文献类型：期刊文献

中文题名：笼型单乙烯基倍半硅氧烷的合成及表征

英文题名：Synthesis and characterization of monovinyl-functionalized silsesquioxane cage

作者：刘勇[1];周燕[1];黄福伟[1];王灿锋[1];沈学宁[1];黄发荣[1]

机构：[1]特种功能高分子材料及相关技术教育部重点实验室(华东理工大学),上海200237

年份：2009

卷号：60

期号：7

起止页码：1831

中文期刊名：化工学报

外文期刊名：CIESC Journal

收录：CSTPCD;;EI(收录号：20093112228512);Scopus;北大核心:【北大核心2008】；CSCD:【CSCD2011_2012】；

基金：国家自然科学基金项目(90816021)~~

语种：中文

中文关键词：笼型单乙烯基倍半硅氧烷;热稳定性;有机-无机杂化材料

外文关键词：monovinyl-functionalized silsesquioxane cage; thermal stability; organic-inorganic hybrid materials

摘要：用环戊基三氯硅烷合成不完全缩合三羟基硅氧烷[(C5H9)7Si7O9(OH)3],再以乙烯基三氯硅烷和不完全缩合三羟基硅氧烷为原料,以四氢呋喃和三乙胺为混合溶剂,通过"顶角-戴帽"反应合成了笼型单乙烯基倍半硅氧烷,即1,3,5,7,9,11,13-七环戊基-15-乙烯基笼型倍半硅氧烷(VinylPOSS)。利用FTIR、1H NMR、29Si NMR、13C NMR、元素分析、WAXD和TGA表征了VinylPOSS的结构及热稳定性。研究结果表明Vinyl-POSS的产率随着反应时间的增加而提高,当反应时间为10 h时,产率高达90%;其在弱极性溶剂中具有较好的溶解性,5%失重温度为283℃,800℃残留率为56%,具有较高的热稳定性。研究了VinylPOSS和高含氢硅油(HHSF)的反应性,结果表明VinylPOSS能与含氢硅油发生α、β加成反应,且以β加成为主。
Monovinyl-functionalized silsesquioxane cage, 1, 3, 5, 7, 9, 11, 13-heptacyclopentyl-15-vinyl silsesquioxane （VinylPOSS）, was prepared via the corner capping reaction of incompletely condensed silsesquioxanes, （C5H9）7Si7O9（OH）3 , with vinyltrichlorosilane. VinylPOSS was characterized by FTIR, ^1H NMR, ^29Si NMR, ^13C NMR, elemental analysis, WAXD and TGA. The yield of VinylPOSS increased with reaction time, when vinyltrichlorosilane reacted with （C5H9）7Si7O9（OH）3 for 10 h, the yield was 90%. VinylPOSS has good solubility in weak polar solvent, and it shows good thermal stability, its temperature with 5% decomposition is 283℃ and the temperature with 56% residue is 800℃. The reactivity of VinylPOSS with high hydrogen-containing silicone fluid （HHSF） was investigated. It can be reacted with HHSF by Michael additions at both α- and β-positions, and the reaction is mainly β-addition.