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Method for removing methyl dichlorosilane and silicon tetrachloride impurities in trimethylchlorosilane

A technology of trimethylchlorosilane and methyldichlorosilane is applied in the field of separation and purification of organosilicon monomers, which can solve the problems of high number of separation theoretical plates and large energy consumption, and achieves simple process, low energy consumption, high energy consumption and the like. The effect of efficiency recovery

Active Publication Date: 2021-08-24
TIANJIN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The object of the present invention is to overcome the existence of prior art on the separation and purification method of the mixture of methyldichlorosilane, silicon tetrachloride and trimethylchlorosilane The number of separation theoretical plates is high and the energy consumption is large. The addition reactant with terminal unsaturated bond and methyldichlorosilane is used for addition hydrosilylation reaction. The reaction product is easy to combine with silicon tetrachloride-trimethyl Separation of chlorosilane to remove methyldichlorosilane, and then use lower alcohol as an esterification agent to partially esterify silicon tetrachloride to achieve separation from trimethylchlorosilane

Method used

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  • Method for removing methyl dichlorosilane and silicon tetrachloride impurities in trimethylchlorosilane
  • Method for removing methyl dichlorosilane and silicon tetrachloride impurities in trimethylchlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In this application example, acetylene is used as the reactant for hydrosilylation, and ethanol is used for esterification of lower alcohols. The hydrosilylation reaction involved is

[0039] SiHCH 3 Cl 2 +C 2 h 2 →CH 3 Si(CHCH 2 )Cl 2

[0040] To obtain methyl vinyl dichlorosilane;

[0041] The partial esterification reaction involved is

[0042] SiCl 4 +C 2 h 5 OH→SiCl 3 OC 2 h 5 +HCl

[0043] SiCl 3 OC 2 h 5 +C 2 h 5 OH→SiCl 2 (OC 2 h 5 ) 2 +HCl

[0044] SiCl 2 (OC 2 h 5 ) 2 +C 2 h 5 OH→SiCl(OC 2 h 5 ) 3 +HCl

[0045] The complete esterification reactions involved are:

[0046] SiCl(OC 2 h 5 ) 3 +C 2 h 5 OH→Si(OC 2 h 5 ) 4 +HCl

[0047] A small amount of monomethyltrichlorosilane undergoes a step-by-step esterification reaction similar to silicon tetrachloride.

[0048] (1) Hydrosilylation reaction. In the reactor of 10L, add the raw material of 5kg, the raw material composition is that the monomethyldichlorosilane conte...

Embodiment 2

[0052] In this application example, the hydrosilylation reactant is 3-chloropropene, and the esterified lower alcohol is ethanol. The hydrosilylation reaction involved is:

[0053] SiH(CH 3 )Cl 2 +C 3 h 5 Cl→Si(C 3 h 5 Cl)CH 3 Cl 2

[0054] To obtain methyl chloropropyl dichlorosilane;

[0055] The partial esterification reaction involved is

[0056] SiCl 4 +C 2 h 5 OH→SiCl 3 OC 2 h 5 +HCl

[0057] SiCl 3 OC 2 h 5 +C 2 h 5 OH→SiCl 2 (OC 2 h 5 ) 2 +HCl

[0058] SiCl 2 (OC 2 h 5 ) 2 +C 2 h 5 OH→SiCl(OC 2 h 5 ) 3 +HCl

[0059] The complete esterification reactions involved are:

[0060] SiCl(OC 2 h 5 ) 3 +C 2 h 5 OH→Si(OC 2 h 5 ) 4 +HCl

[0061] A small amount of monomethyltrichlorosilane undergoes a step-by-step esterification reaction similar to silicon tetrachloride.

[0062] (1) Hydrosilylation reaction. In the reactor of 10L, add the raw material of 5kg, the raw material composition is that the monomethyldichlorosilane content ...

Embodiment 3

[0066] In this application example, styrene is used as the reactant for hydrosilylation, and n-propanol is the esterified lower alcohol. The hydrosilylation reaction involved is:

[0067] HSiCH 3 Cl 2 +PhCH=CH 2 →CH 3 (PhCH 2 CH 2 ) SiCl 2

[0068] Obtain methylethylphenyldichlorosilane;

[0069] The partial esterification reaction involved is

[0070] SiCl 4 +C 3 h 7 OH→SiCl 3 OC 3 h 7 +HCl

[0071] SiCl 3 OC 3 h 7 +C 3 h 7 OH→SiCl 2 (OC 3 h 7 ) 2 +HCl

[0072] SiCl 2 (OC 3 h 7 ) 2 +C 3 h 7 OH→SiCl(OC 3 h 7 ) 3 +HCl

[0073] The complete esterification reactions involved are:

[0074] SiCl(OC 3 h 7 ) 3 +C 3 h 7 OH→Si(OC 3 h 7 ) 4 +HCl

[0075] A small amount of monomethyltrichlorosilane undergoes a step-by-step esterification reaction similar to silicon tetrachloride.

[0076] (1) Hydrosilylation reaction. In the reactor of 10L, add the raw material of 5kg, the raw material composition is that the monomethyldichlorosilane content...

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Abstract

The invention relates to a method for removing methyl dichlorosilane and silicon tetrachloride impurities in trimethylchlorosilane. The method comprises three parts of hydrosilylation reaction, partial esterification reaction and complete esterification reaction. The method comprises the following steps: firstly, adding a trimethylchlorosilane mixture containing methyl dichlorosilane and silicon tetrachloride impurities and hydrosilylation reactants into a reactor for hydrosilylation reaction, enabling the reacted product to enter a separation system, and separating the excess reactants and the hydrosilylation products by adopting a distillation or rectification mode, so as to leave a mixture of trimethylchlorosilane and silicon tetrachloride; then adding low-carbon alcohol as an esterifying agent to carry out partial esterification reaction on the silicon tetrachloride in the mixture, enabling the reacted product to enter a separation system, and separating out the partial esterification product of the silicon tetrachloride by adopting a rectification mode, so as to obtain purified trimethylchlorosilane; and finally, further completely esterifying a part of the esterification product to obtain a valuable tetraalkoxy silicon product. High-efficiency recovery of trimethylchlorosilane is realized, and high-value utilization is also realized.

Description

technical field [0001] The invention belongs to the field of separation and purification of organosilicon monomers, in particular to a technology for refining trimethylchlorosilane containing methyldichlorosilane and silicon tetrachloride impurities in organosilicon synthesis monomers. Background technique [0002] Organochlorosilanes are mainly produced by direct synthesis, and the crude chlorosilanes produced contain various components. The monomers of chlorosilanes can be obtained by distilling and separating the crude chlorosilanes, and then made into the intermediate polysiloxane of organosilicon materials. This is the most critical intermediate in the silicone industry. No matter which method is used to produce organochlorosilane monomers, the obtained products are multi-component mixed products. The separation and purification of mixed monomers occupy an important position in the organic silicon industry and its equipment investment ratio. The content and boiling poi...

Claims

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Application Information

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IPC IPC(8): C07F7/12C07F7/20C07F7/04C07F7/18C07F7/14C07F7/02
CPCC07F7/12C07F7/20C07F7/04C07F7/18C07F7/14C07F7/025
Inventor 许春建曹咏军曾宪友杨成勇何永超
Owner TIANJIN UNIV
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