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Method for inhibiting generation of sulfuryl chloride in thionyl chloride preparation process

A technology for the preparation of thionyl chloride, which is applied in the direction of sulfur and halogen compounds, can solve the problems of increasing equipment investment and energy consumption, high sulfuryl chloride content, and affecting product quality, so as to reduce the content of impurities, sulfur The effect of reducing acid chloride content and improving production efficiency

Inactive Publication Date: 2019-06-07
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the boiling point of thionyl chloride (78.8°C) is very close to the boiling point of sulfuryl chloride (69°C), it is difficult to completely separate thionyl chloride and sulfuryl chloride by conventional rectification methods, resulting in high sulfuryl chloride content in the product, which seriously affects product quality.
[0003] Aiming at the problem of sulfuryl chloride in thionyl chloride: patent US2529671 proposes a method for removing impurities in thionyl chloride with organic solvents; patent US4337235 decomposes sulfuryl chloride by adding sulfur and catalyst aluminum trichloride; patent CN103172031 proposes removing sulfur by activated carbon cracking Acyl chlorides, the above methods are either easy to bring in impurities, or increase equipment investment and energy consumption levels, bringing unnecessary problems to industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] The method for inhibiting the generation of sulfuryl chloride during the preparation of thionyl chloride:

[0013] The raw material mixed gas consisting of disulfide dichloride, sulfur dichloride and chlorine in a ratio of 3:2:1 is passed through a preheater to increase the temperature of the mixed gas to 110 °C, and the raw material mixed gas with a temperature of 120 °C enters the catalytic reactor. Reaction, the crude thionyl chloride produced by the reaction is extracted from the lower part of the catalytic reactor, and the sulfuryl chloride content in the obtained crude thionyl chloride is 0.75%.

Embodiment 2

[0015] During the preparation of thionyl chloride, sulfuryl chloride is inhibited from generating a mixture of 2:1:3. The temperature of the mixture is increased to 130°C through a preheater, and the raw material mixture whose temperature reaches 130°C enters the catalytic reactor for reaction. The crude thionyl chloride is extracted from the lower part of the catalytic reactor, and the sulfuryl chloride content in the obtained crude thionyl chloride is 0.70%.

Embodiment 3

[0017] The method for inhibiting the generation of sulfuryl chloride during the preparation of thionyl chloride:

[0018] The mixed gas consisting of disulfide dichloride, sulfur dichloride and chlorine in a ratio of 2:1:2 is passed through a preheater to increase the temperature of the mixed gas to 100 °C, and the mixed gas whose temperature reaches 100 °C of the raw material enters the catalytic reactor for reaction , the crude thionyl chloride produced by the reaction is extracted from the lower part of the catalytic reactor, and the sulfuryl chloride content in the obtained crude thionyl chloride is 0.80%.

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Abstract

The invention relates to a method for inhibiting generation of sulfuryl chloride in a thionyl chloride preparation process. The temperature of raw material mixed gas consisting of disulfur dichloride,sulfur dichloride and chlorine gas is increased to 100-130 DEG C, then the mixed gas enters a catalytic reactor for carrying out a reaction, and crude product thionyl chloride generated by the reaction is extracted from the lower part of the catalytic reactor, so that the thionyl chloride is obtained, wherein the molar ratio of the disulfur dichloride to the sulfur dichloride to the chlorine gasis (2-3):(1-2):(1-3). The sulfuryl chloride in the crude product thionyl chloride is inhibited to be 0.8% or below, so that quality of the crude product thionyl chloride is effectively improved, the content of impurities is reduced, production efficiency is improved, cost is reduced, and reduction of the content of the sulfuryl chloride in a subsequent refined product is facilitated.

Description

technical field [0001] The invention belongs to the production field of chemical technology, and in particular relates to a method for inhibiting the generation of sulfuryl chloride in the preparation process of thionyl chloride. technical background [0002] At present, most domestic thionyl chloride production enterprises adopt the sulfur dioxide gas-phase method, and in the process of producing thionyl chloride using this method, sulfuryl chloride is inevitably generated. Since the boiling point of thionyl chloride (78.8°C) is very close to that of sulfuryl chloride (69°C), it is difficult to completely separate thionyl chloride and sulfuryl chloride by conventional rectification methods, resulting in the high content of sulfuryl chloride in the product, which seriously affects product quality. . [0003] For the problem of sulfuryl chloride in thionyl chloride: patent US2529671 proposes a method for removing impurities in thionyl chloride with organic solvents; patent U...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/45
Inventor 谢圣斌毕义霞张泰铭张善民马长山李志忠王志国
Owner SHANDONG KAISHENG NEW MATERIALS