双环笼状四配位硅的合成及其结构表征

Synthesis and Characterization of Caged Bicyclic Phosphorous Quadridentate Silicon Complex

研究了以SiO2为原料低温合成高反应活性的五配位硅酸酯,并与1-氧代-1-磷杂-2,6,7-三氧杂双环[2.2.2]-4-氯甲基辛烷反应合成出具有对称结构的双环笼状四配位硅,通过红外光谱、13C和29Si固体核磁共振、质谱等测试手段确定了其结构.热分析结果表明,双环笼状四配位硅在700℃的失重仅为19.98%,且炭层呈密实片层状,说明目标产物具有优异的热稳定性和成炭性质.

A novel caged bicyclic phosphorous quadridentate silicon complex was synthesized by reaction of l-oxo-l-phospha-4-chloromethyl-2,6,7-trioxabicyclo[2.2.2]octane with the pentacoordinate silicon complex, which was synthesized directly from SiO2 by non-carbothermal reduction. Structure of the synthesized substance was confirmed by FTIR, MS, 13C and 29Si MAS NMR spectra, while thermal analysis tests indicated that the target compound possessed exceptional thermal stability.