A kind of organosilicon ternary encapsulation material and preparation method thereof
A packaging material and organosilicon technology, applied in the field of preparation of organosilicon packaging materials, can solve problems such as being unfavorable for large-scale promotion and industrialized production, low refractive index and thermal conductivity, and high cost of laser sintering process, and achieve compatibility. The effect of improving the property and bonding degree, increasing the cross-linking density, and small filling amount
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[0035] The invention provides a method for preparing an organosilicon ternary packaging material, comprising the following steps: S1: Surface modification of the micro-nano silicon dioxide material: uniformly dispersing the micro-nano silicon dioxide material in benzyl alcohol, pressurized and heated to react , cooled, and centrifuged to obtain a surface-modified micro-nano silica material; S2: the surface-modified micro-nano silica material prepared in S1 is miscible with epoxy-based organosilicon monomers, emulsified and dispersed , centrifugally dispersed to obtain a transparent solution, which was concentrated into solution A under dry inert gas conditions; S3: under the action of a catalyst, the silicon glycol crosslinking agent, the solution A and vinyl organosilicon monomer synthesized the first intermediate, silicon Diol crosslinking agent, the solution A and pure silicone monomers are synthesized to obtain the second intermediate, wherein the vinyl silicone monomers in...
Embodiment 1
[0041] Weigh 2g (0.0333moL), 3.33g (0.555mol), 5g (0.833mol), 6.66g (1.11mol), 8.325g (1.39mol), 9.99g (1.665mol) of micron quartz powder in 30mL freshly steamed Evenly dispersed in benzyl alcohol, then poured into a 45mL stainless steel pressure reactor and heated at 240°C for 96 hours, and then centrifuged after cooling to room temperature. Repeat the operation at least 2 times to ensure the surface treatment of the quartz particles is complete. Next, take 0.0315g and 9uL of γ-(2,3-glycidoxy)propyltrimethoxysilane and dissolve them in 20mL of freshly distilled tetrahydrofuran (THF), and ultrasonically emulsify and disperse at room temperature for more than 30 minutes , using the condensation reaction of some hydroxyl groups on the surface of micron-sized quartz with trimethoxysilane to achieve the effect of surface modification. Then, it was centrifuged to obtain a transparent solution A, which was dried and concentrated under dry nitrogen to obtain 5 mL of solution B.
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Embodiment 2
[0050] After 2g of micron quartz (0.0333moL) was treated by benzyl alcohol reprecipitation as described in Example 1, 0.0945g and 27uL of γ-(2,3-glycidoxy)propyltrimethoxy Silane was miscible in 30 mL of freshly distilled tetrahydrofuran and ultrasonically emulsified and dispersed at room temperature for more than 30 minutes, and then centrifuged to obtain a transparent solution C. Blow dry under dry nitrogen to obtain 5 mL of solution D.
[0051] Synthesize diphenylsilanediol and solution D with vinyltrimethoxysilane and methyldiethoxysilane respectively under the action of a catalyst to obtain a first intermediate and a second intermediate. The ratio of vinyltrimethoxysilane to methylphenylsilanediol is 1:1, and the ratio of methyldiethoxysilane to diphenylsilanediol is 1:1.5. Put the first intermediate and the second intermediate above into a vacuum oven and dry at 45° C. for 4 hours.
[0052] Intermediates The first intermediate and the second intermediate were stirred f...
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