Preparation method of vinylphenyl silicon resin for LED (light-emitting diode) packaging
A vinyl phenyl and LED encapsulation technology, which is applied in the field of silicone resin preparation, can solve the problems of large pollution and poor resin stability, and achieve the effects of simple operation, stable product structure and quality, and cheap and easy-to-obtain raw materials
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Embodiment l
[0027] Into a 3000ml glass kettle, add 300ml of water, 500ml of toluene, 300ml of ethanol, MM20g, 1,3-divinyl-1,1,3,3-tetramethyldisiloxane 70g, concentrated hydrochloric acid (36.5wt% ) 20g, stirred rapidly at 40°C, and added dropwise an ethanol solution of 1000g of phenyltrimethoxysilane and 60g of methylphenyldimethoxysilane. Hydrolyze for 3 hours, then raise the temperature to 70°C and reflux for 5 hours, then stop the reaction, let the layers stand, remove the oil agent in the lower layer, neutralize it with aqueous sodium bicarbonate solution, wash it with deionized water until it is neutral, and use anhydrous chlorinated Calcium dries until clear and transparent. Add 20 g of silazane, react at 80°C for 3 hours, then raise the temperature, pull it down to 150°C under high vacuum -0.099Mpa for 6 hours, remove low boilers, and obtain 807g of clear and transparent vinyl phenyl silicone resin . The obtained product has a refractive index of 1.5145, a viscosity of 3300 ...
Embodiment 2
[0029]In a 3000ml glass kettle, add 300ml of water, 500ml of toluene, 300ml of ethanol, 100g of MM, 150g of 1,3-divinyl-1,1,3,3-tetramethyldisiloxane, concentrated hydrochloric acid (36.5wt%) ) 20 g, stirred rapidly at 40° C., and added dropwise 900 g of phenyltrimethoxysilane and 20 g of ethyl orthosilicate in ethanol. Hydrolyze for 3 hours, then heat up to 70°C and reflux for 5 hours, then stop the reaction, let stand to separate layers, remove the oil agent in the lower layer, neutralize it with aqueous sodium bicarbonate solution, add KOH 30 g, react at 80°C for 3 hours, cool down, and use Wash with deionized water until neutral, and dry with anhydrous calcium chloride until clear and transparent. Then the temperature was raised, and the temperature was lowered to 150°C under high vacuum -0.099Mpa for 6 hours to remove the low boilers, and 827g of vinyl phenyl silicone resin was obtained as a clear and transparent product. The obtained product had a refractive index of 1....
Embodiment 3
[0031] Into a 3000ml glass kettle, add water 300ml, toluene 500ml, ethanol 300ml, MM30g, 1,3-divinyl-1,1,3,3-tetramethyldisiloxane 170g, concentrated hydrochloric acid (36.5wt% ) 22g, stirred rapidly at 40°C, and added dropwise an ethanol solution of 800g of phenyltrimethoxysilane and 150g of methylphenyldimethoxysilane. Hydrolyze for 3 hours, then raise the temperature to 70°C and reflux for 5 hours, then stop the reaction, let the layers stand, remove the oil agent in the lower layer, neutralize it with aqueous sodium bicarbonate solution, wash it with deionized water until it is neutral, and use anhydrous chlorinated Calcium dries until clear and transparent. Add 20 g of silazane, react at 80°C for 3 hours, then raise the temperature, pull it down to 150°C under high vacuum -0.099Mpa for 6 hours, remove low boilers, and obtain 840g of clear and transparent vinyl phenyl silicone resin . The obtained product had a refractive index of 1.5356, a viscosity of 5358 mPa.s, a...
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