Synthesis of incompletely caged silsesquioxane (T7-POSS) compounds via a versatile three-step approach

Miaofen Ye, Yiwei Wu, Wenchao Zhang, Rongjie Yang*

*Corresponding author for this work

Research output: Contribution to journalArticlepeer-review

27 Citations (Scopus)

Abstract

Abstract: Three kinds of incompletely condensed polyhedral oligomeric silsesquioxanes (T7-POSS) with three Si–OH groups: (i-C4H9)7Si7O9(OH)3, (i-C8H17)7Si7O9(OH)3 and (C6H5)7Si7O9(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·H2O as catalyst. The structures of the three T7-POSS were characterized by FTIR, 1H NMR, 13C NMR, 29Si NMR, MALDI-TOF MS and XRD. The accurate incompletely caged structure of the three T7-POSS indicated that the built-up three-step approach is a versatile and effective way to synthesize T7-POSS with high yield. The best reaction conditions to synthesize the isobutyl-T7, isooctyl-T7 and phenyl-T7 POSS have been suggested, involving acetone and a co-solvent, the molar ratio of the RSi(OEt)3: LiOH·H2O: H2O and the reaction temperature. The thermal stability of the three T7-POSS were characterized by TGA, showing different degradation behaviors. The thermal stability of phenyl-T7 POSS was the highest among the three T7-POSS.

Original languageEnglish
Pages (from-to)4277-4294
Number of pages18
JournalResearch on Chemical Intermediates
Volume44
Issue number7
DOIs
Publication statusPublished - 1 Jul 2018

Keywords

  • Incompletely caged silsesquioxane
  • POSS
  • Polyhedral oligomeric silsesquioxanes
  • T-POSS
  • Triethoxysilane

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