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.
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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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