Preparation method of methyl phenyl vinyl silicone oil
A technology of methylphenylethylene and phenyldialkoxysilane, which is applied in the field of organic polymer materials, can solve problems such as non-uniform alternate polymerization, affecting light transmittance, cumbersome synthesis process, etc., and achieves uniform distribution of organic groups , Improving mechanical properties, easy refractive index effect
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Embodiment 1
[0040] In a 1L four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 244.0 g of diphenyldimethoxysilane, 180.0 g of dimethyldimethoxysilane, 6.55 g of dimethyl A mixture of vinylethoxysilane, 1.3g of concentrated sulfuric acid and 200.0g of toluene was stirred at 45°C for 1h, then at 35-50°C, 136.4g of deionized water was added dropwise within 2h, and the temperature was raised to Reflux at 70°C for 4 hours to carry out hydrolysis and condensation reaction to obtain a hydrolysis mixture;
[0041] Stand to cool the hydrolysis mixture to room temperature, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.5 g of potassium hydroxide to the organic layer and raise the temperature to 130 ° C for 4 hours to obtain azeotropic reflux liquid;
[0042] Then the azeotropic reflux liquid is cooled to room temperature, and 60.0g of cationic resin is added to stir and neutral...
Embodiment 2
[0046] In a 1L four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 218.0 g of diphenyldiethoxysilane, 89.0 g of octamethylcyclotetrasiloxane, 13.1 g of dimethyl The mixture of vinylethoxysilane, 5.8g concentrated hydrochloric acid and 200.0g xylene was stirred at 45°C for 0.5h, then at 35-50°C, 45.9g deionized water was added dropwise within 2h, after the dropwise addition was completed Heat up to 72°C and reflux for 5 hours to obtain a hydrolysis mixture;
[0047] Stand to cool the mixture to room temperature, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.5 g of sodium hydroxide to the organic layer and raise the temperature to 140 ° C for 5 hours to obtain the azeotropic reflux liquid ;
[0048] Then the azeotropic reflux liquid was cooled to room temperature, and 40.0 g of cationic resin was added to stir and neutralize, and the Na in the mixture was s...
Embodiment 3
[0052] In a 1L four-necked flask equipped with a reflux condensing device, a dropping funnel, a stirring device and a thermometer, add 73.2g of diphenyldimethoxysilane, 81.7g of diphenyldiethoxysilane, 48.0g of dimethyl A mixture of dimethoxysilane, 59.2g dimethyldiethoxysilane, 3.93g dimethylvinylethoxysilane, 0.5g trifluoromethanesulfonic acid and 200.0g toluene, stirred at 30°C 4h, then drop 76.4g of deionized water within 1h at 35~50°C, after the dropwise addition, raise the temperature to 80°C and reflux for 2h to obtain a hydrolysis mixture;
[0053] Stand to cool the hydrolysis mixture to room temperature, separate the organic layer and wash the organic layer with deionized water to neutrality, then add 0.5g sodium hydroxide to the organic layer, raise the temperature to 150°C and azeotropically reflux for 6h to obtain an azeotropic Reflux liquid;
[0054] Then the azeotropic reflux liquid was cooled to room temperature, and 40.0 g of acid clay was added to stir and ne...
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