分别采用乙烯基三甲氧基硅烷和乙烯基三乙氧基硅烷为原料,盐酸作为催化剂,通过水解缩合反应合成了乙烯基笼型倍半硅氧烷,探讨了温度、盐酸和去离子水的配比、溶剂用量和聚合时间对实验产率的影响。并通过红外和核磁共振氢谱/碳谱等手段对产物进行了表征。结果表明:合成的化合物为乙烯基笼型倍半硅氧烷。同时,热失重分析表明,失重5%对应的温度在244.1℃,说明产物的热稳定性很高。
In the presence of hydrochloric acid as the catalyst,octavinyloctasilsesquioxane(OVPOSS) was synthesized by hydrolysis condensation reaction with vinyltrimethoxysilane and vinyltriethoxysilane as raw materials.The effects of polymerization time,temperature,the ratio of hydrochloric acid and deionized water,the amount of solvent on the yield of experimental were studied.The structure of OVPOSS was characterized by FT-IR,1H-NMR and 13C-NMR,the compound were proved to be OVPOSS.The temperature corresponding to 5% weight loss was 244.1℃ by TG plot.This showed that OVPOSS had a high stability to heat.
[1] 浦侃裔,范曲立,汪联辉,等.POSS聚合物及其新进展[J].化学进展,2006,18(5):609-615.
[2] Ronald H,Maki H,Akihito S,et al.Silsesquioxanes[J].Chem Rev,1995,95(21):1409-1430.
[3] Kim G M,Qin H,Fang X,et al.Hybrid epoxy-based thermosets based on polyhedral oligosilsesquioxane:cure behavior and toughening mechanisms[J].J Polym Sci Part B:Polym Phys,2003,41(24):3299-3313.
[4] Cordes D B,Lickiss P D,Pataboul F.Recentdevelopments in the chemistry of cubic polyhedral oligosilsesquioxanes[J].Chem Rev,2010,110(4):2081-2173.
[5] 张增平,梁国正.笼型倍半硅氧烷(POSS)合成的研究进展[J].高分子材料科学与工程,2011,27(9):179-182.
[6] Wen J Y,Wikes G L.Organic/inorganic hybrid network materials by the sol-gel approach[J].Chem Mater,1996,8(8):1667-1681.
[7] Lee T W,Park O O,Hong J M,et al.Mobilities of polymer organo-clay nanocomposite electroluminescent deviees[J].Thin Solid Films,2001,393(3):34-35.
[8] 范敬辉,张凯,吴菊英,等.二步法合成乙烯基八聚笼型倍半硅氧烷[J].化工新型材料,2010,38(S1):60-62.
[9] 张万里,陈清,陆凤英.八乙烯基笼型倍半硅氧烷的合成[J].有机硅材料,2012,26(6):392-395.
[10] 窦金涛,曹皎洁,李春晓,等.笼型八乙烯基倍半硅氧烷的合成及结晶行为研究[J].有机硅材料,2014,28(1):1-5.
[11] 陆方,严宝珍,胡高飞.笼型倍半硅氧烷NMR的研究[J].波普学杂志,2004,21(1):57-60.
[12] Lichtenhan J D,Hait S B,Schwab J J,et al.Process for continuous production of olefin polyhedral oligomeric silsesquioxane cages:US,0263318A1[P].2006-11-23.
[13] Lichtenhan J D,Gilman J W.Preceramic addi-tives as fire retardants for plastics:US,6362279B2[P].2002-03-26.
基金资助
辽宁省高等学校创新团队项目(LT2015022)
PDF
(1271KB)
