笼状纳米化合物八乙烯基倍半硅氧烷的合成及表征  

Synthesis and characterization of nanocompound octavinyl polyhedral oligomeric silsesquioxane

作　　者：薛裕华[1] 顾雪萍[1] 冯连芳[1] 王嘉骏[1] 胡国华[2] 

机构地区：[1]浙江大学化学工程与生物工程系化学工程国家重点实验室,浙江杭州310027 [2]法国国家科学研究中心化学工程科学实验室,法国南锡54001

出　　处：《浙江大学学报（工学版）》2007年第4期679-682,共4页Journal of Zhejiang University：Engineering Science

基　　金：国家"973"重点基础研究发展规划资助项目(2001CB711203)

摘　　要：以无水三氯化铁和浓盐酸为催化剂,甲醇-石油醚-二氯甲烷为溶剂,乙烯基三氯硅烷水解缩合得到了笼状八乙烯基多面体低聚倍半硅氧烷.该方法反应时间短,产率高(34.7%).通过1H1、3C和29Si核磁共振光谱、红外光谱、元素分析和凝胶渗透色谱等对产物的结构进行了表征,表明产物是笼状的八乙烯基倍半硅氧烷.采用TGA对OvPOSS的热稳定性进行了研究.结果表明,OvPOSS初始分解温度(失重5%)为278.5℃,热稳定性良好.对反应条件的研究发现,温度对OvPOSS产率影响不大,而适度延长反应时间或提高溶剂中甲醇的质量分数均可以提高OvPOSS的产率.Octavinyl polyhedral oligomeric silsesquioxane （OvPOSS） was synthesized via hydrolytic condensation of vinyltrichlorosilane catalyzed by concentrated hydrochloric acid and anhydrous FeCl3. This synthesis approach was versatile, and OvPOSS was obtained rapidly at high yield （34.7%）. The structure of the synthesized product was determined and validated by ^1H, ^13C, ^29Si nuclear magnetic resonance （NMR）, Fourier transform infrared spectroscopy（FTIR）, elementary analysis and gel permeation chromatogram （GPC）. The initial decompose temperature analyzed by thermogravimetric analysis （TGA） was equal to 278.5 ℃,which showed that OvPOSS has good stability to heat. The influence of reaction conditions on the vinyltrichlorosilane hydrolytic polycondensation was studied. Increase in temperature has no significant effect on the yield of OvPOSS, but either prolonging the reaction time or enhancing concentration of methanol in solution leads to the increase of OvPOSS yield.

关 键 词：多面体低聚倍半硅氧烷 水解 缩合 

分 类 号：TQ264.1[化学工程—有机化工]