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New vinyl alkoxy silane preparation process

A technology of vinyl alkoxysilane and alkoxysilane, which is applied in the field of new synthetic technology of vinyl alkoxysilane, can solve problems such as poor economy, underutilization of chlorine resources, negative environmental impact, etc., and achieve improvement The effect of the addition reaction rate

Active Publication Date: 2016-03-02
ZHEJIANG KAIHUA SYNTHETIC MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The first method adopts vinyl chlorosilane as a raw material, and the price is high; at the same time, the hydrogen chloride produced is treated in the form of waste acid, which is economical, chlorine resources are not fully utilized, and waste acid increases the difficulty of processing, causing environmental damage certain negative impact
CN1320600A has reported a kind of preparation method of vinyltrimethoxysilane, and hydrogen chloride gas is generated in the production process, and its hydrogen chloride is absorbed by lye, which increases production cost
CN101012237A has reported the synthesis of vinyl alkoxysilane by hydrosilylation addition method, but in the addition process, inert solutions such as toluene, chlorobenzene and petroleum ether are used as solvents, as additional new substances introduced will affect the vinyl alkoxy silane. The quality of the base silane product increases the difficulty of the post-processing of the product, and at the same time faces the problem of dealing with by-products

Method used

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  • New vinyl alkoxy silane preparation process

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Effect test

Embodiment 1

[0032] Put the solvent bis(triethoxy)silylethane into the reaction kettle, add the catalyst, raise the temperature to 70°C, then put the triethoxysilane into the addition kettle and open the acetylene inlet valve to start the reaction. The reactor pressure was 30kpa, and when the reactor pressure began to slowly rise to 50kpa, the reaction was stopped. The feed liquid is poured into a rectification tower for rectification, vinyltriethoxysilane is extracted from the top of the tower, and bis(triethoxy)silylethane, a by-product at the bottom of the tower, is recovered and used as a reaction solvent. The product yield of vinyltriethoxysilane is 92.9%, and the purity is more than 99%.

Embodiment 2

[0034] The trichlorosilane and methanol obtained by the reaction of hydrogen chloride and silicon powder at 230°C to 260°C are pumped into the double-tower reactor respectively with a metering pump, the temperature is raised to 40°C, and the reaction circulation pump is turned on. The hydrogen chloride produced in the process passes through the cryogenic , and return to the trichlorosilane synthesis device after compression. After reacting for 6 hours, the solution was neutralized and rectified to obtain trimethoxysilane with a yield of 81%. Put the solvent bis(trimethoxy)silylethane into the reaction kettle, add the catalyst, raise the temperature to 70°C, then put the trimethoxysilane into the addition kettle and open the acetylene inlet valve to start the reaction. The reactor pressure was 30kpa, and when the reactor pressure began to slowly rise to 50kpa, the reaction was stopped. The feed liquid is poured into a rectification tower for rectification, vinyltrimethoxysilan...

Embodiment 3

[0036] The trichlorosilane and ethanol obtained by the reaction of hydrogen chloride and silicon powder at 230°C to 260°C are pumped into the double-tower reactor respectively with a metering pump, the temperature is raised to 80°C, and the reaction circulation pump is turned on. The hydrogen chloride produced in the process passes through the cryogenic , and return to the trichlorosilane synthesis device after compression. After reacting for 6 hours, the solution was neutralized and rectified to obtain triethoxysilane with a yield of 86%. Put the solvent bis(triethoxy)silylethane into the reaction kettle, add the catalyst, raise the temperature to 85°C, then put the triethoxysilane into the addition kettle and open the acetylene inlet valve to start the reaction. The reactor pressure was 30kpa, and when the reactor pressure began to slowly rise to 50kpa, the reaction was stopped. The feed liquid is poured into a rectification tower for rectification, vinyltriethoxysilane is ...

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Abstract

The present invention discloses a new vinyl alkoxy silane preparation process, which is characterized in that hydrogen chloride produced during a preparation process is adopted as a reactant to synthesize an initial raw material trichlorosilane, the hydrogen chloride is recycled, and the byproduct bis(trialkoxy)silyl ethane is adopted as a reaction solvent during a hydrogen silicon addition process, such that the byproduct emission is reduced, the new impurity introduction is avoided, and the product purity is improved. According to the present invention, the new process has characteristics of stable production, simple preparation process, and mild reaction conditions, and the yield of the product vinyl alkoxy silane is high, and the product purity is more than 99%.

Description

technical field [0001] The invention relates to a new synthesis process of vinyl alkoxysilane, which belongs to the field of chemical synthesis. Background technique [0002] Vinyl alkoxysilane is a widely used silane coupling agent. There are two main synthesis methods: (1) alcoholysis reaction of vinyl chlorosilane with methanol or ethanol; (2) acetylene and alkoxysilane A hydrosilylation reaction occurs. [0003] The first method adopts vinyl chlorosilane as a raw material, and the price is high; at the same time, the hydrogen chloride produced is treated in the form of waste acid, which is economical, chlorine resources are not fully utilized, and waste acid increases the difficulty of processing, causing environmental damage Certain negative effects. CN1320600A reports a method for preparing vinyltrimethoxysilane. During the production process, hydrogen chloride gas is generated, and the hydrogen chloride gas is absorbed by lye, which increases the production cost. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 陈道伟郑云峰李巧汪玉林侯建超
Owner ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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