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Interrupter method for producing high-purity methyl sulfonyl chloride

A methylsulfonyl chloride, high-purity technology, applied in the field of organic synthesis in the chemical industry, can solve the problems of high trace impurity content, specific equipment, complex and other problems, and achieve the effects of improving product yield, high product purity, and simple equipment

Inactive Publication Date: 2004-01-07
HEBEI YANUO CHEM IND
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AI Technical Summary

Problems solved by technology

The advantage of the batch method is that the equipment is universal, simple, easy to operate, and trace impurities: such as chloromethanesulfonyl chloride (some users strictly control the content of this impurity) are low in content (for example: the content of this impurity in the crude product of methylsulfonyl chloride is 50ppm), Therefore the product purity of this method is higher (generally all>99.6%), but the shortcoming of this method is that productive rate is on the low side
The advantage of the continuous method is that the yield is higher, and the disadvantage is that the equipment is specific, relatively complicated, difficult to operate, and the content of trace impurities is high (for example: when the method is simulated in the laboratory, chloromethylsulfonyl chloride in the crude product of methylsulfonyl chloride Impurity content > 300ppm)

Method used

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  • Interrupter method for producing high-purity methyl sulfonyl chloride
  • Interrupter method for producing high-purity methyl sulfonyl chloride

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specific Embodiment approach

[0023] The following examples are used to illustrate the present invention, but not to limit the present invention.

Embodiment

[0025] Add 1000KG dimethyl disulfide and 1800KG 30% recovered hydrochloric acid to the 3000L chlorination kettle, after cooling to 20°C, control the temperature in the kettle to be 20-30°C, and then feed chlorine gas. After 20-25 hours of passing chlorine, the end point of the reaction is reached, and the reaction solution is sent to a stratifier to stand for 10-12 hours to separate layers. The stratified crude product is sent to the washing tower of Φ400, and is washed countercurrently with 1000-1100KG30% recovered hydrochloric acid. The crude methanesulfonyl chloride after washing is sent to rectification under reduced pressure, and intermittent rectification is carried out at 40-60 mmHg (absolute), to obtain the finished product of methanesulfonyl chloride (hereinafter referred to as finished product 1).

[0026] Layered to obtain 800-900KG hydrochloric acid aqueous solution and 30% impurity-containing washing hydrochloric acid (1000-1100KG) combined, sent back to the chlor...

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Abstract

The present invention relates to a method for producing high-purity methyl sulfonyl chloride by using intermittent process. In the aqueous solution of hydrochloric acid it uses dimethyl disulfur and chlorine gas and makes them produce reaction to produce methyl sulfonyl chloride. Its reaction yield can be up to 97%, and its product purity is greater than or equal to 99.7%.

Description

technical field [0001] The invention relates to a method for producing high-purity methanesulfonyl chloride by batch method. The invention belongs to the technical field of organic synthesis in the chemical industry. Background technique [0002] In the field of organic synthesis in the chemical industry, methylsulfonyl chloride is a widely used organic synthesis intermediate, which is used to prepare intermediates in pesticides, color display, and pharmaceutical industries, and is also used in large quantities to manufacture methylsulfonic acid. Used in electroplating industry. There are many processes for preparing methanesulfonyl chloride in the prior art, but the common method for producing methanesulfonyl chloride in industry is: chlorine gas and suspended dimethyl disulfide carry out gas-liquid phase reaction in aqueous solution to produce methyl Sulfonyl chloride. There are two kinds of industrial implementation methods in the above-mentioned process route, a kind ...

Claims

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Application Information

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IPC IPC(8): C07C303/16C07C309/80
Inventor 刘晓民
Owner HEBEI YANUO CHEM IND
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