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Method for removing ethyl dichlorosilane impurities in dimethyldichlorosilane

A technology of dimethyldichlorosilane and ethyldichlorosilane is applied in the separation and purification field of the organosilicon industry, and can solve the problems of high energy consumption, large reflux ratio and high number of trays

Active Publication Date: 2021-09-28
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Avoid the traditional separation method relying solely on rectification operation, resulting in high energy consumption, high plate number, large reflux ratio, large equipment investment and other shortcomings

Method used

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  • Method for removing ethyl dichlorosilane impurities in dimethyldichlorosilane
  • Method for removing ethyl dichlorosilane impurities in dimethyldichlorosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0044] The content of ethyldichlorosilane in the feed is 1000ppm, and ethylene is used as the reactant for the reaction, and the isopropanol solution of chloroplatinic acid hydrate is used as the catalyst, and the catalyst concentration is 15ppm. The reactor is a stirred tank reactor with a reaction volume of 5 L, an operating pressure of 0.1 MPaG, and a reaction temperature of 90°C. Control the molar ratio of the circulating amount of reactants to dimethyldichlorosilane to be 8:1, the reaction residence time is 0.2 hours, and the reaction kettle has a jacket, external circulation or internal coil heater. Adjust the amount of heating to stabilize the liquid level of the reactor, add the reactants continuously, and the reaction products enter the rectification system. After delightening, the light component ethylene returns to the reactor in the gas phase, and the remaining mixture of dimethyldichlorosilane and diethyldichlorosilane is refined to obtain dimethyldichlorosilane p...

Embodiment 2

[0050] In this example, acetylene is used as the hydrosilylation reactant, and the content of ethyldichlorosilane in the feed is 1000ppm. The process is similar to the use of ethylene. The isopropanol solution of chloroplatinic acid hydrate is used as the catalyst, and the catalyst concentration is 150ppm. The reactor is a stirred tank reactor with a reaction volume of 5 L, an operating pressure of 0 MPaG, and a reaction temperature of 120°C. Control the molar ratio of the circulating amount of reactants to dimethyldichlorosilane to be 8:1, the reaction residence time is 1 hour, and the reaction kettle has a jacket, external circulation or internal coil heater. Adjust the amount of heating to stabilize the liquid level of the reactor, add the reactants continuously, and the reaction products enter the rectification system. After delighting, the light component acetylene returns to the reactor in the gas phase, and the remaining dimethyldichlorosilane, ethylvinyldichlorosilane ...

Embodiment 3

[0058] The content of ethyldichlorosilane in the feed is 1000ppm, and 1-octene is used as a reactant for the reaction, and a Karstedt catalyst is used with a catalyst concentration of 10ppm. The reactor is a stirred tank reactor with a reaction volume of 5 L, an operating pressure of 1.0 MPaG, and a reaction temperature of 120°C. Control the molar ratio of the circulating amount of reactants to dimethyldichlorosilane to 3:1, the reaction residence time is 0.1 hour, and the reaction kettle has a jacket, external circulation or internal coil heater. Adjust the amount of heating to stabilize the liquid level of the reactor, add the reactants continuously, and the reaction products enter the rectification system. A small amount of light component impurities are recovered after delightening, and then the dimethyldichlorosilane product is obtained after delightening treatment. 1-octene and ethyloctyldichlorosilane continue to be rectified and separated as heavy components, respectiv...

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Abstract

The invention relates to a method for removing ethyl dichlorosilane impurities in dimethyldichlorosilane. A reactor and a separation system are included; a dimethyldichlorosilane feed containing ethyl dichlorosilane and a hydrosilylation reactant are added into a reactor for reaction, an isopropanol solution of chloroplatinic acid hydrate or a Karstedt catalyst is adopted, and a product after the reaction enters the separation system; a rectification mode is adopted, and excessive reactant, dimethyldichlorosilane and hydrosilylation reaction products are separated through light component and heavy component removal operation; and the reacted mixture enters the separation system to be separated, and the dimethyldichlorosilane product is obtained. According to the method, ethyldichlorosilane is converted through reaction, and the characteristic that the boiling point difference between the reactant and the reaction product and dimethyldichlorosilane is large is utilized, so that the system separation difficulty is effectively reduced, the number of theoretical plates and reflux ratio requirements of subsequent rectification separation operation are reduced, the equipment investment is reduced, the energy consumption is greatly reduced, and the industrial application value is relatively high.

Description

technical field [0001] The invention belongs to the field of separation and purification of organic silicon industry, and in particular relates to the refining technology of dimethyl dichlorosilane containing ethyl dichlorosilane impurity. Background technique [0002] Dimethyldichlorosilane is an important organosilicon monomer and the main raw material for the production of high-performance organosilicon compounds. It has high requirements on purity and must strictly control the impurity content. At present, the separation and purification of dimethyldichlorosilane in the industry mostly adopts rectification technology, and the mode of multi-tray and large reflux ratio is generally adopted. After analysis, the key impurity that affects the purity of dimethyldichlorosilane is ethyldichlorosilane. Although the content of ethyldichlorosilane in the synthetic monomer is less than 0.5%, it has a very large impact on the quality of downstream products and must be strict control...

Claims

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Application Information

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IPC IPC(8): C07F7/12C07F7/20
CPCC07F7/12C07F7/20Y02P20/10
Inventor 许春建曾宪友曹咏军杨成勇何永超
Owner TIANJIN UNIV
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