Synthesis of incompletely caged silsesquioxane (T7-POSS) compounds via a versatile three-step approach
Synthesis of incompletely caged silsesquioxane (T7-POSS) compounds via a versatile three-step approach
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通过多功能三步法合成不完全笼状倍半硅氧烷 (T-7-POSS) 化合物
DOI：
10.1007/s11164-018-3368-2
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发表时间：
2018-07-01
影响因子：
3.3
通讯作者：
Yang, Rongjie
中科院分区：
文献类型：
--
作者：
Ye, Miaofen;Wu, Yiwei;Yang, Rongjie
以i-C4H9Si(OEt)(3)、i-C8H17Si(OEt)(3)和C6H5Si(OEt)(3)为原料，以LiOH中心点H2O为催化剂，采用水解、缩合、中和的三步法，分别制备了3种不完全缩合的硅氧烷（T-7-POSS），具有3个Si-OH基团：（i-C4H9）(7)Si7O9(OH)(3)、（i-C8H17）(7)Si7O9(OH)(3)和（C6H5）(7)Si7O9(OH)(3)。采用FTIR、H-1 NMR、C-13 NMR、Si-29 NMR、MALDI-TOF MS和XRD对三种T-7-POSS的结构进行了表征。三种T-7-POSS的非完全笼化结构的精确分析表明，构建三步法是一种高效、通用的合成T-7-POSS的方法。提出了合成异丁基- t -7、异辛基- t -7和苯基- t -7 POSS的最佳反应条件，包括丙酮和助溶剂、RSi(OEt)(3): LiOH中心点H2O: H2O的摩尔比和反应温度。通过热重分析对3种T-7-POSS的热稳定性进行了表征，显示出不同的降解行为。在三种t -7 POSS中，苯基t -7 POSS的热稳定性最高。
Three kinds of incompletely condensed polyhedral oligomeric silsesquioxanes (T-7-POSS) with three Si-OH groups: (i-C4H9)(7)Si7O9(OH)(3), (i-C8H17)(7)Si7O9(OH)(3) and (C6H5)(7)Si7O9(OH)(3) were prepared by a versatile three-step approach (hydrolysis, condensation, and neutralization) from i-C4H9Si(OEt)(3), i-C8H17Si(OEt)(3), and C6H5Si(OEt)(3), respectively, with the LiOH center dot H2O as catalyst. The structures of the three T-7-POSS were characterized by FTIR, H-1 NMR, C-13 NMR, Si-29 NMR, MALDI-TOF MS and XRD. The accurate incompletely caged structure of the three T-7-POSS indicated that the built-up three-step approach is a versatile and effective way to synthesize T-7-POSS with high yield. The best reaction conditions to synthesize the isobutyl-T-7, isooctyl-T-7 and phenyl-T-7 POSS have been suggested, involving acetone and a co-solvent, the molar ratio of the RSi(OEt)(3): LiOH center dot H2O: H2O and the reaction temperature. The thermal stability of the three T-7-POSS were characterized by TGA, showing different degradation behaviors. The thermal stability of phenyl-T-7 POSS was the highest among the three T-7-POSS.[GRAPHICS].