TY - JOUR
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
N1 - Publisher Copyright:
© 2018, Springer Science+Business Media B.V., part of Springer Nature.
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 - http://www.scopus.com/inward/record.url?scp=85043687906&partnerID=8YFLogxK
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 -