Preparation method for vinyl tris(trimethylsiloxane)silane

A technology of ethoxytrimethylsilane and vinyltriethoxysilane, which is applied in the field of preparation of vinyltrisilane, can solve the problems of too fast product hydrolysis, severe reaction heat release, complex process flow, etc. Simple, easy to remove, and the effect of improving the preparation process

Pending Publication Date: 2019-05-03
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing synthetic methods have the following problems: one is that the reaction is difficult to control; due to the high activity of the raw materials, the exothermic reaction is serious, resulting in too fast hydrolysis of the product and low yield; the other is that the reaction raw materials use chlorosilane, which produces A large amount of hydrochloric acid will cause corrosion to the equipment, and it will take a lot of water to wash and deacidify, which has poor environmental performance and low safety; third, the process is complicated, the condensation efficiency is low, and the product yield is low

Method used

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  • Preparation method for vinyl tris(trimethylsiloxane)silane
  • Preparation method for vinyl tris(trimethylsiloxane)silane
  • Preparation method for vinyl tris(trimethylsiloxane)silane

Examples

Experimental program
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Effect test

Embodiment 1

[0038] The reaction flask containing 30 g of vinyltriethoxysilane was placed in a constant temperature magnetic stirring device. Stir and heat to 60°C, slowly add 11.2ml, 0.001mol / L hydrochloric acid solution and 67.12g ethoxytrimethylsilane dropwise with a constant pressure dropping funnel, after the dropwise addition is completed, react at a constant temperature, condense and reflux for 2.5h, and the reaction ends , to obtain the crude product. Vacuum rotary evaporation at 70°C to remove ungrafted reaction raw materials, ethanol, water and other low-boiling impurities. Extract with an appropriate amount of toluene, wash twice with sodium carbonate, wash repeatedly with deionization, separate the funnel for stratification, take the toluene layer until the pH value is neutral, dry with anhydrous sodium sulfate for 1 hour, and finally use The organic layer was distilled under reduced pressure, and the fraction with a temperature of 130-140° C. and a vacuum of -0.09 MPa was tak...

Embodiment 2

[0047] Place a reaction bottle containing 50ml of solvent toluene and 12g of vinyltriethoxysilane in a constant temperature magnetic stirring device, stir and heat to 55°C, and mix well. Slowly add 10.43ml of 0.01mol / L hydrochloric acid aqueous solution and 34.44g of ethoxytrimethylsilane dropwise with a constant pressure dropping funnel. After the dropwise addition, react at constant temperature, condense and reflux for 3 hours, and the crude product is obtained after the reaction is completed. Rotary steaming at 70°C to remove ungrafted reaction raw materials, ethanol, water, solvent toluene and other low-boiling impurities. Extract with toluene, wash with appropriate amount of sodium carbonate twice, deionize and wash repeatedly, separate the funnel for stratification, take the toluene layer, repeat until the pH value is neutral, dry with anhydrous sodium sulfate for 1 hour, and finally use reducing Distill the organic layer under pressure, and take the fraction whose tempe...

Embodiment 3

[0050] Place the reaction flask containing 12 g of vinyltriethoxysilane in a constant temperature magnetic stirring device, stir and heat to 30° C., and mix well. Prepare 0.01mol / L dilute hydrochloric acid solution. Slowly add 10.43ml of hydrochloric acid aqueous solution and 34.44g of ethoxytrimethylsilane dropwise with a constant pressure dropping funnel. After the dropwise addition, react at constant temperature, condense and reflux for 1 hour, and the crude product is obtained after the reaction is completed. Rotary steaming at 70°C to remove ungrafted reaction raw materials, ethanol, water, and other low-boiling impurities. Extract with toluene, wash with appropriate amount of sodium carbonate twice, deionize and wash repeatedly, separate the funnel for stratification, take the toluene layer, repeat until the pH value is neutral, dry with anhydrous sodium sulfate for 1 hour, and finally use reducing The organic layer was distilled under pressure, and the fraction tempera...

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Abstract

The invention discloses a preparation method for vinyl tris(trimethylsiloxane)silane. The preparation method comprises the following steps: with hydrochloric acid as a catalyst, weighing a certain amount of ethoxytrimethylsilane, slowly dropwise adding the ethoxytrimethylsilane into vinyltriethoxysilane at a certain temperature at the same time, carrying out stirring at a constant temperature, carrying out a reaction so as to obtain a colorless transparent liquid, and carrying out separation and purification so as to obtain the vinyl tris(trimethylsiloxane)silane. The preparation method provided by the invention has simple preparation process, can reach a yield of 76% or more, avoids the use of chlorosilane, and is safe and environmentally-friendly. The vinyl tris(trimethylsiloxane)silaneprepared by using the preparation method provided by the invention can be used as a functional modified silicone oil intermediate or a coupling agent, and can be applied to the fields of coatings, moisture-proofing agents, cables, cosmetics, etc.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a preparation method of vinyl tris(trimethylsiloxane) silane. Background technique [0002] With the vigorous development of the silicone industry, the research and development of high-performance, multifunctional siloxane products has become the focus. In particular, the modification of silane coupling agents and silicone oils used in the fields of coatings, textiles, and daily chemicals has attracted widespread attention. In this context, vinyltris(trimethylsiloxane)silane, as an intermediate containing active groups, has attracted extensive attention in recent years because of its highly branched silicon chain structure. [0003] At present, there are three synthetic routes of vinyl tri(trimethylsiloxane) silane: the reaction of trimethylchlorosilane and vinyltriethoxysilane under the catalyst to generate the target product; trimethylchlorosilane and viny...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
Inventor 杨成何彤
Owner JIANGNAN UNIV
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