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Preparation method of vinyl tri(dimethyl siloxane) silane

The technology of vinyltrimethoxysilane and dimethylsiloxane is applied in the field of preparation of vinyltrisilane, which can solve the problems of reducing product yield, hydrolysis of raw materials, slow reaction and the like, and achieves easy temperature control and reaction. The effect of mild temperature and short process

Active Publication Date: 2018-05-25
SHANDONG GUIKE NEW MATERIAL CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] (1) The reaction raw material is chlorosilane, which requires high quality reaction equipment, and produces a large amount of by-product hydrochloric acid in the reaction;
[0007] (2) The low temperature (around 0°C) needs to be strictly controlled during the reaction process. If the temperature is too high, the raw materials will be severely hydrolyzed and the product yield will be reduced;
[0008] (3) Exothermic heat is serious in the reaction process, and the strict requirement to temperature makes reaction carry out slowly;
[0009] (4) After the reaction is completed, the synthetic solution is strongly acidic, and needs to be washed with a large amount of water and alkali to neutrality, then dried, filtered, and distilled to obtain the finished product. The process is complicated

Method used

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  • Preparation method of vinyl tri(dimethyl siloxane) silane
  • Preparation method of vinyl tri(dimethyl siloxane) silane
  • Preparation method of vinyl tri(dimethyl siloxane) silane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Add 5g of concentrated sulfuric acid, 64g of methanol, and 81g of water into a 1000mL three-necked flask equipped with a magnetic stirrer, a thermometer, a condenser tube, and an oil bath heating device to obtain a mixed solution A, and add 268.7g of tetramethyl Disiloxane, stirred and heated up to 40°C to react to obtain mixed solution B;

[0033] (2) Add 74g of vinyltrimethoxysilane dropwise to the mixed solution B to continue the reaction for 2h, the reaction is completed to obtain the mixed solution C, and the gas chromatography detects the reaction situation, wherein the product content is 60%;

[0034] (3) The mixed solution C is separated, washed twice with 500g of water, and the supernatant is filtered after drying with anhydrous magnesium sulfate for 3h, and the filtrate is transferred to the distillation equipment, and the solvent methanol is separated by atmospheric distillation first, and the Pressure distillation separated the front fraction and the pro...

Embodiment 2

[0036] (1) Add 0.33g of hydrochloric acid, 16g of methanol, and 36g of water into a 1000mL three-neck flask equipped with a magnetic stirrer, a thermometer, a condenser tube, and an oil bath heating device to obtain a mixed solution A, and add 201.5g of tetramethyl Disiloxane, stirred and heated to 20°C to react to obtain mixed solution B;

[0037] (2) Add 74g of vinyltrimethoxysilane dropwise to the mixed solution B to continue the reaction for 6h. After the reaction is completed, the mixed solution C is obtained. The reaction situation is detected by gas chromatography, and the product content is 48%;

[0038] (3) The mixed solution C is separated, washed twice with 500g of water, and the supernatant is filtered after drying with anhydrous magnesium sulfate for 3h, and the filtrate is transferred to the distillation equipment, and the solvent methanol is separated by atmospheric distillation first, and the Pressure distillation separated the front fraction and the product, a...

Embodiment 3

[0040] (1) Add 7.4g sodium methoxide, 160g methanol, and 108g water into a 1000mL three-neck flask equipped with magnetic stirring, thermometer, condenser and oil bath heating device to mix to obtain mixed solution A, and add 403g tetramethyl Disiloxane, stirred and heated up to 50°C for reaction to obtain mixed solution B;

[0041] (2) Add 74g of vinyltrimethoxysilane dropwise to the mixed solution B to continue the reaction for 3h. After the reaction is completed, the mixed solution C is obtained. The reaction situation is detected by gas chromatography, and the product content is 37%;

[0042] (3) The mixed solution C is separated, washed twice with 500g of water, and the supernatant is filtered after drying with anhydrous magnesium sulfate for 3h, and the filtrate is transferred to the distillation equipment, and the solvent methanol is separated by atmospheric distillation first, and the Pressure distillation is separated front cut and product, and remaining high-boiling ...

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Abstract

The invention relates to a preparation method of vinyl tri(dimethyl siloxane) silane, which includes steps of firstly, mixing catalyst, methanol and water to obtain mixed fluid A; feeding tetramethyldisiloxane in mixed fluid A, stirring and heating to 20-100 DEG C to react and obtain mixed fluid B; dropwise adding vinyl trimethoxy silane in mixed fluid B to continue reaction; completing reactionto obtain mixed fluid C; separating the mixed fluid C and cleaning by water; taking supernatant liquid, drying, filtering and distilling the supernatant liquid to obtain a finished product. The raw material applied to the method contains siloxane, and has low equipment quality requirement; moreover, the reaction is free from side product hydrochloric acid, and does not need massive water washing and alkali washing; the technique is simple and flow is short; meanwhile, the preparation method does not need to strictly control low temperature, the reaction temperature is gentle, and easy to control; the prepared product yield is up to 84.8%; after distilling and purification, the product purity is up to 98%, and the purity is high.

Description

technical field [0001] The invention belongs to the technical field of new silane materials, and in particular relates to a preparation method of vinyl tris(dimethylsiloxane) silane. Background technique [0002] Vinyltris(dimethylsiloxy)silane, having the following structural formula: [0003] [0004] Vinyl tris(dimethylsiloxane)silane is mainly used in silane cross-linked polyethylene cables and pipes, and can also be used in low-smoke halogen-free cables to improve the oxygen index of cables. As a water-repellent agent, it can be used to disperse organic coatings and improve the water resistance of coatings. This substance contains silicon-hydrogen bonds and has the properties of further processing. According to different requirements, functional groups can be introduced in a directional way, and it can be used as functional silicone oil or coupling agent. It is a high-quality intermediate. [0005] In the prior art, the most traditional method for preparing vinyl t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
CPCC07F7/0874
Inventor 孔凡振杨甜甜李杭杭齐萧孔禄刘秋元
Owner SHANDONG GUIKE NEW MATERIAL CO LTD
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