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A kind of transesterification method for preparing vinyl tri-(2-methoxyethoxy)-silane

A technology of trimethoxysilane and methoxyethoxy, which is applied in the field of transesterification for the preparation of vinyl tri-silane, can solve the problems of high equipment investment, high safety cost of acetylene, and increased cost.

Active Publication Date: 2019-03-15
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The disadvantage of this method is that the safety cost of the raw material acetylene is high. Acetylene is a flammable and explosive gas. Acetylene as a production raw material not only requires high equipment investment, but also requires cumbersome approval procedures
Another disadvantage of this method is the use of expensive chloroplatinic acid as a catalyst, which further increases the cost. In addition, this method cannot avoid the excessive addition of acetylene and hydrosilane to generate ethyldialkoxysilane, resulting in the main product lower yield

Method used

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  • A kind of transesterification method for preparing vinyl tri-(2-methoxyethoxy)-silane
  • A kind of transesterification method for preparing vinyl tri-(2-methoxyethoxy)-silane
  • A kind of transesterification method for preparing vinyl tri-(2-methoxyethoxy)-silane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 148 g of vinyltrimethoxysilane, 228 g of ethylene glycol monomethyl ether, and 1 g of anhydrous aluminum potassium sulfate into a 1000 ml four-neck flask equipped with a magnetic stirrer, a thermometer, and a spherical condenser. Raise the temperature to 70-80°C and react for 2h. Then the temperature was raised and the methanol was distilled off. When the temperature of the kettle rose to 100° C., the recovery of the methanol was completed, and a total of 94 g of methanol was obtained. Then lower the temperature, when cooled to below 50°C, filter, reclaim to obtain anhydrous potassium aluminum sulfate 0.96g, obtain colorless and transparent vinyl tri-(2-methoxyethoxy)-silane product 278g, yield is 99.5%. Its content is detected by gas chromatography to be 99.5%.

Embodiment 2

[0034] Add 148 g of vinyltrimethoxysilane, 228 g of ethylene glycol monomethyl ether, and 1 g of anhydrous potassium ferric sulfate into a 1000 ml four-neck flask equipped with a magnetic stirrer, a thermometer, and a spherical condenser. Raise the temperature to 70-80°C and react for 4h. Then the temperature was raised and the methanol was distilled off. When the temperature of the kettle rose to 100° C., the recovery of the methanol was completed, and the amount of methanol obtained was 90 g. Then the temperature was lowered, and after cooling to below 50°C, it was filtered to recover 0.96 g of double salt transesterification catalyst and 277 g of vinyl tris-(2-methoxyethoxy)-silane product with a yield of 99.0%. Its content is detected by gas chromatography to be 99.3%.

Embodiment 3

[0036] Add 148 g of vinyltrimethoxysilane, 228 g of ethylene glycol monomethyl ether, and 1 g of anhydrous ferrous ammonium sulfate into a 1000 ml four-neck flask equipped with a magnetic stirrer, a thermometer, and a spherical condenser. Raise the temperature to 70-80°C and react for 4h. Then the temperature was raised and the methanol was distilled off. When the temperature rose to 100° C., the recovery of methanol was completed, and the amount of methanol obtained was 90 g. Then the temperature was lowered, and after cooling to below 50° C., it was filtered to recover 0.96 g of double salt transesterification catalyst and 276 g of vinyl tris-(2-methoxyethoxy)-silane product, with a yield of 98.5%. Its content is detected by gas chromatography to be 99.3%.

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Abstract

The invention relates to an ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane, and belongs to the technical field of organic chemical. The ester exchange method uses ethylene glycol monomethyl ether and vinyl trimethoxy silane as raw materials, uses neutral double salt type catalyst to perform the ester exchange reaction, and generates tri-(2- methoxy ethyoxyl)-silane. Through filtering and recycling, the catalyst can be repeatedly used. Compared with traditional esterification method, the method has the advantages that 1, the ester exchange reaction process cannot cause the deepened color of product, methanol is removed by distilling after reaction, and the product can be obtained by direct filtering. 2. The catalyst can be recycled and repeatedly used for 10 times, and the activity is still kept.

Description

technical field [0001] The invention relates to a transesterification method for preparing vinyl tris-(2-methoxyethoxy)-silane, which belongs to the technical field of organic chemistry. Background technique [0002] The structural formula of vinyl tri-(2-methoxyethoxy)-silane is as follows: [0003] [0004] Vinylalkoxysilane is usually prepared by esterifying vinyltrichlorosilane with alcohols, followed by neutralization, filtration, and rectification (for example, Chinese patent CN1320600A). The reaction equation is as follows: [0005] Main response: [0006] [0007] side effects: [0008] [0009] The raw material vinyltrichlorosilane used in this method and the by-product hydrogen chloride gas are highly corrosive to the equipment, and the by-product hydrogen chloride is not easy to handle, so it is generally necessary to use an alkaline neutralizer to absorb it, or to increase equipment investment, Use equipment such as falling film absorption towers to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
CPCY02P20/584
Inventor 靳军张宇陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM