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Vinyl trialkoxy silane coupling agent preparation method

The technology of vinyl trialkoxysilane coupling agent and trialkoxyhydrosilane is applied in the field of preparation of vinyl trialkoxysilane coupling agent, which can solve the problems of poor production safety, complex catalyst system, The problem of low yield, etc., achieves the effect of low cost, high product quality and high molar yield

Active Publication Date: 2014-10-01
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The above methods all use the method of hydrosilylation to synthesize vinyltrialkoxysilane. The reaction conditions are different. There are reactions under high temperature and high pressure, reactions with immobilized catalysts, and reactions under the conditions of adding cocatalysts and various solvents. The yields of the two methods are not high. Although the yield of the latter is relatively high, the catalyst system is complex, and it is necessary to add petroleum ether solvents with low flash points or benzene solvents with relatively high toxicity. The production safety is not good, and requires Separation and recovery of solvent, high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 500 g of 1,2-bistrimethoxysilylethane solvent to a four-necked reaction flask equipped with magnetic stirring, a constant pressure dropping funnel, an acetylene vent tube, a thermometer, and a low-temperature condenser, and then start to slowly pass through it to dry 1. Purified acetylene, after replacing the air in the system, add 80 μmol of Pt(0) divinyltetramethyldisiloxane solution catalyst with a micro-injector, then start to heat up slowly, and continue to pass through acetylene, the speed is controlled at 100ml / min. When the temperature in the reaction system reaches 50° C., 500 g of trimethoxyhydrogensilane raw materials are added dropwise, and the dropping speed is controlled at a constant speed, and the dropping time is 4.5 hours. After the dropwise addition, the reaction was continued for 10 minutes, and then the reaction solution was taken for detection and analysis. When it is detected that the content of trimethoxyhydrogensilane in the reaction soluti...

Embodiment 2

[0027] Add 500 g of 1,2-bistrimethoxysilylethane solvent to a four-necked reaction flask equipped with magnetic stirring, a constant pressure dropping funnel, an acetylene vent tube, a thermometer and a low-temperature condenser, and then start to slowly pass through it to dry 1. Purified acetylene, after replacing the air in the system, add 80 μmol of Pt(0) divinyltetramethyldisiloxane solution catalyst with a micro-injector, then start to raise the temperature slowly, and continue to pass through acetylene, the speed is controlled at 200ml / min. When the temperature in the reaction system reaches 80°C, a total of 500 g of the triethoxyhydrogensilane raw material is added dropwise; the dropping rate is controlled at a constant rate, and the dropping time is 3 hours. After the dropwise addition, the reaction was continued for 10 minutes, and then the reaction solution was taken for detection and analysis. When it is detected that the content of trimethoxyhydrogensilane in the ...

Embodiment 3

[0029]Add 500 g of 1,2-bistrimethoxysilylethane solvent to a four-necked reaction flask equipped with magnetic stirring, a constant pressure dropping funnel, an acetylene vent tube, a thermometer, and a low-temperature condenser, and then start to slowly pass through it to dry 1. Purified acetylene, after replacing the air in the system, add 70 μmol of Pt(0) divinyltetramethyldisiloxane solution catalyst with a micro-injector, then start to slowly heat up, and continue to pass through acetylene, the speed is controlled at 300ml / min. When the temperature in the reaction system reached 90°C, a total of 400 g of tris(2-methoxyethoxy)hydrosilane raw material was added dropwise; the rate of addition was controlled at a constant rate, and the addition time was 3 hours. After the dropwise addition, the reaction was continued for 10 minutes, and then the reaction solution was taken for detection and analysis. When it is detected that the content of trimethoxyhydrogensilane in the rea...

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PUM

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Abstract

The invention relates to a vinyl trialkoxy silane coupling agent preparation method and belongs to the field of organic chemistry. According to the invention, with the Pt(0) divinyl tetramethyl disiloxane solution as the catalyst and the secondary affixture 1,2-trialkoxy silica-based ethane as the reaction solvent, acetylene and trialkoxy hydrogenous silane have hydrosilylation to generate a vinyl trialkoxy silane product. According to the invention, the vinyl trialkoxy silane product is high and stable in quality, high in yield, fewer in impurities, low in chlorine ion content, simple in technology, low in production cost, safe and environment-friendly, and facilitates industrial production.

Description

technical field [0001] The invention relates to a preparation method of a vinyltrialkoxysilane coupling agent, which belongs to the field of organic chemistry. 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. . Vinyltrialkoxysilane, as an important vinyl silane coupling agent, is widely used in filler surface treatment, high-voltage cables and other fields. It can improve the electrical and mechanical properties of the cable insulation layer and shorten the mixing time. , rapid extrusion, and improved abrasive wear and other advantages. Due to the good comprehensive cost and process performance, this product has been adopted by the industry standard specification of American ethylene propylene copolymer, EPDM rubber, XLPE wire and cable. [0003] At present, there are generall...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 王欣刘宇甘俊陈圣云甘书官
Owner JINGZHOU JIANGHAN FINE CHEM