摘要
以甲基异丁基甲酮和无水乙醇为混合溶剂,浓盐酸为催化剂,环己基三乙氧基硅烷水解缩聚高产率地合成了笼型八聚环己基倍半硅氧烷.讨论了影响反应的各个因素,得到了反应的最佳条件,当单体浓度为0.45mol/L,水和催化剂的用量与单体的摩尔比约为3左右时,反应具有较高的产率,且高温有利于八聚体的形成和缩短反应时间.合成化合物用元素分析、FTIR、1H1、3C、29S i NMR和MS进行了表征,证实其结构式为(c-C6H11)8S i8O12.热性能分析结果表明该化合物具有较高的热稳定性.
The compound of octa （cyclohexylsilsesquioxane） （ c - C6H11 ） 8 Si8 O12 was prepared in higher yield by the hydrolysis and polycondensation of trifunctional monomer （c -C6H11 ）Si （OC2H5 ）3 in the mixture solvents of methyl isobutyl ketone and anhydrous ethanol with the concentratiou hydrochloric acid as the catalyst. The effects of reaction conditions, such as monomer concentration, the contents of water and catalyst were investigated. The results show that the better values of these reactive factors were 0. 45mol/L, H20： XSiY3 = 3 ： 1 （molar ratio）, Et4NOH： XSiY3 = 3：1 （molar ratio）, respectively. The higher reaction temperature can accelerate the formation of octamer, reduce the reaction time and increase the yield. FFIR spectrum and ^1H, ^13C, ^29Si NMR spectra show the compound has the formula of （c - C6H11 ）8Si8O12 and the cage structure. TGA curve shows that the cage compound has a high decomposition temperature of 343.68℃, high thermal residue and the inorganic composition does not change during the thermal processing.
出处
《材料科学与工艺》
EI
CAS
CSCD
北大核心
2006年第5期527-531,534,共6页
Materials Science and Technology
基金
陕西省自然科学基金项目(2006B12)
陕西省教育厅专项科研基金(03JK075)
关键词
八聚倍半硅氧烷
笼型结构
水解-缩聚反应
Octa（cyclohexylsilsesquioxane） , Cage structure, Hydrolysis - Condensation reaction
