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Method and device for removing impurity sulfur dichloride in thionyl chloride

A technology of thionyl chloride and sulfur dichloride, which is applied in the direction of sulfur and halogen compounds, can solve problems such as pipeline blockage, packing blockage in the distillation tower pipeline tower, and gas condensation, etc., to achieve convenient replenishment Effect

Active Publication Date: 2017-12-15
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (1) The specific conditions for the conversion of sulfur dichloride and solid sulfur into sulfur monochloride are not given, and the complete removal of sulfur dichloride cannot be ensured
[0009] (2) When the device is shut down and started up again, due to the temperature drop of the pipeline, the oversulfurization tank and the solid sulfur in it, some of the gas will condense, and the condensed material will wash the solid sulfur to the bottom of the oversulfurization tank, causing the pipeline road congestion, especially in winter
However, when the phenomenon of flushing is serious, it will still cause the blockage of the bottom pipeline of the rectification tower and even the packing in the tower
Moreover, it is very inconvenient to add sulfur by setting the oversulfur tank on the top of the tower more than 20 meters high.
[0010] (3) In the above-mentioned patents, when adding sulfur to the oversulfur tank, the vehicle must be stopped, and the pressure in the oversulfur tank must be discharged to the exhaust gas absorption system before proceeding, and continuous production cannot be realized

Method used

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  • Method and device for removing impurity sulfur dichloride in thionyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-3

[0031] The following devices are used in this embodiment 1-3:

[0032] Such as figure 1 As shown, the device for removing sulfur dichloride impurities in thionyl chloride includes crude product receiving tank 1, crude product receiving tank 1 through pipeline and sulfur distribution tank 2, rectification tower 3, heater 4, oversulfur The tanks 5 are connected in sequence, and a liquid sulfur line 8 is provided on the top of the sulfur distribution tank 2.

[0033] The top of the oversulfur tank 5 is connected with a sulfur feed tank 7 through a pipeline, and a spherical valve 6 is provided on the pipeline between the oversulfur tank 5 and the sulfur feed tank 7.

[0034] The bottom of the supersulfur tank 5 is connected to the crude product receiving tank 1 and the sulfur distributing tank 2 respectively.

Embodiment 1

[0036] The crude product of thionyl chloride is pumped from the crude product receiving tank 1 into the sulfur distributing tank 2, and then liquid sulfur is added to the sulfur distributing tank 2 through the liquid sulfur line 8, so that sulfur dichloride and sulfur are reacted and converted into sulfur monochloride. The sulfur dichloride in the crude thionyl chloride after sulfur was measured to be 2.3%, and it was fed into the rectification tower 3 for rectification and separation under the condition of the top pressure of 4kPa. The thionyl chloride separated at the top Sulfur dichloride enters the heater 4, the temperature rises to 85℃, enters from the bottom of the oversulfur tank 5, after passing through the 700mm high sulfur bed, the sulfur dichloride in the product thionyl chloride at the top of the oversulfur tank 5 is measured The content is 0.003%, which meets the requirements of the industry standard for the color of superior product 1#.

[0037] Wherein, the diamete...

Embodiment 2

[0039] The crude product of thionyl chloride is pumped from the crude product receiving tank 1 into the sulfur distributing tank 2, and then liquid sulfur is added to the sulfur distributing tank 2 through the liquid sulfur line 8, so that sulfur dichloride reacts with sulfur to convert to sulfur monochloride. The sulfur dichloride content in the crude thionyl chloride after sulfur is measured to be 2.0%. It is fed into the rectification tower 3 for rectification separation under the condition of the top pressure of 7kPa. The thionyl chloride separated at the top Sulfur dichloride enters the heater 4, the temperature rises to 88°C, enters from the bottom of the oversulfur tank 5, after passing through the 790mm high sulfur bed, the sulfur dichloride in the product thionyl chloride at the top of the oversulfur tank 5 is measured The content of sulfur is 0.0025%. After 2 hours of continuous operation, the height of the sulfur bed becomes 650mm, and the content of sulfur dichloride...

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Abstract

The invention belongs to the technical field of chemical production, and in particular relates to a method and a device for removing impurity sulfur dichloride in thionyl chloride. The method is as follows: the sulfur oxychloride gas containing 1 to 3% of sulfur dichloride steamed from the top of the rectification tower enters the oversulfur tank for reaction after heating up, the device includes a crude product receiving tank, and the crude product receiving tank passes through the pipeline and the distribution tank. The sulfur tank, rectification tower, heater, and oversulfur tank are connected in sequence, and a liquid sulfur line is installed on the top of the sulfur distribution tank. The invention can reduce the 1-3% sulfur dichloride contained in the thionyl chloride to less than 0.004%, which meets the requirement of 1# color of the superior product in the industry standard; solves the problem of pipeline blockage at the bottom of the oversulfurized tank , to achieve continuous production.

Description

Technical field [0001] The invention belongs to the technical field of chemical production, and specifically relates to a method and a device for removing sulfur dichloride impurities in thionyl chloride. Background technique [0002] Thionyl chloride is a commonly used chlorinating agent. Because the by-products of the reaction are only sulfur dioxide and hydrogen chloride, it is easy to separate from the target product. It is widely used in the synthesis and production of medicines, pesticides, dyes and food additives. In recent years It has also been widely used in the lithium battery industry. As the use of thionyl chloride continues to expand, its quality requirements are getting higher and higher. [0003] Sulfur dichloride is the raw material for the synthesis of thionyl chloride by sulfur dioxide gas phase method, and it is also an impurity in the crude product of thionyl chloride. The reaction formula is Cl 2 +SCl 2 +SO 2 = 2SOCl 2 . Sulfur dichloride is reddish-brown wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/45
Inventor 张善民贾远超张乐毕义霞谢圣斌田恒强孙丰春李志忠王志国
Owner SHANDONG KAISHENG NEW MATERIALS
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