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Method for preparing vinyl tri(2,2,2-trifluoroethoxy) silane

A technology of vinyltrichlorosilane and trifluoroethoxy, which is applied in the field of preparation of vinyltrisilane, can solve the problems of increasing the difficulty of product separation, low single-pot output, and low economic benefits, and achieves easy industrial production and equipment The effect of less investment and high utilization rate of equipment

Active Publication Date: 2020-01-14
ZHEJIANG KAIHUA SYNTHETIC MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the vinyl tri(2,2,2-trifluoroethoxy) silane synthesis method disclosed in this patent, not only the synthesis yield is low, but also a large amount of dichloromethane is used as the reaction solvent, resulting in low single-pot output, At the same time, it increases the separation difficulty of the product, and the economic benefit is low

Method used

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  • Method for preparing vinyl tri(2,2,2-trifluoroethoxy) silane
  • Method for preparing vinyl tri(2,2,2-trifluoroethoxy) silane

Examples

Experimental program
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Embodiment 1

[0029] (1) Add 48.6g (0.3mol) of vinyl trichloride into a 250mL three-necked flask equipped with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube bubbling device, and an HCl tail gas absorption device. Chlorosilane, a cooling medium at -30°C was introduced into the reflux condenser, the temperature of the material in the three-necked flask was raised to 50°C, and 105g (1.05mol) of trifluoroethanol was added dropwise to the three-necked flask at a constant speed through a constant pressure dropping funnel, It took 60 minutes and the dropping rate was 1.75g / min. After the dropwise addition of trifluoroethanol is completed, the materials in the three-necked flask are maintained at 50°C for 60 minutes; Put it into a three-necked flask to take away the generated HCl gas, and discharge it after being neutralized by the tail gas absorption device. After the material is kept in the reflux state and the blowing and purging stat...

Embodiment 2

[0032](1) Add 48.6g (0.3mol) of vinyl trichloride into a 250mL three-necked flask equipped with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube bubbling device, and an HCI tail gas absorption device. Chlorosilane, a cooling medium at -20°C was introduced into the reflux condenser, and after the material in the three-necked flask was lowered to -20°C, 90g (0.90mol) of trifluoroethanol was dropped into the three-necked flask at a constant speed through a constant pressure dropping funnel In the process, it took 180min and the dropping rate was 0.5g / min. After the dropwise addition of trifluoroethanol is completed, the materials in the three-necked flask are maintained at -20°C for 90 minutes; Put it into a three-necked flask to take away the generated HCl gas, and discharge it after being neutralized by the tail gas absorption device. After the material is kept in the reflux state and blowing and purging state for 4 hou...

Embodiment 3

[0035] (1) Add 48.6g (0.3mol) of vinyl trichloride into a 250mL three-necked flask equipped with a thermometer, a mechanical stirrer, a constant pressure dropping funnel, a reflux condenser, a bottom tube bubbling device, and an HCl tail gas absorption device. Chlorosilane, a cooling medium at -10°C was introduced into the reflux condenser, and after the material in the three-neck flask was raised to 60°C, 97.5g (0.975mol) of trifluoroethanol was added dropwise at a constant speed to the three-necked flask through a constant pressure dropping funnel In the flask, it took 60min and the rate of addition was 1.63g / min. After the dropwise addition of trifluoroethanol is completed, the temperature of the material in the three-necked flask is raised to reflux, and at the same time, dry nitrogen gas is sent into the three-necked flask through the bottom tube bubbling device to take away the generated HCl gas, which is absorbed by the tail gas After the device was neutralized and disc...

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Abstract

The invention relates to the field of organic chemicals, aims to solve the problems that a solvent is used and the reaction yield is low in the synthesis process of vinyl tri(2,2,2-trifluoroethoxy) silane, and discloses a method for preparing the vinyl tri(2,2,2-trifluoroethoxy) silane. The method comprises the following steps: adding dropwise trifluoroethanol into vinyl trichlorosilane which is maintained to a certain temperature in advance, keeping the temperature to implement a reaction, increasing the temperature till refluxing, and maintaining the refluxing process; cooling the reaction material to the room temperature so as to obtain a crude synthesis produce, neutralizing the system by using an alkali neutralizer, performing filtering, and collecting filtrate; and transferring the collected filtrate into a rectification tower, and performing treatment, so as to obtain the vinyl tri(2,2,2-trifluoroethoxy) silane. The method is simple in operation condition, simple in step, free of extra solvent except raw materials for reactions, high in target product yield, easy in separation and purification, and very applicable to large-scale production.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of vinyl tris(2,2,2-trifluoroethoxy)silane. Background technique [0002] Fluorosilicone-containing polymer is a new type of advanced polymer synthetic material. It has repeated -Si-O-Si chain links as the main chain, and the fluoroalkyl group is connected to the Si atom and is located in the side chain of polysiloxane. , Fluorine-containing polysiloxane combines the advantages of silicone materials such as excellent high and low temperature resistance, UV resistance, and oxidative degradation resistance with the unique chemical stability, weather resistance, corrosion resistance, and oxidation resistance of fluorine-containing materials. Vinyl tris(2,2,2-trifluoroethoxy)silane molecule contains not only easy-to-polymerize C=C double bond, but also hydrolyzable 2,2,2-trifluoroethoxy functional group. An important raw material of fluororubber, it can also be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/188Y02E60/10
Inventor 陈道伟伍川郑云峰蒋攀黄亮兵董红侯建超瞿志荣栾文耕邱化玉蒋剑雄
Owner ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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