Method and device for impurity removal and purification of dimethyldichlorosilane by reaction and rectification

A technology of dimethyldichlorosilane and reactive distillation, applied in separation methods, chemical instruments and methods, fractionation and other directions, can solve the problems of large investment and cumbersome process, and achieve high-efficiency separation, high purity, and low equipment investment. Effect

Inactive Publication Date: 2020-01-03
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Patent No. CN105906659B also introduces the method of adding hydrogen chloride to react in a fixed-bed reactor first, and then conduct rectification and separation of the product to remove the hydrosilane in dimethyldichlorosilane, which can make the removal of impurities reach more than 99.9% ;The methods introduced above all use fixed-bed reaction first and then rectification to remove hydrosilane, the process is cumbersome and requires a lot of investment

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  • Method and device for impurity removal and purification of dimethyldichlorosilane by reaction and rectification

Examples

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Effect test

example 1

[0036] The crude dimethyldichlorosilane and hexachloroethane enter the reactive distillation column from the upper and lower parts of the reaction section of the reactive distillation column respectively. The reaction section in the column is alternately filled with 1m of wire mesh corrugated packing and structural catalyst from bottom to top. 1m has 4 sections and 8m in total, which plays the role of reactive distillation. The catalyst is a 1% nickel-supported artificial zeolite catalyst, and the number of plates in both the column rectification section and the stripping section is 40. The temperature at the top of the tower is controlled to be between 50°C and 55°C, and the cooling medium of the condenser is circulating water at 28°C. The operating pressure of the reactive distillation column is controlled at 50Kpa, the temperature of the tower reactor is about 90℃, the temperature in the middle reaction section is gradually increased from top to bottom, the temperature in th...

example 2

[0038] The crude dimethyldichlorosilane and chlorobenzene enter the reactive distillation tower from the lower part and the upper part of the reaction section of the reactive distillation tower respectively. The 3 sections of 6m play the role of reactive distillation, the catalyst is a 1% platinum-supported activated carbon catalyst, and the number of plates in both the column rectification section and the stripping section is 40. The temperature at the top of the tower is controlled to be between 50°C and 55°C, and the cooling medium of the condenser is circulating water at 28°C. The operating pressure of the reactive distillation column is controlled at 100Kpa, the temperature of the tower reactor is about 130℃, the temperature in the middle reaction section is gradually increased from top to bottom, the temperature in the reaction section is controlled between 60-70℃, and the reflux ratio at the top of the column is 8. The number of plates in the reactive rectification towe...

example 3

[0039] Example 3: Dimethyldichlorosilane crude material and carbon tetrachloride enter into the reactive distillation tower from the upper and lower parts of the reaction section of the reactive distillation tower respectively, and the reaction section in the tower is alternately filled with wire mesh corrugated packing 1m and 1m from bottom to top. The structural catalyst is 1 m and has 4 sections and 8 m in total, which plays the role of reactive distillation. The catalyst is a 1% palladium-supported alumina catalyst. The temperature at the top of the tower is controlled to be between 50°C and 55°C, and the cooling medium of the condenser is circulating water at 28°C. The operating pressure of the reactive distillation column is controlled at 120Kpa, the temperature of the tower is about 90℃, the temperature of the middle reaction section is gradually increased from top to bottom, the temperature of the reaction section is controlled between 60-70℃, and the reflux ratio at th...

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Abstract

The invention relates to a method and device for impurity removal and purification of dimethyldichlorosilane by reaction and rectification. A dimethyldichlorosilane crude material enters a tower through an inlet pipeline in a reaction section, the temperature of a stripping section is controlled, and the dimethyldichlorosilane crude material enters the reaction section upwards in a gas phase form;a chlorine source reactant enters the tower through a chlorine source reactant inlet pipeline in the reaction section, the temperature of a rectification section is controlled, and the dimethyldichlorosilane crude material enters the reaction section downwards in a liquid phase form; hydrogen-containing silane impurities in the dimethyldichlorosilane crude material react with the chlorine sourcereactant under action of a catalyst to generate a high-boiling-point substance; after the reaction, the high-boiling-point substance is extracted from the tower bottom through a tower bottom extraction pipeline; the chlorine source reactant enters the tower through a reactant return pipeline in the stripping section to supplement the chlorine source reactant, and the condensed gas phase at the tower top is intermittently extracted through an outlet of a gas phase pipeline; a part of the condensed chlorine source reactant flows back to the tower top through a tower top return pipeline, and a part of the condensed chlorine source reactant is extracted through a tower top liquid phase extraction pipeline. Hydrogen-containing silane is enriched by 10-100 times to obtain a high-purity dimethyldichlorosilane product.

Description

technical field [0001] The invention relates to a method for removing impurities by reactive distillation of dimethyldichlorosilane, a raw material for organosilicon production. The dimethyldichlorosilane product in a conventional organosilicon monomer rectification process is purified by a reactive distillation method, and further Obtain ultra-high purity products. Background technique [0002] Organosilicon, that is, organosilicon compound, has both the properties of inorganic and organic materials due to its unique structure, and is a popular material in electronics, textiles, construction and other industries. production is necessary. It is well known that organosilicon is further processed by converting the monomer dimethyldichlorosilane into siloxane polymers with various functional groups and structures through hydrolysis and polycondensation reactions. In order to obtain high-performance organosilicon materials, the purity of the raw material dimethyldichlorosilane...

Claims

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Application Information

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IPC IPC(8): B01D3/14B01D3/00B01J8/04C07F7/20
CPCB01D3/009B01D3/143B01J8/04C07F7/20Y02P20/10
Inventor 黄国强张明鑫
Owner TIANJIN UNIV
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