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Production method for preparing trialkoxysilane by adopting direct method

A technology of trialkoxysilane and production method, applied in directions such as organic silicon compounds

Active Publication Date: 2015-03-04
湖北武大有机硅新材料股份有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method involves extractive distillation, azeotropic distillation or adding organic or inorganic substances to prevent the generation of azeotrope, so as to improve the stability of trimethoxysilane, etc. These methods are not ideal.

Method used

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  • Production method for preparing trialkoxysilane by adopting direct method
  • Production method for preparing trialkoxysilane by adopting direct method
  • Production method for preparing trialkoxysilane by adopting direct method

Examples

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preparation example Construction

[0101] The preparation of the above-mentioned silicon-copper intermetallic compound catalyst is completed by the following three-step process:

[0102] The first step: first, the precursor for preparing the catalyst——copper compound and silicon powder are mixed evenly in the presence of an inert heat carrier, so that the copper compound is evenly distributed and adsorbed on the surface of the silicon powder.

[0103] The second step: the uniform mixture of copper compound, silicon powder and heat carrier is placed in the reaction device for preparing the catalyst, under the protection of an inert gas, evenly stirred and heated, and heated to a suitable temperature for a certain period of time to form a brown sticky Thick intermediates for preparing catalysts—silicon-copper composites are packaged and sealed in plastic containers under inert gas and stored for later use.

[0104] The third step: the catalyst intermediate silicon-copper compound prepared by the first two steps o...

Embodiment 1

[0132] Embodiment 1 catalyst intermediate-A and its activation

[0133] (1) 100 parts of cuprous chloride and 60-150 parts of chemical silicon powder are mixed evenly in the presence of 100 parts of inert heat carrier by mass parts, so that the compound of copper is evenly distributed and adsorbed on the surface of silicon powder;

[0134] (2) The homogeneous mixture of copper compound, silicon powder and heat carrier is placed in the reaction device for preparing the catalyst, under the protection of inert gas, evenly stirred and heated, and the temperature is raised to 220°C-260°C for 8-12h to form a The brown viscous intermediate used to prepare the catalyst—silicon-copper composite, is packaged and sealed in a plastic container under an inert gas and stored for later use;

[0135] (3) Put the catalyst intermediate silicon-copper compound prepared by the first two steps in a glass reactor, under the protection of an inert gas, and raise the temperature under even stirring. ...

Embodiment 2

[0136] Embodiment 2 catalyst intermediate-B and its activation

[0137] (1) 100 parts of cuprous oxide and 60-150 parts of chemical silicon powder are mixed evenly in the presence of 100 parts of inert heat carrier by mass parts, so that the compound of copper is evenly distributed and adsorbed on the surface of silicon powder;

[0138] (2) Put the homogeneous mixture of copper compound, silicon powder and heat carrier in the reaction device for preparing the catalyst, under the protection of inert gas, uniformly stir and heat, raise the temperature to 220-260°C for 8-12h, and make it form a brown color The viscous intermediate used to prepare the catalyst—silicon-copper composite, is packaged and sealed in a plastic container under an inert gas and stored for later use.

[0139] (3) Put the catalyst intermediate silicon-copper compound prepared by the first two steps in a glass reactor, under the protection of an inert gas, and raise the temperature under even stirring. When ...

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Abstract

The invention provides a production method for preparing trialkoxysilane by adopting a direct method. According to the production method, firstly a copper compound is used as a precursor for preparing a catalyst intermediate body, the catalyst intermediate body is activated to form a silicon-copper intermetallic compound catalyst with catalytic activity, and the silicon-copper intermetallic compound catalyst is applied to industrial production in which the direct reaction of silicon and alcohol is catalyzed by the silicon-copper intermetallic compound catalyst in order to prepare the trialkoxysilane. An intermittent-continuous operation method is adopted to replace intermittent operation process for production, liquid alcohol is added continuously and silicon powder is replenished in batches during production, and synthesis condition is regulated duly so as to adapt to a stable production process. Besides, technological processes such as product separation, purification, suspending agent recycling and tail gas recycling are improved as well. In crude products generated in the overall reaction process, the content of trimethoxy silane is about 80%; the utilization rate of silicon powder in production adopting an intermittent process is as high as 83%; if an improved intermittent-continuous production process is adopted, the utilization rate of the silicon powder can be increased by more than 10%.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and in particular relates to a production method for synthesizing trialkoxysilane by direct reaction of silicon / alcohol and the improvement of related process. Background technique [0002] The traditional production process of trialkoxysilane usually adopts a two-step method. First, silicon is reacted with hydrogen chloride to form trichlorosilane, and then trichlorosilane is alcoholyzed with methanol (or ethanol) to prepare trimethoxysilane or triethoxysilane. , and its reaction formula is as follows: [0003] The first step: Si+3HCl→HSiCl 3 +H 2 ↑+ other chlorosilane by-products; [0004] Step 2: HSiCl 3 +3ROH→HSi(OR) 3 +3HCl↑R=Me, Et and other alkyl groups; [0005] The two-step method to produce trialkoxysilane has a long process flow, large material loss, and the generation of by-product HCl, which will cause equipment corrosion and environmental pollution, and the productio...

Claims

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Application Information

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IPC IPC(8): C07F7/02C07F7/04
Inventor 张先亮廖俊高胜波何运凡刘成刚余攀张柏平余劲张波张彦谦
Owner 湖北武大有机硅新材料股份有限公司
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