Preparation method of methyl phenyl vinyl silicone resin
A technology of methylphenylethylene and tetraethoxysilane, applied in the field of organic polymer materials, can solve the problems of difficult control of polymerization degree, unstable quality, cumbersome synthesis process, etc., and achieve good reaction repeatability and controllability , process is easy to control, storage performance is stable
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Embodiment 1
[0033] In a four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 140.4g of deionized water, 1.1g of concentrated sulfuric acid and 200.0g of toluene and mix and stir for 30min. Under stirring conditions at 40°C, within 2h Add dropwise 237.6g of phenyltrimethoxysilane, 16.2g of hexamethyldisiloxane, 26.2g of dimethylvinylethoxysilane, 41.6g of tetraethoxysilane, 24.0g of dimethyldimethoxy A mixture of silane and 22.4g of diphenyldimethoxysilane was subjected to hydrolysis reaction, and after the dropwise addition was completed, the temperature was raised to 72°C for reflux reaction for 4 hours to obtain a mixed solution;
[0034] Cool and let the mixed solution stand, separate the organic layer and wash the separated organic layer with deionized water to neutrality, then add 0.4g potassium hydroxide to the organic layer, raise the temperature to 140°C and azeotropically reflux for 4h to obtain an azeotropic Refl...
Embodiment 2
[0038] In a four-neck flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 126.9 g of deionized water, 6.5 g of concentrated hydrochloric acid and 200.0 g of xylene and mix and stir for 1 h. Under the condition of stirring at 35°C, 240.4g phenyltriethoxysilane, 24.3g hexamethyldisiloxane, 13.1g dimethylvinylethoxysilane, 41.6g tetraethoxysilane were added dropwise within 1h , a mixture of 29.7g dimethyldiethoxysilane and 48.8g diphenyldimethoxysilane was subjected to hydrolysis reaction, and after the dropwise addition was completed, the temperature was raised to 70°C for reflux reaction for 5 hours to obtain a mixed solution;
[0039] Cool and let the mixed solution stand, separate the organic layer and wash the organic layer with deionized water until neutral. Add 0.4 g of sodium hydroxide to the organic layer, raise the temperature to 140° C. and azeotropically reflux for 6 hours to obtain an azeotropic reflux liquid; ...
Embodiment 3
[0043] In a four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 156.6g of deionized water, 1.4g of nitric acid and 200.0g of isopropanol and mix and stir for 2h. Under stirring conditions at 45°C, 2h 158.8g of phenyltrimethoxysilane, 54.4g of methyltrimethoxysilane, 91.0g of methylphenyldimethoxysilane, 26.0g of methylvinyldimethoxysilane, 32.4g of hexamethyldimethoxysilane were added dropwise The mixture of siloxane, 20.8g tetraethoxysilane and 36.0g dimethyldimethoxysilane was subjected to hydrolysis reaction, and after the dropwise addition was completed, the temperature was raised to 75° C. for reflux reaction for 6 hours to obtain a mixed solution.
[0044] Cool and let the mixed solution stand, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.4 g of cesium hydroxide to the organic layer, heat up to 130 ° C and azeotropically reflux for 5 hours to obtain ...
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