Liquid phase circulation method in synthesis of thionyl chloride

A technology of thionyl chloride and liquid phase circulation, applied in the direction of sulfur and halogen compounds, etc., can solve the problems of complex process, large investment, and difficulty in obtaining high purity.

Active Publication Date: 2008-10-15
JIANGXI SELON INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] (1) Phosphorus pentachloride reacts with sulfur dioxide, the process is simple, but SOCl 2 with POCl 3 Difficult to separate, difficult to obtain high-purity SOCl 2 ;
[0010] (2) Using antimony chloride etc. as a catalyst, sulfur chloride reacts with chlorosulfonic acid, which is widely used in China at present, with complex process and large investment;
[0014] However, in the published literature, although it is proposed that the closed internal circulation method is used for production, as a large-scale engineering project, there is no specific technical scheme for how to produce thionyl chloride by the closed internal circulation method. In view of this , the present invention is proposed

Method used

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  • Liquid phase circulation method in synthesis of thionyl chloride
  • Liquid phase circulation method in synthesis of thionyl chloride
  • Liquid phase circulation method in synthesis of thionyl chloride

Examples

Experimental program
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Embodiment 1

[0091] A method for liquid phase circulation in the synthesis of thionyl chloride, comprising:

[0092] (1) The crude product sulfur oxychloride whose content of sulfur oxychloride accounts for 68% of the crude product sulfur oxychloride total amount is vulcanized in a vulcanization kettle, and also contains 15% sulfur dichloride in the crude product sulfur oxychloride , the temperature in the vulcanization kettle is that the residual temperature of the crude product thionyl chloride is 80° C., and the pressure is normal pressure. In the crude product thionyl chloride, add sulfur that is not excessive relative to the sulfur dichloride therein, and the addition of sulfur The amount is 80% of the amount of sulfur required for the complete reaction with the sulfur dichloride in the crude product thionyl chloride to obtain the sulfided crude product thionyl chloride; its components are: the content of thionyl chloride is 50% , the sulfur dichloride content is 15%, and the sulfur m...

Embodiment 2

[0103] (1) The crude product sulfur oxychloride whose content of sulfur oxychloride accounts for 65% of the crude product sulfur oxychloride is vulcanized in a vulcanization kettle, and the crude product sulfur oxychloride also contains 20% of sulfur dichloride , the temperature in the vulcanization kettle is that the residual temperature of the crude product thionyl chloride is 60° C., and the pressure is normal pressure. In the crude product thionyl chloride, sulfur that is not excessive relative to the sulfur dichloride therein is added, and the addition of sulfur The amount is 88% of the amount of sulfur required for the complete reaction of sulfur dichloride in the crude product thionyl chloride, so that other substances in the crude product thionyl chloride are converted into sulfur monochloride except thionyl chloride, Obtain the crude product thionyl chloride after sulfidation, in the crude product thionyl chloride after described sulfidation, its each component is: the...

Embodiment 3

[0113] A method for liquid phase circulation in the synthesis of thionyl chloride, comprising:

[0114] (1) Vulcanize the crude product sulfur oxychloride whose content of sulfur oxychloride accounts for 68% of the crude product sulfur oxychloride total amount in a vulcanization kettle, and also contain 25% of sulfur dichloride in the crude product sulfur oxychloride , the temperature in the vulcanization kettle is that the residual temperature of the crude product thionyl chloride is 70° C., and the pressure is normal pressure. To the crude product thionyl chloride, add sulfur that is not excessive relative to the sulfur dichloride therein, and the addition of sulfur The amount is 98% of the amount of sulfur required for the complete reaction of sulfur dichloride in the crude product thionyl chloride, and other substances in the crude product thionyl chloride except thionyl chloride are converted into sulfur monochloride to obtain The crude product sulfur oxychloride after vu...

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Abstract

The invention relates to a liquid phase circulation method for synthesizing thionyl chloride. Specifically, the method comprises a process that the condensate of a crude product of the thionyl chloride and the purified mixed liquid of the crude product of the thionyl chloride in a degassing device are vulcanized and distilled, and then the distilled tower bottom residual liquid is again pumped to the sulfur dichloride for synthesis, thereby forming the fully-closed and full-circulation method for synthesizing the thionyl chloride.

Description

technical field [0001] The present invention relates to a method for liquid phase circulation in the synthesis of thionyl chloride, specifically, the method includes the condensate from the crude thionyl chloride to the purified crude oxychloride in a degasser The sulfone mixed liquid is then vulcanized and rectified, and the residual liquid at the bottom of the rectified tower is re-pumped to the synthesis process of sulfur dichloride, thereby forming the synthesis method of the fully closed and full cycle thionyl chloride. Background technique [0002] Thionyl chloride is very important in organic synthesis. It is an intermediate raw material for the synthesis of pesticides, medicines, photosensitive materials and polymer intermediates. The prior art discloses some technical solutions for the synthesis and purification of thionyl chloride, including: [0003] ZL95110380 discloses a kind of manufacture method of thionyl chloride, this method is to utilize sulfur dioxide and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/45
Inventor 汪国清汪新泉戴恒文潘英曙李世群郑小辉刘朔
Owner JIANGXI SELON INDAL
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