation O, the method for O-diethyl thiophosphoryl chloride, it comprises the steps:

[0045] 1) synthesis of ethyl chloride crude product:

[0046] ①Ethylation: Add 100mL of ethyl sulfide mother liquor into a 500mL four-neck flask equipped with a stirrer, thermometer, reflux condenser and dropping funnel, and directly add 30g of phosphorus pentasulfide under stirring; The quality of the mass is 0.03% of the mass of phosphorus pentasulfide, the catalyst hydroxymethylpyridine is selected, and the temperature is controlled to add the catalyst hydroxymethylpyridine at 5° C., stirring; the molar ratio of phosphorus pentasulfide and dehydrated alcohol is 1: 4.0 to select dehydrated alcohol, dropwise Dehydrated ethanol, the temperature is controlled at 5 ° C, after the dropwise addition, keep warm for 20 minutes, cool to room temperature, filter to obtain light-colored and transparent O, O-diethyl phosphorodithioate (abbreviated as ethyl sulfide, i.e. filtrate),...

Embodiment 2

[0056] A kind of preparation O, the method for O-diethyl thiophosphoryl chloride, it comprises the steps:

[0057] 1) synthesis of ethyl chloride crude product:

[0058] ①Ethylation: Add 150mL of ethyl sulfide mother liquor into a 500mL four-neck flask equipped with a stirrer, thermometer, reflux condenser and dropping funnel, and directly add 60g of phosphorus pentasulfide under stirring; The quality of the mass is 0.1% of the mass of phosphorus pentasulfide, the catalyst hydroxymethylpyridine is selected, and the temperature is controlled to add the catalyst hydroxymethylpyridine at 25° C., stirring; the molar ratio of phosphorus pentasulfide and dehydrated alcohol is 1: 4.1 to select dehydrated alcohol, dropwise Dehydrated ethanol, the temperature is controlled at 25 ° C, after the dropwise addition, keep warm for 40 minutes, cool to room temperature, filter to obtain light-colored and transparent O, O-diethyl phosphorodithioate (referred to as ethyl sulfide, i.e. filtrate)...

Embodiment 3

[0068] A kind of preparation O, the method for O-diethyl thiophosphoryl chloride, it comprises the steps:

[0069] 1) synthesis of ethyl chloride crude product:

[0070]①Ethylation: Add 180mL of ethyl sulfide mother liquor into a 500mL four-necked flask equipped with a stirrer, thermometer, reflux condenser and dropping funnel, and directly add 80g of phosphorus pentasulfide under stirring; The quality of the mass is 0.5% of the mass of phosphorus pentasulfide, the catalyst hydroxymethylpyridine is selected, and the temperature is controlled to add the catalyst hydroxymethylpyridine at 30° C., stirring; the molar ratio of phosphorus pentasulfide and dehydrated alcohol is 1: 4.2 to select dehydrated alcohol, dropwise Dehydrated ethanol, the temperature is controlled at 40 ° C, after the dropwise addition, keep warm for 60 minutes, cool to room temperature, filter to obtain light-colored and transparent O, O-diethyl phosphorodithioate (abbreviated as ethyl sulfide, i.e. filtrate...

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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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/20
Inventor 陈金芳王新洪陈启明邹菁
Owner 湖北蕲农化工有限公司
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