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Preparation method of methyl phenyl vinyl silicone oil

A technology of methylphenylethylene and phenyldialkoxysilane, which is applied in the field of organic polymer materials, can solve problems such as non-uniform alternate polymerization, affecting light transmittance, cumbersome synthesis process, etc., and achieves uniform distribution of organic groups , Improving mechanical properties, easy refractive index effect

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

The traditional preparation of methylphenyl vinyl silicone oil is mainly obtained by copolymerization of octaphenylcyclotetrasiloxane and octamethylcyclotetrasiloxane, but this method has many shortcomings
First of all, octaphenylcyclotetrasiloxane is a white powdery solid that has poor miscibility with octamethylcyclotetrasiloxane. When the two are copolymerized, they cannot be uniformly and alternately polymerized, so different molecular chains The refractive index of the chain segment is different, so that the uniform and transparent phenyl silicone oil cannot be obtained
Second, octaphenylcyclotetrasiloxane is not easy to obtain, and generally needs to be formed by hydrolysis and condensation of diphenyldialkoxysilane, which not only increases the cost but also makes the whole synthesis process more cumbersome
[0004] In addition, the preparation methods of some reported phenyl silicone oils also have certain defects.
As reported in CN200410018067.4, use tetramethylammonium hydroxide or its silicon alkoxide to catalyze the synthesis of phenyl silicone oil, because tetramethylammonium hydroxide or its silicon alkoxide cannot withstand high temperature, it can only be used at low temperature, but at low temperature The rearrangement reaction of siloxane units containing phenyl chain members is not sufficient. Therefore, the storage stability of the synthesized phenyl silicone oil is unreliable and easy to mix. The higher the phenyl content, the more obvious the phenomenon
In addition, the color of phenyl silicone oil synthesized by this method is yellowish, and if it is used in the packaging of optical and electronic components, it will affect the light transmittance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] In a 1L four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 244.0 g of diphenyldimethoxysilane, 180.0 g of dimethyldimethoxysilane, 6.55 g of dimethyl A mixture of vinylethoxysilane, 1.3g of concentrated sulfuric acid and 200.0g of toluene was stirred at 45°C for 1h, then at 35-50°C, 136.4g of deionized water was added dropwise within 2h, and the temperature was raised to Reflux at 70°C for 4 hours to carry out hydrolysis and condensation reaction to obtain a hydrolysis mixture;

[0041] Stand to cool the hydrolysis mixture to room temperature, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.5 g of potassium hydroxide to the organic layer and raise the temperature to 130 ° C for 4 hours to obtain azeotropic reflux liquid;

[0042] Then the azeotropic reflux liquid is cooled to room temperature, and 60.0g of cationic resin is added to stir and neutral...

Embodiment 2

[0046] In a 1L four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 218.0 g of diphenyldiethoxysilane, 89.0 g of octamethylcyclotetrasiloxane, 13.1 g of dimethyl The mixture of vinylethoxysilane, 5.8g concentrated hydrochloric acid and 200.0g xylene was stirred at 45°C for 0.5h, then at 35-50°C, 45.9g deionized water was added dropwise within 2h, after the dropwise addition was completed Heat up to 72°C and reflux for 5 hours to obtain a hydrolysis mixture;

[0047] Stand to cool the mixture to room temperature, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.5 g of sodium hydroxide to the organic layer and raise the temperature to 140 ° C for 5 hours to obtain the azeotropic reflux liquid ;

[0048] Then the azeotropic reflux liquid was cooled to room temperature, and 40.0 g of cationic resin was added to stir and neutralize, and the Na in the mixture was s...

Embodiment 3

[0052] In a 1L four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 73.2g of diphenyldimethoxysilane, 81.7g of diphenyldiethoxysilane, 48.0g of dimethyl A mixture of dimethoxysilane, 59.2g dimethyldiethoxysilane, 3.93g dimethylvinylethoxysilane, 0.5g trifluoromethanesulfonic acid and 200.0g toluene, stirred at 30°C 4h, then drop 76.4g of deionized water within 1h at 35~50°C, after the dropwise addition, raise the temperature to 80°C and reflux for 2h to obtain a hydrolysis mixture;

[0053] Stand to cool the hydrolysis mixture to room temperature, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.5g sodium hydroxide to the organic layer, raise the temperature to 150°C and azeotropically reflux for 6h to obtain an azeotropic Reflux liquid;

[0054] Then the azeotropic reflux liquid was cooled to room temperature, and 40.0 g of acid clay was added to stir and ne...

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PUM

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Abstract

The invention discloses a preparation method of methyl phenyl vinyl silicone oil. The preparation method comprises the following steps: firstly, mixing and agitating phenyl dialkoxy silane, alkyl dialkoxy silane or methyl cyclosiloxane, an end-capping agent, an organic solvent and strong acid, then dropwise adding deionized water, increasing temperature and reflowing to conduct hydrolytic condensation reaction to obtain hydrated mixed solution; 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, increasing the temperature for azeotropic reflowing to obtain azeotropic reflowing solution; finally adding solid acidic neutralizer for neutralizing under a stirring conditionand conducting vacuum purification to obtain the methyl phenyl vinyl silicone resin. The preparation method is wide in raw material sources and low in cost, hydrolysate does not produce waste gas and does not corrode equipment; the reaction is mild and easy to control; and organic groups in synthetic products are more evenly distributed, and products with high refractive index and good light transmittance can be easily obtained.

Description

【Technical field】 [0001] The invention relates to a method for preparing organic silicon, in particular to a method for preparing methylphenylvinyl silicone oil, and belongs to the field of organic polymer materials. 【Background technique】 [0002] Silicone oil usually refers to linear polysiloxane that remains liquid at room temperature. It is a type of silicone product with many varieties and a wide range of applications. The organic groups of the most commonly used silicone oil are all methyl groups, called methyl silicone oil. Methylphenylvinyl silicone oil is a product in which some methyl groups in methyl silicone oil are replaced by phenyl and vinyl groups. It has excellent high and low temperature resistance, lubricity, radiation resistance and compatibility, and is a product with broad development prospects. product. [0003] Methylphenylvinyl silicone oil is a basic raw material for silicone packaging materials for optical and electronic components. Its quality a...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/06
Inventor 贡玉圭谢荣斌马汉喜
Owner 中山市卫宝婴儿用品有限公司