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Preparation method for phenyl vinyl methyl MQ silicone resin which has high refractive index and is used for LED package

A kind of phenylvinylmethyl, LED encapsulation technology

Active Publication Date: 2018-02-09
山东盛宇新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since epoxy resin contains a large number of aromatic rings, it will be oxidized to carbonyl and become a chromophore after absorbing ultraviolet rays, making the resin yellow.
In addition, epoxy resin will also change color when heated, which reduces the light transmittance in the near ultraviolet region and affects the luminous efficiency of LED light sources.
Moreover, epoxy resin itself absorbs moisture, is easy to age, has poor heat resistance, and has a large curing internal stress, which will affect the service life of the material, thereby affecting the life of the LED light source.

Method used

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  • Preparation method for phenyl vinyl methyl MQ silicone resin which has high refractive index and is used for LED package
  • Preparation method for phenyl vinyl methyl MQ silicone resin which has high refractive index and is used for LED package

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Add 170 g of ethyl silicate, 111 g of hexamethyldisiloxane, 12 g of vinyl double caps, and 10 g of phenyl double caps in the three-necked flask, and mix well. At a reaction temperature of 10°C, 4 g of concentrated sulfuric acid and 30 g of water were slowly added dropwise. After 1 h of reaction, the temperature was raised to reflux for 4 h, and 40 wt % KOH solution was added dropwise to adjust the system to be neutral. Then distilled with toluene and filtered to obtain a clear and transparent silicone resin toluene solution. The toluene solvent was distilled off to obtain 270 g of a clear and transparent silicone resin with a phenyl vinyl network structure, with a yield of 89% and a vinyl content of 5%.

Embodiment 2

[0020] Add 170 g of ethyl silicate, 111 g of hexamethyldisiloxane, 15 g of vinyl double caps, and 10 g of phenyl double caps in the three-necked flask, and mix well. At a reaction temperature of 8° C., 4 g of concentrated sulfuric acid and 30 g of water were slowly added dropwise, and after 1 h of reaction, the temperature was raised to reflux for 5 h, and 50 wt % KOH solution was added dropwise to adjust the system to be neutral. Then distilled with toluene and filtered to obtain a clear and transparent silicone resin toluene solution. The toluene solvent was distilled off to obtain 280 g of a clear and transparent silicone resin with a phenyl vinyl network structure, with a yield of 91% and a vinyl content of 5.5%.

Embodiment 3

[0022] Add 170 g of ethyl silicate, 111 g of hexamethyldisiloxane, 10 g of vinyl double caps, and 10 g of phenyl double caps in the three-necked flask, and mix well. At a reaction temperature of 8°C, 4 g of concentrated sulfuric acid and 30 g of water were slowly added dropwise, and after 1 h of reaction, the temperature was raised to reflux for 6 h, and 60 wt % KOH solution was added dropwise to adjust the system to be neutral. Then distilled with toluene and filtered to obtain a clear and transparent silicone resin toluene solution. The toluene solvent was distilled off to obtain 265 g of a clear and transparent silicone resin with a phenyl vinyl network structure, with a yield of 88% and a vinyl content of 3%.

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Abstract

The present invention relates to a preparation method for phenyl vinyl methyl MQ silicone resin which has a high refractive index and is used for LED package. The method comprises the following steps:ethyl silicate is hydrolyzed under the actions of sulfuric acid or a solid acid catalyst to obtain silicic acid, condensation is further performed, and then a phenyl di-blocking agent and a vinyl di-blocking agent are reacted with the condensed material for blocking ends; and after the reaction is finished, reflux is performed to make the obtained material highly crosslinked, then neutralizationis performed by using an alkaline liquid, distillation is performed by using toluene, and finally a toluene solution of the phenyl vinyl methyl silicone resin is obtained. According to the invention,the reaction activity of the synthetic process is relatively low and easy to control, the reaction speed is quick and the reaction is performed fully, the effective yield of the product is improved, and the colorless and transparent silicone resin which has the high refractive index and stable quality and meets different requirements can be obtained according to selected different functional groups.

Description

technical field [0001] The invention relates to the technical field of organosilicon polymer compounds, in particular to a preparation method of phenylvinylmethyl MQ silicone resin for high-fold LED packaging. Background technique [0002] At present, most of the packaging materials used in high-fold LEDs are epoxy resins. Epoxy resins have excellent adhesion, electrical insulation, sealing and dielectric properties, and are low in cost, flexible in formula, easy to form, High production efficiency has become the mainstream material for low-power LED packaging. However, because epoxy resin contains a large number of aromatic rings, it will be oxidized into carbonyl and become a chromophore after absorbing ultraviolet rays, making the resin yellow. In addition, the epoxy resin will also change color when heated, which reduces the light transmittance in the near ultraviolet region and affects the luminous efficiency of the LED light source. Moreover, the moisture absorption ...

Claims

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Application Information

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IPC IPC(8): C08G77/20C08G77/08C08G77/06
CPCC08G77/06C08G77/08C08G77/20C08G77/70C08G77/80
Inventor 卢旭刘明强顾振涛原亚敏
Owner 山东盛宇新材料有限公司
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