甲基苯基硅油合成反应的影响因素

Study on Key Influencing Factors in Synthesis of Methyl Phenyl Silicone Oil

以甲基苯基二甲氧基硅烷和四甲基二乙烯基二硅氧烷为原料,通过水解缩合反应制得甲基苯基硅油。采用正交实验研究了催化剂、水解反应时间、水的用量、缩合反应温度和时间等对甲基苯基硅油合成反应的影响。结果表明,缩合温度是反应最主要的影响因素,且聚合物的平均摩尔质量可通过封端剂用量来控制。最佳合成条件为:KOH作催化剂、用量1.5%,水与甲基苯基二甲氧基硅烷的量之比为1.7∶1,原料在72℃水解回流反应2 h后,于110℃缩合反应5 h。在此条件下,可制得高透明、高折射率性质稳定的甲基苯基硅油,能用于LED封装材料等领域。

Methylphenyl disiloxane by the hydrolysis silicone oil was obtained by condensation reaction. Orth methylphenyldimethoxysilane and divinyhetramethyl- ogonal experiment was used to discuss the effects of catalyst, hydrolysis time, water amount, condensation temperature and time. Results showed that the condensation temperature was the most important factor in the reaction, and the average molar mass of the polymer could be controlled by the amount of the end-capping reagent. The optimal synthetic conditions were as follows： KOH as the catalyst, the amount was 1.5%, the molar mass ratio of water and methylphenyldimethoxysilane was 1.7： 1, the raw materials were hydrolyzed at 72℃ for 2 h then condensed at 110℃ for 5 h. Under the optimal conditions, the high transparent, high-refractive and stable methylphenyl silicone oil was obtained, applied in the field of LED packaging.