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Gas phase circulation method in synthesis of thionyl chloride

A technology of thionyl chloride and gas phase circulation, which is applied in the direction of sulfur and halogen compounds, and can solve problems such as difficult separation, complicated process, and difficult to obtain high purity

Active Publication Date: 2009-04-22
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 there is a proposal to adopt the closed internal circulation method 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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  • Gas phase circulation method in synthesis of thionyl chloride
  • Gas phase circulation method in synthesis of thionyl chloride

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Effect test

Embodiment 1

[0084] This embodiment is to describe the method of using the gas released from the crude product condenser as a part of the source of synthesis gas for thionyl chloride in the present invention, and then enter the thionyl chloride synthesis reactor for recycling, thereby completing the gas phase cycle. The method includes :

[0085] (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 78°C of the residual temperature of the crude product thionyl chloride, and the pressure is normal pressure. To the crude product thionyl chloride, no excess sulfur is added relative to the sulfur dichloride therein, and the amount of sulfur added is For 80% of the amount of sulfur required for the complete reaction with sulfur dichlori...

Embodiment 2

[0095] This embodiment is to describe the method of using the gas extracted from the crude product degassing and purification kettle as a part of the raw material source of the thionyl chloride synthesis gas in the present invention, and re-entering the thionyl chloride synthesis kettle 2 for recycling, thereby completing the gas phase cycle. . The method is as follows:

[0096] As described in step (5) of Example 1, the mixed gas of thionyl chloride is condensed in the crude product condenser at 38°C, and the content of thionyl chloride in the obtained condensed product is 65%. The sulfur content is 25%, and the chlorine gas is 10%. The condensed product is degassed and purified in the crude product degassing purification kettle at a temperature of 90°C and a pressure of 0.02Mpa to obtain the crude product sulfur oxychloride, the crude product sulfur oxychloride Then proceed to the next cycle. And the SO released from the degassing purification kettle 2 content of 25%, chl...

Embodiment 3

[0098] This embodiment is to describe the method of using the gas discharged from the rectification tower as a part of the source of synthesis gas for thionyl chloride in the present invention, and then enter the thionyl chloride synthesis tank for recycling, thereby completing the gas phase cycle. The method is as follows:

[0099] As described in embodiment 1 step (2), the crude product sulfur oxychloride after sulfidation carries out rectification in rectification tower, obtains sulfur oxychloride and mixed high boiler and tail gas, and the gas contained in this tail gas has Sulfur dioxide (about 45%), thionyl chloride (about 45%), chlorine (about 2%), and other non-condensable gases (about 8%). The mixed high boilers are discharged from the tower directly to the kettle, and then the mixed high boilers are sent to the sulfur dichloride synthesis kettle through a pump to complete the liquid phase circulation. The tail gas is mainly sulfur dioxide and chlorine, which are sen...

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Abstract

The invention relates to a method of gas phase in the synthesis of thionyl chloride, and particularly includes synthesizing sulfur dichloride by adding chlorine to sulfur monochloride, synthesizing crude thionyl chloride gas of light concentration by adding chlorine and sulfur dioxide, then subjecting the thionyl chloride gas to condensation, desaeration, purification, sulfuration and distillation to obtain the sulfur monochloride, and then rectifying the sulfur monochloride, thereby representing the method for all gases to enter the circulated use during the whole process.

Description

technical field [0001] The present invention relates to a gas-phase circulation method in the synthesis of thionyl chloride. Specifically, it comprises the synthesis of sulfur dichloride from sulfur monochloride plus chlorine gas, and the synthesis of crude product chlorination with a lower concentration from sulfur dichloride plus chlorine gas and sulfur dioxide. The sulfoxide gas is then condensed, degassed and purified, sulfurized, distilled out of sulfur monochloride and rectified. In the whole link, all the gas enters the method of recycling. 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 uti...

Claims

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Application Information

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Patent Type & Authority Patents(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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