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Preparation method of phenyl hydrogen-containing methyl MQ silicone resin with high refractive index for LED packaging

A technology of LED encapsulation and MQ silicone resin is applied in the field of preparation of phenyl hydrogen-containing methyl MQ silicone resin for high-fold LED encapsulation, which can solve the problems of the influence of the service life of the material, the influence of the service life of the LED light source, and poor heat resistance.

Inactive Publication Date: 2018-01-16
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 of phenyl hydrogen-containing methyl MQ silicone resin with high refractive index for LED packaging
  • Preparation method of phenyl hydrogen-containing methyl MQ silicone resin with high refractive index for LED packaging

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 170 g of ethyl silicate, 111 g of hexamethyldisiloxane, 10 g of hydrogen-containing 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 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 277 g of clear and transparent silicone resin with phenyl hydrogen-containing network structure, the yield was 92%, and the viscosity was 30000 cs.

Embodiment 2

[0020] Add 170 g of ethyl silicate, 111 g of hexamethyldisiloxane, 20 g of hydrogen-containing 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, and after 1 h of reaction, the temperature was raised to reflux for 5 h, and 60 wt % of 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 clear and transparent silicone resin with phenyl vinyl network structure, the yield was 90%, and the viscosity was 20000 cs.

Embodiment 3

[0022] Add 170 g of ethyl silicate, 111 g of hexamethyldisiloxane, 30 g of hydrogen-containing 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, and after 1 h of reaction, the temperature was raised to reflux for 6 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 282 g of clear and transparent silicone resin with phenyl vinyl network structure, the yield was 88%, and the viscosity was 20000 cs.

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Abstract

The invention relates to a preparation method of phenyl hydrogen-containing methyl MQ silicone resin with high refractive index resin for LED packaging. The method comprises steps as follows: ethyl silicate is hydrolyzed under the action of sulfuric acid or a solid acid catalyst, silicic acid is obtained and is subjected to further condensation, and a product reacts with 1,3-diphenyl-1,1,3,3,-tetramethyldisiloxane and 1,1,3,3-tetramethyldisiloxane for end capping; after the reaction, the product is subjected to reflux to be highly crosslinked, then the product is neutralized with alkali liquorand distilled with toluene, and a toluene solution of the phenyl hydrogen-containing methyl MQ silicone resin is obtained finally. According to the synthesis technology, reaction activity is relatively lower, control is easy, reaction speed is high, reaction is sufficient, so that not only is effective yield of the product increased, but also the silicone resin which is colorless, transparent, high in refractive index and stable in equality and meets different requirements can be obtained according to difference of selected functional groups.

Description

technical field [0001] The invention relates to the technical field of organosilicon polymer compounds, in particular to a preparation method of phenyl hydrogen-containing methyl 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 mois...

Claims

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Application Information

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IPC IPC(8): C08G77/12C08G77/20C08G77/08
Inventor 卢旭刘明强原亚敏顾振涛
Owner 山东盛宇新材料有限公司
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