巯基官能化倍半硅氧烷的合成及表征

Synthesis and characterization of a mercaptopropyl polyhedral oligomeric silsesquioxane(POSS)

以巯丙基三甲氧基硅烷为原料,在甲醇体系中进行水解缩合,在盐酸催化下合成得到笼型、无规、梯形等多种结构倍半硅氧烷的混合物;在四甲基氢氧化铵或苄基三甲基氢氧化铵碱性条件催化下,均可合成得到成分单一、纯净的巯基官能化笼型结构倍半硅氧烷,其产率分别为46%和64%。利用FT-IR、13C-NMR2、9Si-NMR、XRD和DSC等手段,对其结构和性质进行了表征。巯基笼型倍半硅氧烷具有较高的熔点352℃和分解温度530℃,热性能优良且具进一步反应性。

（3-Mercaptopropyl）trimethoxysilane has been hydrolyzed and condensed in methanol solution. The results showed that a mixture of cage, random and trapezoidal silsesquioxane structures was synthesized in the presence of a hydrochloric acid catalyst. Mercaptopropyl polyhedral oligomeric silsesquioxane （POSS） was ob- tained in the presence of the alkaline catalysts Me4NOH or （C6H5CH2）Me3NOH, and the yields were 46 % and 64%, respectively. The products were characterized by FT-IR, ^13C-NMR, ^29Si-NMR, XRD and DSC. POSS had excellent thermal performance with a high melting point of 352 ℃ and decomposition temperature of 530℃.