Preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging

A technology of methylphenylvinylpolysiloxane and tetramethyltetravinylcyclotetrasiloxane, applied in the direction of adhesives and the like, can solve the problems of wide product molecular weight distribution, large amount of waste acid, troublesome post-processing, etc., Achieve the effect of narrow molecular weight distribution, simple post-processing and environmental protection process

Inactive Publication Date: 2014-12-17
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The technical problem to be solved by the present invention is to overcome the disadvantages of a large amount of waste acid produced by the general chlorosilane hydrolysis method, troublesome after-treatment and wide molecular weight distribution of the products of the hydrolysis method of chlorosilane or alkoxysilane

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  • Preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging
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  • Preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging

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Embodiment 1

[0042]The preparation method of the reticular methylphenylvinylpolysiloxane for LED encapsulation of preferred embodiment 1 of the present invention, its process is: under N protection, in 250ml, thermometer, reflux condensing tube, mechanical agitation four ports are equipped with Add 11.0g of tetramethyltetravinylcyclotetrasiloxane, 9.3g of octamethylcyclotetrasiloxane, 11.7g of hexamethyldisiloxane, 10.3g of diphenylsiloxane, and 25.0g of toluene into the bottle , DMSO 0.347g, KOH 0.037g, react at 75°C for 4h; after the reaction, add 40.0g of phenylsilsesquioxane, 29.0g of toluene, several grams of KOH, re-protect the nitrogen, and heat to toluene reflux, react After 5 h, the reaction was cooled to room temperature, and a sufficient amount of deionized water was added to terminate the reaction. After continuing to stir for 30min, the product was poured into a 500ml separatory funnel, washed with deionized water to neutrality (washed three times), and the upper toluene solut...

Embodiment 2

[0050] The preparation method of the reticular methylphenyl vinyl polysiloxane for LED encapsulation of preferred embodiment two of the present invention, its process is: 2 Under protection, add 5.33g of tetramethyltetravinylcyclotetrasiloxane, 13.8g of octamethylcyclotetrasiloxane, 13.8g of hexamethyldi Siloxane 10.2g, diphenylsiloxane 12.3g, toluene 28g, DMSO 0.452g, KOH 0.035g, react at 75°C for 4h; after the reaction, add phenylsilsesquioxane 40.0g, toluene 28g, KOH 0.107g, nitrogen protection again, and heated to toluene reflux, reacted for several hours, cooled to room temperature after the reaction, added enough deionized water to terminate the reaction, and continued to stir for 30min. Pour the product into a 500ml separatory funnel, wash it with deionized water to neutrality (wash three times), obtain the upper toluene solution layer, add anhydrous magnesium sulfate to dry, filter to remove the magnesium sulfate solid, evaporate under reduced pressure at 4000 Pa Afte...

Embodiment 3

[0057] The preparation method of the reticular methylphenyl vinyl polysiloxane for LED encapsulation of preferred embodiment three of the present invention, its process is: 2 Under protection, add 2.7g of tetramethyltetravinylcyclotetrasiloxane, 16.1g of octamethylcyclotetrasiloxane, 16.1g of hexamethyldi Siloxane 10.2g, diphenylsiloxane 12.3g, toluene 28g, DMSO 0.452g, KOH 0.044g, react at 75°C for 4h; after the reaction, add phenylsilsesquioxane 40.0g, toluene 28g, KOH 0.117g, nitrogen protection again, and heated to toluene reflux, reacted for 10 hours, cooled to room temperature after the reaction, added enough deionized water to terminate the reaction, continued to stir for 30min. Pour the product into a 500ml separatory funnel, wash it with deionized water to neutrality (wash three times), obtain the upper toluene solution layer, add anhydrous magnesium sulfate to dry, filter to remove the magnesium sulfate solid, evaporate under reduced pressure at 4000 Pa After toluen...

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Abstract

The invention discloses a preparation method for net-like methyl phenyl vinyl polysiloxane for LED packaging, and concretely relates to a preparation method for a vinyl polysiloxane prepolymer containing methyl and phenyl groups and possessing a net-like structure. According to the preparation method, phenyl silsesquioxane, diphenylsiloxane, octamethyl cyclotetrasiloxane, tetramethyl tetravinyl cyclotetrasiloxane and an end-capping reagent are subjected to a copolymerization reaction under an alkali catalytic condition according to a certain, so that the methyl phenyl vinyl polysiloxane prepolymer which possesses a net-like structure and is a liquid at room temperature is obtained. The prepolymer and an organic silicon monomer or prepolymer containing a silicon-hydrogen structure are subjected to addition polymerization, so that organic silicon resin with excellent performances for LED packaging is prepared. The method simultaneously overcomes the disadvantages that a chlorosilane hydrolysis method generates too much waste acids and is complex in post treatment, the molecular weight distribution is wide and the like, and is the method is an environment-friendly good-repeatability technology.

Description

technical field [0001] The invention relates to a method for preparing network-like methylphenyl vinyl polysiloxane by alkali catalysis, and the prepared polysiloxane is especially suitable as a prepolymer of organic silicon resin for LED packaging. Background technique [0002] Power-type light-emitting diodes have long life, high brightness, small size, energy saving, environmental protection, and high luminous efficiency. As a new type of energy-saving light source, they have been widely used in traffic lights, street lights, automotive lighting and indoor lighting, and are expected to replace Light sources such as incandescent lamps have become the fourth generation of lighting sources. [0003] At present, the packaging material of ordinary LED is mainly epoxy resin. With the development of high-power LEDs, especially the development of white LEDs based on ultraviolet light, the packaging material is required to maintain high transmittance in the visible light region a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/20C08G77/08C08L83/07C09J183/07
Inventor 王涛张贤顺晁鹏杰
Owner BEIJING UNIV OF CHEM TECH
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