以无水乙醇为溶剂,将乙烯基三甲氧基硅烷和甲基三甲氧基硅烷在酸性条件下进行共水解共缩聚反应合成二乙烯基六甲基八聚笼型倍半硅氧烷。讨论了影响反应的各种因素,得出了该反应的最佳条件,在单体浓度为0.35 mol/L,催化剂浓度为0.4 mol/L,水与单体物质的量比为6时,于50℃反应40 h得到的产物有最高的产率。利用红外、核磁共振(1H-NMR、29S-i NMR)和X射线衍射(XRD)对其结构进行了表征,结果证明,产物形成了完整的笼型结构,产物的结构式为[Si8O12(CH=CH2)2(CH3)6],XRD测试也表明产物具有较好的结晶性。
The compound of polyhedral oligomeric silsesquioxane(POSS) [Si8O12(CH=CH2)2(CH3)6] was synthesized by the cohydrolysis and cocondensation of methyltrimethoxysilane and vinyltrimethoxysilane in ethanol solvent under acidic conditions.The structure of the product obtained was studied using Fourier transform infrared spectrum(FT-IR),nuclear magnetic resonance spectrum(1H-NMR and 29Si-NMR) and X-ray diffraction(XRD).The experimental results indicate that the product generates a cage structure,the molar ratio of methyls and vinyls attached on POSS is approximately 3:1,and the molecular possesses a morphology of crystallization.Furthermore,the optimal reaction conditions with the monomer concentration(0.35 mol/L),the catalyst concentration(0.4 mol/L),molar ratio of water and monomers(6∶1),and reaction time(40h) are obtained.The reaction under these conditions can provide the product with the highest yield.The XRD results indicate that the product obtained has good crystallinity and the structure is high symmetry.
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