Preparation method of methyl phenyl vinyl silicone resin

A technology of methylphenylethylene and tetraethoxysilane, applied in the field of organic polymer materials, can solve the problems of difficult control of polymerization degree, cumbersome synthesis process, complex reaction, etc., and achieve good reaction repeatability and controllability, Improved operating environment and stable storage performance

Active Publication Date: 2013-04-03
中山市卫宝婴儿用品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But above-mentioned preparation method has following deficiency: (1) because Ph 2 SiCl 2 with Me 2 SiCi 2 and MeViSiCl 2 The large difference in hydrolysis activity makes the composition of the product complex. There are organic block polymers containing both diphenylsiloxane chains and dimethylsiloxane chains, and there are only dimethylsiloxane chains or The polymer composed of diphenylsiloxane chains has a large difference in the refractive index of each component, which ultimately leads to a low light transmittance of the product.
(2) The reaction monomer is organochlorosilane, which is more dangerous during transportation and storage, and a large amount of hydrogen chloride gas is generated during the reaction process, and the heat released by dissolving in water promotes the spontaneous condensation reaction between silicon hydroxyl groups, As a result, the degree of polymerization is difficult to control, the reaction system is prone to gel, and the hydrochloric acid generated by the reaction will cause corrosion to the equipment
(3) The synthesis process is cumbersome, the reaction products are complex, need to be washed many times, and there are poor storage and unstable quality, etc.
(4) The cycle is long, the efficiency is low, and the degree of reaction is not easy to control
This reaction does not produce hydrogen chloride, has good reaction repeatability and controllability, and does not produce waste water. However, this method produces many raw materials, complex reactions, and poor temperature resistance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] In a four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 140.4g of deionized water, 1.1g of concentrated sulfuric acid and 200.0g of toluene and mix and stir for 30min. Under stirring conditions at 40°C, within 2h Add dropwise 237.6g of phenyltrimethoxysilane, 16.2g of hexamethyldisiloxane, 26.2g of dimethylvinylethoxysilane, 41.6g of tetraethoxysilane, 24.0g of dimethyldimethoxy A mixture of silane and 22.4g of diphenyldimethoxysilane was subjected to hydrolysis reaction, and after the dropwise addition was completed, the temperature was raised to 72°C for reflux reaction for 4 hours to obtain a mixed solution;

[0034] Cool and let the mixed solution stand, separate the organic layer and wash the separated organic layer with deionized water to neutrality, then add 0.4g potassium hydroxide to the organic layer, raise the temperature to 140°C and azeotropically reflux for 4h to obtain an azeotropic Refl...

Embodiment 2

[0038] In a four-neck flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 126.9 g of deionized water, 6.5 g of concentrated hydrochloric acid and 200.0 g of xylene and mix and stir for 1 h. Under the condition of stirring at 35°C, 240.4g phenyltriethoxysilane, 24.3g hexamethyldisiloxane, 13.1g dimethylvinylethoxysilane, 41.6g tetraethoxysilane were added dropwise within 1h , a mixture of 29.7g dimethyldiethoxysilane and 48.8g diphenyldimethoxysilane was subjected to hydrolysis reaction, and after the dropwise addition was completed, the temperature was raised to 70°C for reflux reaction for 5 hours to obtain a mixed solution;

[0039] Cool and let the mixed solution stand, separate the organic layer and wash the organic layer with deionized water until neutral. Add 0.4 g of sodium hydroxide to the organic layer, raise the temperature to 140° C. and azeotropically reflux for 6 hours to obtain an azeotropic reflux liquid; ...

Embodiment 3

[0043] In a four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 156.6g of deionized water, 1.4g of nitric acid and 200.0g of isopropanol and mix and stir for 2h. Under stirring conditions at 45°C, 2h 158.8g of phenyltrimethoxysilane, 54.4g of methyltrimethoxysilane, 91.0g of methylphenyldimethoxysilane, 26.0g of methylvinyldimethoxysilane, 32.4g of hexamethyldimethoxysilane were added dropwise The mixture of siloxane, 20.8g tetraethoxysilane and 36.0g dimethyldimethoxysilane was subjected to hydrolysis reaction, and after the dropwise addition was completed, the temperature was raised to 75° C. for reflux reaction for 6 hours to obtain a mixed solution.

[0044] Cool and let the mixed solution stand, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.4 g of cesium hydroxide to the organic layer, heat up to 130 ° C and azeotropically reflux for 5 hours to obtain ...

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Abstract

The invention discloses a preparation method of methyl phenyl vinyl silicone resin. The preparation method comprises the following steps: firstly mixing and agitating organic solvent, deionized water and strong acid, then dropwise adding a mixture for hydrolysis reaction, and increasing temperature and reflowing to obtain mixed solution, wherein the mixture consists of difunctional alkoxy silane, trifunctional alkoxy silane, monofunctional alkoxy silane and tetraethoxysilane; standing the mixed solution, cooling to room temperature, separating out an organic layer, washing the organic layer with deionized water till the organic layer becomes neutral, then adding an alkaline catalyst into the organic layer, increasing the temperature for azeotropic reflowing for a certain time to obtain azeotropic reflowing solution; cooling the azeotropic reflowing solution to 50 DEG C below, then adding solid acidic neutralizer, stirring for neutralizing, filtering, and conducting vacuum purification to obtain the methyl phenyl vinyl silicone resin. According to the preparation method, the process is easy to control, the labor intensity is low, the whole process has small toxicity, and the preparation method has the advantages that monomer sources are wide, cost is low, and the prepared methyl phenyl vinyl silicone resin has stable storage performance.

Description

【Technical field】 [0001] The invention relates to a method for preparing an organic silicon resin, in particular to a method for preparing a methylphenyl vinyl silicone resin, and belongs to the technical field of organic polymer materials. 【Background technique】 [0002] Silicone resin has the characteristics of both organic resins and inorganic materials, such as excellent heat resistance, weather resistance, electrical insulation, water repellency and resistance to chemical agents, etc. It is an electrical insulation material with good development prospects. This is because the main chain of silicone has -Si(Me) 2 -O- is formed by chemical bonds, and its side groups are connected by silicon and organic groups. The polymer chain contains both "inorganic structure" and "organic structure". This special composition and unique molecular structure make it integrate the functions of inorganic substances and the characteristics of organic substances, thus reflecting the charact...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/06
Inventor 谢荣斌贡玉圭马汉喜
Owner 中山市卫宝婴儿用品有限公司
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