High refractive index silicone resin and its preparation method and application
A silicone and resin technology, applied in the field of high-performance polymer manufacturing, can solve problems such as decreased adhesion, general temperature resistance, and low refractive index
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Embodiment 1
[0104] The preparation of embodiment 1 p-methoxyphenyltriethoxysilane
[0105]
[0106] Under the protection of argon, add 1.44 grams (0.06mol) of magnesium strips, 20.8 grams (0.1mol) of tetraethyl orthosilicate, a small amount of iodine and 100 milliliters of dry-treated toluene into a dry 250 milliliter three-neck flask, stir and slowly add 9.35 g (0.05 mol) of 4-bromoanisole and 20 ml of dry treated tetrahydrofuran mixture, heat slightly until the color of the system fades, react in an ice-water bath for 24 hours, remove the solvent after filtration with diatomaceous earth, and collect under reduced pressure at 80°C / 10 mba fraction 7.34 g, 54% yield. 1 H NMR (400MHz, CDCl3, δin ppm): 7.58-7.60 (d, 2H), 6.89-6.91 (d, 2H), 3.79-3.86 (m, 9H), 1.20-1.24 (t, 9H).
Embodiment 2
[0107] The preparation of embodiment 2 methyl vinyl silicone resin
[0108] Add 50 milliliters of water, 50 milliliters of concentrated hydrochloric acid and 30 milliliters of toluene into a clean 500 milliliter three-necked flask, and add 5.2 grams (0.025mol) of ethyl orthosilicate, 50.0 grams (0.25mol) of ) phenyltrimethoxysilane, 27.3 grams (0.15mol) methylphenyldimethoxysilane, 6.61 grams (0.05mol) methylvinyldimethoxysilane, 9.5 grams (0.05mol) vinyltriethyl A mixed solution of oxysilane and 20ml of toluene, the reaction temperature is controlled below 20°C, continue to react for 3h after the dropwise addition, then heat to 80°C for 3h, cool to room temperature, wash with water until neutral, the organic layer is washed with anhydrous Dry over sodium sulfate, remove toluene after filtration, heat up under reduced pressure to 150°C / 10mba to remove small molecule compounds, and obtain 25.5 g of methylphenylvinyl silicone resin with a refractive index of 1.544.
Embodiment 3
[0109] Embodiment 3 Preparation of p-methoxyphenylmethylphenylvinyl silicone resin
[0110] Add 25 milliliters of water, 25 milliliters of concentrated hydrochloric acid and 15 milliliters of toluene into a clean 250 milliliter three-necked flask, and add 5.4 grams (0.02 mol) of p-methoxyphenyltriethoxysilane dropwise through a constant pressure dropping funnel under vigorous stirring , 27.7 grams (0.14mol) of phenyltriethoxysilane, 19.5 grams (0.08mol) of diphenyldimethoxysilane, 10.0 grams (0.075mol) of methylvinyldimethoxysilane and 10 milliliters of toluene Mix the solution, control the reaction temperature below 20°C, continue the reaction for 3 hours after the dropwise addition, then heat to 80°C and continue the reaction for 3 hours, cool to room temperature, wash with water until neutral, dry the organic layer with anhydrous sodium sulfate, filter and remove Toluene was heated under reduced pressure to 150°C / 10mba to remove small molecular compounds, and 12.2 g of p-me...
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