Preparation method of silicone resin type organic/inorganic hybrid material for packaging
A technology of hybrid material and silicone resin, which is applied in the direction of electrical components, circuits, semiconductor devices, etc., can solve the problems of long reaction time, easy gelation, low light transmittance of products, etc., and achieve short reaction time and high light transmittance Effect
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Embodiment 1
[0026] 1) To a 1L three-neck flask filled with 46ml xylene and 360ml water, add 50ml PhSiCl dropwise within 2 hours under stirring at 40°C 3 , 22ml MeViSiCl 2 , 18ml Me 2 SiCl 2 , 11ml TiCl 4 , Mixed solution of 88ml xylene, continue to stir for 1h. Stand still, separate layers, and remove the acid solution in the lower layer. Wash with deionized water at 40°C~50°C until neutral.
[0027] 2) Take 50g of the obtained prepolymer solution, add 50g of solvent for xylene, 0.15g of KOH, reflux in a 250ml three-necked flask at 100°C for 5h, cool, and add 1.5g of end-capping agent MeSiCl 3 , stirred for 1 h, washed with deionized water until neutral. Concentrate at 0.8~0.96MPa, and remove the remaining xylene and water generated by polycondensation reaction to obtain clear and transparent silicone resin.
[0028] 3) Mix the obtained vinyl silicone resin with dimethylhydrogen silicone oil containing 0.7wt% hydrogen according to Si-H:Si-Vi=1.5:1, platinum complex catalyst H 2 Pt...
Embodiment 2
[0030] 1) To a 1L three-neck flask filled with 46ml of toluene and 360ml of water, add 50ml of PhSiCl dropwise within 2h under stirring at 60°C 3 , 22ml MeViSiCl 2 , 18ml Me 2 SiCl 2 , 9ml of zinc isooctanoate, 88ml of toluene mixed solution, continue to stir for 1h. Stand still, separate layers, and remove the acid solution in the lower layer. Wash with deionized water at 40°C~50°C until neutral.
[0031] 2) Take 50g of the obtained prepolymer solution, add 50g of toluene, 0.15g of tetrabutylammonium hydroxide, reflux in a 250ml three-necked flask at 100°C for 5h, cool, and add 4.5g of capping agent α,ω-dimethylphenylsilane Vinyl silicone oil, stirred for 1 h, washed with deionized water until neutral. Concentrate at 0.8~0.96MPa, and remove the remaining toluene and the water generated by the polycondensation reaction to obtain a clear and transparent silicone resin.
[0032] 3) Mix the obtained vinyl silicone resin with methylphenyl hydrogen-containing silicone oil wit...
Embodiment 3
[0034] 1) To a 1L three-neck flask filled with 46ml of toluene and 360ml of water, add 50ml of PhSiCl dropwise within 2h under stirring at 60°C 3 , 22ml MeViSiCl 2 , 18ml Me 2 SiCl 2 , 9ml MePhSiCl 2 , 15ml of zirconium isooctanoate, 88ml of toluene mixed solution, continue to stir for 1h. Stand still, separate layers, and remove the acid solution in the lower layer. Wash with deionized water at 40°C~50°C until neutral.
[0035] 2) Take 50g of the obtained prepolymer solution, add 50g of toluene and 0.15g of KOH, reflux in a 250ml three-necked flask at 100°C for 5h, cool, add 6.0g of decamethyltetrasiloxane as an end-capping agent, stir for 1h, deionized water Wash to neutral. Concentrate at 0.8~0.96MPa, and remove the remaining toluene and the water generated by the polycondensation reaction to obtain a clear and transparent silicone resin.
[0036] 3) Mix the obtained vinyl silicone resin with methylphenyl hydrogen-containing silicone oil with a hydrogen content of 0....
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