Method and device for refining sulfoxide chloride

A refining method, the technology of thionyl chloride, applied in the direction of thionyl chloride, sulfur and halogen compounds, etc., can solve the problems of high by-products, inability to completely separate the rectification tower, etc., and achieve the effect of flexible export of finished products

Active Publication Date: 2015-05-06
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve SO in the prior art 2 Cl 2 , SOCl 2 The problem of incomplete separation and high temperature in

Method used

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  • Method and device for refining sulfoxide chloride

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0034] Example 1:

[0035] The crude product produced by the thionyl chloride synthesis reactor is transported by the pump to the distillation tower 2. The pressure of the distillation tower is 0.002-0.012MPa and the temperature is 77.4-90℃; the heavy components are removed by the distillation tower 2. , SOCl on top of distillation tower 2 2 The purity of the rectification tower 2 is 80%; the top stream of the rectification tower 2 is subjected to sulfur treatment in the first supersulfur tank 3. The pressure of the first supersulfur tank is 0.001-0.002MPa and the temperature is 29-50℃; The first condenser 4 enters the first separator 5 for gas-liquid separation after condensing. The pressure of the first separator is 0.001-0.002MPa and the temperature is 29°C; the gaseous component Cl 2 , SO 2 Into the reaction system for recycling, the top of liquid rectification tower 2 refluxes; SOCl extracted from the side line of rectification tower 2 2 , SO 2 Cl 2 And a small amount of S 2 ...

Example Embodiment

[0036] Example 2:

[0037] The crude product produced by the thionyl chloride synthesis reactor is transported by the pump to the rectification tower 2, the pressure of the rectification tower is 0.002-0.012MPa, the temperature is 90-95℃; the heavy components are removed by the rectification tower 2 , SOCl on top of distillation tower 2 2 The purity of the rectification tower 2 is 80%; the top stream of the rectification tower 2 is over-sulfurized in the first over-sulfur tank 3. The pressure of the first over-sulfur tank is 0.001-0.002MPa, and the temperature is 50-55℃; The first condenser 4 enters the first separator 5 for gas-liquid separation after condensing. The pressure of the first separator is 0.001-0.002MPa and the temperature is 29°C; the gaseous component Cl 2 , SO 2 Into the reaction system for recycling, the top of liquid rectification tower 2 refluxes; SOCl extracted from the side line of rectification tower 2 2 , SO 2 Cl 2 And a small amount of S 2 Cl 2 Enter the f...

Example Embodiment

[0038] Example 3:

[0039] The crude product produced by the thionyl chloride synthesis reactor is transported by the pump to the rectification tower 2, the pressure of the rectification tower is 0.002-0.012MPa, the temperature is 100-120℃; the heavy components are removed by the rectification tower 2 , SOCl on top of distillation tower 2 2 The purity of the rectification tower 2 is 80%; the top stream of the rectification tower 2 is over-sulfurized in the first over-sulfur tank 3. The pressure of the first over-sulfur tank is 0.001-0.002MPa and the temperature is 70-80℃; The first condenser 4 enters the first separator 5 for gas-liquid separation after condensing. The pressure of the first separator is 0.001-0.002MPa and the temperature is 29°C; the gaseous component Cl 2 , SO 2 Into the reaction system for recycling, the top of liquid rectification tower 2 refluxes; SOCl extracted from the side line of rectification tower 2 2 , SO 2 Cl 2 And a small amount of S 2 Cl 2 Enter the ...

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Abstract

The invention relates to a method and a device for refining sulfoxide chloride. The method comprises the following steps: after rectifying a crude product generated in a sulfoxide chloride synthesis step, performing overvulcanization and condensation on the rectified light component, putting a liquid-phase component obtained through gas-liquid separation into a rectification cycle and putting a gas-phase component obtained through gas-liquid separation into a synthesis step cycle; condensing the gas-phase component generated after the rectified light component is subjected to first vacuum distillation and then putting the condensed gas-phase component into the synthesis step cycle, and performing second vacuum rectification on a heavy component; performing overvulcanization and condensation on the light component obtained by virtue of the second vacuum rectification, returning the liquid-phase component obtained through gas-liquid separation to the second vacuum rectification step cycle, and returning the heavy component to the rectification step cycle; putting the gas-phase components obtained in the two stages of vacuum rectification steps into the synthesis step cycle, respectively. According to the method, a tower system sequence is arranged reasonably, the easily decomposable components are separated under vacuum and at a controlled temperature, and the components difficult to separate are cyclically rectified, and therefore, the separation accuracy and the product quality are improved; after multi-stage rectification, the purity of sulfoxide chloride is above 99.9%.

Description

technical field [0001] The invention belongs to the technical field of chemical production, and in particular relates to a method and a device for refining the crude product produced in the synthesis step of thionyl chloride. Background technique [0002] Thionyl chloride (SOCl 2 ) is an important fine chemical product and an intermediate in the synthesis of many chemicals. Because of its strong chlorination and acid chlorination ability, it can significantly improve the utilization of some expensive raw materials. As a chlorination reagent and acyl chloride reagent, thionyl chloride is mainly used in pesticides, medicines, dyes and other industries. It can also be used as a chlorination agent for the synthesis or replacement of alcohols, acid anhydrides, and nitro compounds. It can also be used as a chloracylating agent for the synthesis of compounds such as thiazoline, pyrrolidine, and amides in ring-closing reactions and in some organic synthesis reactions. Catalysts, e...

Claims

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Application Information

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IPC IPC(8): C01B17/45
CPCC01B17/4584
Inventor 陈光辉仇如臣周艳霞李建隆
Owner QINGDAO UNIV OF SCI & TECH
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