Preparation method of vinyl tris(2-methoxyethoxy)silane coupling agent

A technology of methoxyethoxy and silane coupling agents, applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., can solve the problems affecting the quality of vinyl alkoxysilane products, Recycling solvents consumes a lot of energy, and the catalytic system is complicated, etc., to achieve the effects of good selectivity and stability, reduced requirements, and high catalytic efficiency

Inactive Publication Date: 2018-05-22
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] For the synthesis method (2), CN101012237A pointed out that vinyl alkoxysilane was synthesized by hydrosilylation, but inert solutions such as toluene, chlorobenzene, and petroleum ether were used as solvents during the addition process, and these additional new substances introduced It will affect the quality of vinyl alkoxysilane products, increase the difficulty of the post-processing of the products, and the catalytic system of the reaction is complicated. When adding metal platinum complexes as catalysts, co-catalysts need to be added at the same time, resulting in complicated operation processes. Product quality is not high
CN105367598A pointed out that two (trialkoxy) silyl ethanes were used as the reaction solvent in the hydrosilylation process, and this technique required strict separation of products and solvents to ensure product quality, while two (trialkoxy) silyl ethanes The boiling point of alkane is much higher than that of the product, and the energy consumption of recovering the solvent is large

Method used

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  • Preparation method of vinyl tris(2-methoxyethoxy)silane coupling agent
  • Preparation method of vinyl tris(2-methoxyethoxy)silane coupling agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 800 g of vinyl tris (2-methoxyethoxy) silane solvents to a self-made three-mouth long-bottomed reaction vessel with a constant pressure dropping funnel, an acetylene air duct with a bubbler, a thermometer and a condenser tube, and then add 800 g of vinyl tris (2-methoxyethoxy) silane solvent, and then add 200 ml of At a flow rate of / min, dry and purified acetylene was introduced and the temperature began to rise slowly. When the system temperature reached 45°C, 40uL of pt(0) divinyltetramethyldisiloxane solution catalyst was added, and the temperature continued to rise until the system temperature reached 85°C At this time, start to drop a total of 400g of tris(2-methoxyethoxy)hydrosilane at a uniform speed, and finish dropping after 6 hours. base) hydrosilane content is 0.32%, stop feeding acetylene and lower the temperature to obtain the reaction crude product. The reaction crude product was distilled under reduced pressure to obtain 441.2 g of vinyl tris(2-metho...

Embodiment 2

[0030] Add 800 g of vinyl tris (2-methoxyethoxy) silane solvents to a self-made three-port long-bottomed reaction vessel with a constant pressure dropping funnel, an acetylene gas guide tube with a bubbler, a thermometer and a condenser tube, and then add 800 g of vinyl tris (2-methoxyethoxy) silane solvent, and then add 170 ml At a flow rate of / min, dry and purified acetylene was introduced and the temperature began to rise slowly. When the system temperature reached 45°C, 60uL of pt(0) divinyltetramethyldisiloxane solution catalyst was added, and the temperature continued to rise until the system temperature reached 90°C At this time, a total of 400 g of tris(2-methoxyethoxy)hydrosilane was added dropwise at a uniform speed, and the drop was completed in 6.5 hours. Oxygen) hydrosilane content is 0.28%, stop feeding acetylene and lower the temperature to obtain the reaction crude product. The reaction crude product was distilled under reduced pressure to obtain 438.5 g of vi...

Embodiment 3

[0032] Add 800 g of vinyl tris (2-methoxyethoxy) silane solvents to a self-made three-port long-bottomed reaction vessel with a constant pressure dropping funnel, an acetylene gas guide tube with a bubbler, a thermometer and a condenser, and then add 800 g of vinyl tris (2-methoxyethoxy) silane solvent, and then add 220 ml At a flow rate of / min, dry and purified acetylene was introduced and the temperature began to rise slowly. When the system temperature reached 45°C, 60uL of pt(0) divinyltetramethyldisiloxane solution catalyst was added, and the temperature continued to rise until the system temperature reached 95°C At this time, a total of 400g of tris(2-methoxyethoxy)hydrosilane was added dropwise at a constant speed, and the drop was completed after 7 hours. base) hydrosilane content is 0.22%, stop feeding acetylene and lower the temperature to obtain the reaction crude product. The reaction crude product was distilled under reduced pressure to obtain 439.7 g of vinyl tr...

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Abstract

The invention relates to a preparation method of a vinyl tris(2-methoxyethoxy)silane coupling agent. The method comprises the following steps of taking tris(2-methoxyethoxy)chloride silane and acetylene as raw materials, taking a vinyl tris(2-methoxyethoxy)silane product per se as a reaction solvent, and taking a metal platinum complex as a catalyst to perform hydrosilylation reaction. The vinyl tris(2-methoxyethoxy)silane product per se is used as the reaction solvent, the production operation process is simplified, the separation steps of a reaction product are reduced, the production efficiency is improved, the quality and stability of the product are improved, and the vinyl tris(2-methoxyethoxy)silane coupling agent is economical and environmentally friendly.

Description

technical field [0001] The invention relates to a preparation method of vinyl tris(2-methoxyethoxy)silane coupling agent, which belongs to the field of fine chemical industry. Background technique [0002] Organosilicon materials have excellent properties such as high and low temperature resistance, atmospheric aging resistance, water repellency and moisture resistance, electrical insulation and physiological inertness. . Vinyl tris(2-methoxyethoxy)silane is a widely used silane coupling agent in organosilicon materials. At present, there are generally two synthetic methods at home and abroad, and the reaction equations are as follows: [0003] [0004] Method (1) is to use acetylene to add trichlorosilane first to obtain vinyl trichlorosilane, and then esterify to obtain vinyl tri(2-methoxyethoxy) silane; method (2) is to use acetylene to directly add Tris(2-methoxyethoxy)hydrosilane undergoes an addition reaction to obtain vinyltris(2-methoxyethoxy)silane. Compared w...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1876
Inventor 张宇王欣陈其阮少阳陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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