笼形八聚(二甲基硅氧基)倍半硅氧烷的合成与表征  

Synthesis and Characterization of Octakis(dimethylsiloxy)silsesquioxane

作　　者：张晓静[1] 韩喜妞[1] 方少明[1] 李亚东[1] 张忠厚[1] 张成贵[1] 

机构地区：[1]郑州轻工业学院材料与化学工程学院河南省表界面科学重点实验室,河南郑州450002

出　　处：《精细化工》2010年第3期209-212,233,共5页Fine Chemicals

基　　金：国家自然科学基金(No.20804041);河南省教育厅自然科学基金(No.2009A430025);河南省高校科技创新团队支持计划资助项目(No.2008IRTSTHN004);郑州轻工业学院博士科研基金(No.000310)~~

摘　　要：以四乙氧基硅烷〔Si(OEt)4〕与五水合四甲基氢氧化铵(Me4NOH.5H2O)为原料水解缩合得到笼形八聚四甲基铵硅酸盐([SiO1.5ONMe4]8),继而与二甲基氯硅烷〔HSi(CH3)2Cl〕反应,一锅法合成了笼形八聚(二甲基硅氧基)倍半硅氧烷(Q8M8H),最佳反应条件为:反应温度25℃,反应时间36 h,n〔Si(OEt)4〕∶n(Me4NOH.5H2O)∶n〔HSi(CH3)2Cl〕=1∶1∶4,产率80%。FTIR和NMR研究证明,所得产物为Q8M8H;SEM、EDS和XRD研究表明,所制备的Q8M8H具有较高的纯度和完整的晶型结构,属于单斜晶系,a=1.18 nm,b=1.52 nm,c=1.51nm,α=γ=90°,β=108°;TG表明,Q8M8H热失重5%时的温度为210℃。The cage-like octakis（dimethylsiloxy）silsesquioxane（Q8M8^H） was synthesized via the one-pot method,in which the tetramethylammonium silicate octamer was prepared at first by the hydrolysis and polycondensation of tetraethoxysilane with the aqueous tetramethylammonium hydroxide and then the tetramethylammonium silicate octamer was silanized by dimethylchlorosilane to give the product.The optimal experiment condition was determined as： reaction temperature 25 ℃,reaction time 36 hours,n（Si（OEt）4）∶n（Me4NOH·5H2O）∶n（HSi（CH3）2Cl）=1∶1∶4,the yield was 80%.The FTIR,^1HNMR and ^29Si-NMR results proved that Q8M8^H was successfully synthesized.The product has a high purity and complete crystal structure with monoclinic crystal system,a=1.18 nm,b=1.52 nm,c=1.51 nm,α=γ=90°,β=108°,which was confirmed by SEM、EDS and XRD.TG analysis and showed that 5% mass loss temperature of Q8M8H was 210 ℃.

关 键 词：倍半硅氧烷 二甲基氯硅烷 表征 功能材料 

分 类 号：O623.1[理学—有机化学]