新型无溶剂有机硅耐高温树脂的制备及性能研究

以甲基三乙氧基硅烷、二甲基二乙氧基硅烷、二苯基二乙氧基硅烷、乙烯基三乙氧基硅烷为原料,在无水乙醇和水组成的混合溶剂中进行水解。经缩聚封端,脱除溶剂,活性稀释剂调整固含量等工艺,最终制得无溶剂甲基苯基耐高温硅树脂溶液。研究了水解温度、单体配比、用水量、乙烯基硅氧烷含量等因素对无溶剂硅树脂合成反应的影响,并得到最佳合成工艺:n(R)/n(Si)=1.3,n(Ph)/n(R)=0.4,水解温度为50℃。采用热失重测试研究了硅树脂的耐热性能。结果表明:无溶剂有机硅耐高温树脂具有优异的耐热性能,当温度达到350℃时热失重仅为2.4%,800℃时仍有73%的硅树脂残留分率。

Synthesis of Solvent-free Addition Heat-resistant Silicone Resin and Study on Its Properties

The solvent-flee addition heat-resistant silicone resin was synthesized by hydrolysis polycondensation with methyl triethoxysilane, dimethyldiethoxysilane, phenyltfiethoxysilane and tfiethoxyvinylsilane as monomers, in defined amount absolute ethyl alcohol and water mixed solvents, the self-made vinyl silicone oil was used to control the solid content. The factors influencing the synthesis were investigated. The results indicate that excellent solvent-free silicone resin can be synthesized when the hydrolysis temperature was 50℃ n（R）/n（Si）was 1.3, n（Ph）/n（R）was 0.4. The thermal properties of silicone resin were investigated using thermo-gravimetfic analysis（TGA）, It was found that silicone resin possesses excellent thermal stability, and has only 2.4 % mass loss when the temperature was 350℃, there was still 73 % remaining rate.