高度单分散氰基聚倍半硅氧烷微球的可控合成及羧基化

Controlled Synthesis and Carboxylation of Highly Monodisperse Poly(cyanoethylsilsesquioxane)Microspheres

在水溶液中,以氰乙基三乙氧基硅烷(CTES)为前驱体,氨水为催化剂,通过一步法合成聚氰基倍半硅氧烷(PCSQ)微球,并通过进一步酸化实现了氰基到羧基的转化。通过扫描电子显微镜(SEM)、傅里叶变换红外光谱(FTIR)、热重(TG)分析对所得微球的形貌、有机功能基及热性能进行了表征,研究表明CTES的用量与催化剂氨水的浓度对PCSQ微球的形貌和粒径有着重要影响,当去离子水为30mL、CTES为1mL、氨水为1mL时,可以制备出平均粒径在600nm、高度单分散的PCSQ微球。将所制备的PCSQ微球分散在30%硫酸溶液中,65℃搅拌24h可以将微球上负载的氰基水解酸化为羧基。

In aqueous solution, poly（cyanoethylsilsesquioxane） （PCSQ） microspheres have been prepared suc- cessfully via one-step method using 2-cyanoethyltriethoxysilane（CTES） as a precursor and ammonia hydroxide as cata- lyst. The morphology, functional groups and thermal performance of the obstained microspheres were characterized by scanning electron microscopy（SEM）, fourier transform infrared spectroscopy （FTRT） and therrnogravimetric analysis （TGA）, respectively. The results showed that,morphology of the microspheres could be greatly influenced by concen- tration of the organosilane precursor and the ammonia. Highly monodisperse PCSQ microspheres with average diame- ter of 600 nm could be prepared under the condition of 30 mL deionized water, 1 mL CTES, 1 mL ammonia. Dispersed in 30%HzSO4 solution and stirred for 24 h under 65℃ ,the -CN groups of PCSQ can be hydrolyzed to-COOH.