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

Miaofen Ye; Yiwei Wu; Wenchao Zhang; Rongjie Yang

doi:10.1007/s11164-018-3368-2

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

School of Material Science and Engineering

Beijing Institute of Technology

Research output: Contribution to journal › Article › peer-review

32 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 language	English
Pages (from-to)	4277-4294
Number of pages	18
Journal	Research on Chemical Intermediates
Volume	44
Issue number	7
DOIs	https://doi.org/10.1007/s11164-018-3368-2
Publication status	Published - 1 Jul 2018

Keywords

Incompletely caged silsesquioxane
POSS
Polyhedral oligomeric silsesquioxanes
T-POSS
Triethoxysilane

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10.1007/s11164-018-3368-2

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

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.",

keywords = "Incompletely caged silsesquioxane, POSS, Polyhedral oligomeric silsesquioxanes, T-POSS, Triethoxysilane",

author = "Miaofen Ye and Yiwei Wu and Wenchao Zhang and Rongjie Yang",

note = "Publisher Copyright: {\textcopyright} 2018, Springer Science+Business Media B.V., part of Springer Nature.",

year = "2018",

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T1 - Synthesis of incompletely caged silsesquioxane (T7-POSS) compounds via a versatile three-step approach

AU - Ye, Miaofen

AU - Wu, Yiwei

AU - Zhang, Wenchao

AU - Yang, Rongjie

PY - 2018/7/1

Y1 - 2018/7/1

N2 - 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.

AB - 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.

KW - Incompletely caged silsesquioxane

KW - POSS

KW - Polyhedral oligomeric silsesquioxanes

KW - T-POSS

KW - Triethoxysilane

UR - https://www.scopus.com/pages/publications/85043687906

U2 - 10.1007/s11164-018-3368-2

DO - 10.1007/s11164-018-3368-2

M3 - Article

AN - SCOPUS:85043687906

SN - 0922-6168

VL - 44

SP - 4277

EP - 4294

JO - Research on Chemical Intermediates

JF - Research on Chemical Intermediates

IS - 7

ER -

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

Abstract

Keywords

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