有机化学 ›› 2007, Vol. 27 ›› Issue (03): 424-427. 上一篇    下一篇

研究简报

双环笼状取代倍半硅氧烷的合成与表征

张利利,刘安华*,曾幸荣   

  1. (华南理工大学材料科学与工程学院 广州 510640)
  • 收稿日期:2006-06-12 修回日期:2006-09-01 发布日期:2007-02-13
  • 通讯作者: 刘安华

Synthesis of Caged Bicyclic Phosphorous-Functionalized Silsesquioxane

ZHANG Li-Li,LIU An-Hua*,ZENG Xing-Rong   

  1. (College of Materials Science and Engineering, South China University of Technology, Guangzhou 510640)
  • Received:2006-06-12 Revised:2006-09-01 Published:2007-02-13
  • Contact: LIU An-Hua

以双环笼状含磷四配位硅为前驱体, 四甲基氢氧化铵为催化剂反应得到具有高度对称结构的双环笼状磷酸酯取代倍半硅氧烷, 通过红外光谱, 29Si固体核磁共振谱, 质谱和X衍射光谱等手段确定了产物的结构和晶型. 热分析结果表明, 添加5%集磷硅为一体的倍半硅氧烷, 能使环氧树脂的分解温度提高45 ℃, 700 ℃时成炭量达到12.2%.

关键词: 磷硅协同效应, 环氧树脂, 双环笼状四配位硅, 双环笼状倍半硅氧烷

A novel type of caged bicyclic phosphorous functionalized silsesquioxane was synthesized from caged bicyclic phosphorous quadridentate silicon complex in the presence of tetramethylammonium hydroxide. The product was confirmed by FTIR, 29Si MAS NMR, MS and XRD spectra. Thermal analysis tests indicated that as a result of the synergistic effect between phosphorus and silicon, the initial temperature of thermal decomposition of epoxy resin was increased by 45 ℃, and the residual ratio reached to 12.2% at 700 ℃ by adding 5% the synthesized compound.

Key words: phosphorus/silicon synergistic effect, epoxy resin, phosphorous-functionalized silsesquioxane, caged bicyclic phosphorous quadridentate silicon complex