Synthesis of phosphorus‐containing polyhedral oligomeric silsesquioxanes via hydrolytic condensation of a modified silane

Synthesis of phosphorus‐containing polyhedral oligomeric silsesquioxanes via hydrolytic condensation of a modified silane
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DOI:
10.1002/app.34471
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发表时间:
2011-12
影响因子:
3
通讯作者:
Wenchao Zhang;Rongjie Yang
Wenchao Zhang;Rongjie Yang
中科院分区:
化学3区
文献类型:
--
作者:
Wenchao Zhang;Rongjie Yang

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报道了一种新型含磷多面体低聚硅氧烷(DOPO-POSS)的高效水解缩聚合成方法。以9,10-二氢-9-氧-10-磷菲-10-氧化物(DOPO)与乙烯基三乙氧基硅烷(VTES)加成反应合成含磷三乙氧基硅烷(DOPO - VTES)。用盐酸催化剂在甲醇中水解缩合。采用1H、13C、29Si-NMR、MALDI-TOF MS、XRD、DSC和FTIR对新型含磷POSS进行了表征。这些结果表明DOPO-POSS是T8、T9(OH)的非晶态混合物,DOPO-POSS的TGA曲线表明该笼状化合物具有较高的热稳定性。©2011 Wiley期刊公司高分子学报,2011
A simple route to synthesize a new type of phosphorus-containing polyhedral oligomeric silsesquioxanes (DOPO–POSS) in high yield, by the hydrolytic condensation of a modified silane, is reported. The starting material was a phosphorus-containing triethoxy silane (DOPO–VTES), which was synthesized by addition reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and vinyl triethoxy silane (VTES). This product was subjected to hydrolytic condensation using an HCl catalyst in methanol. The new types of phosphorus-containing POSS were obtained and characterized using 1H, 13C, 29Si-NMR, MALDI-TOF MS, XRD, DSC, and FTIR. All of these results suggested that the DOPO–POSS were amorphous mixtures of T8, T9(OH), and TGA curve of DOPO–POSS shows that the cage-like compound has high thermal stability. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011