笼型八聚(γ-氨丙基)硅倍半氧烷盐酸盐的合成与表征  

Synthesis and characterization of octaammonium chloride salt of octaaminopropyl polyhedral oligomeric silsesquioxane

作　　者：沈媛[1] 李齐方[1] 

机构地区：[1]北京化工大学材料科学与工程学院,北京100029

出　　处：《有机硅材料》2007年第1期14-17,共4页Silicone Material

基　　金：国家自然科学基金资助项目(20374007;50203002)

摘　　要：在盐酸催化下,将γ-氨丙基三乙氧基硅烷在甲醇溶液中水解缩合,合成出笼型八聚(γ-氨丙基)硅倍半氧烷盐酸盐;并用四氢呋喃作沉淀剂将产物沉淀出来。利用红外、核磁和差热分析等对其结构和性质进行了表征,讨论了反应温度、反应时间、盐酸和四氢呋喃用量对反应产率的影响。结果表明,较佳合成工艺为:γ-氨丙基三乙氧基硅烷用量15mL,甲醇用量360mL,盐酸用量30mL,四氢呋喃用量250mL,在90℃下反应18h;产物熔点为412.65℃。Octaammonium chloride salt of octaaminopropyl polyhedral oligomeric silsesquioxane(oap-POSS) was synthesized by hydrolytic condensation of γ-aminopropyltrithoxysilane in the methanol solution catalyzed by concentrated hydrochloric acid.The salt was precipitated with tetrahydrofuran.It was characterized by FTIR, ~1H NMR, ~ 29 Si NMR, ~ 13 C NMR and DSC.The effects of temperature,reaction time,amount of hydrochloric acid,amount of THF on yield were discussed in details.The optimal reaction conditions were as follows: the volume of γ-aminopropyltrithoxysilane,methanol,hydrochloric acid and tetrahydrofuran was 15 mL,360 mL,30mL,and 250 mL respectively.The reaction temperature was 90℃ and the reaction time is 18 hours.DSC analysis showed the melt point was 412.65℃.

关 键 词：笼型 八聚(γ-氨丙基)倍半硅氧烷盐酸盐 Γ-氨丙基三乙氧基硅烷 甲醇 盐酸 四氢呋喃 

分 类 号：O627.415[理学—有机化学]