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Epoxy/silsesquioxane organic–inorganic hybrids: Sol–gel synthesis of inorganic precursors containing amino and phenyl groups
Author(s) -
Farias M.A.,
Coelho L.A.F.,
Pezzin S.H.
Publication year - 2012
Publication title -
polymer engineering and science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.503
H-Index - 111
eISSN - 1548-2634
pISSN - 0032-3888
DOI - 10.1002/pen.22044
Subject(s) - silsesquioxane , diglycidyl ether , thermogravimetric analysis , materials science , epoxy , thermal stability , hybrid material , polymer chemistry , catalysis , sol gel , glass transition , bisphenol a , ether , chemical engineering , polymer , organic chemistry , chemistry , composite material , nanotechnology , engineering
The synthesis of silsesquioxane oligomers containing amino and phenyl groups by sol–gel process and the formation of an organic–inorganic hybrid, by the reaction of amino groups of the silsesquioxane precursor with epoxy rings of diglycidyl ether of bisphenol A, have been investigated. Acid catalysis proved to be more efficient than basic catalysis for the condensation reaction between 3‐aminopropyltriethoxysilane (APES) and phenyltriethoxysilane (PETS) in ethanol. Liquid state 29 Si nuclear magnetic resonance ( 29 Si NMR) analysis indicated that T 3 structures are the major phase forming the network structure. Infrared spectroscopy analyses confirmed the formation of the epoxy/silsesquioxane hybrid and showed that a high degree of cure was achieved. A distinct behavior of the glass transition temperature ( T g ) between the hybrids cured at different time intervals after the chemical modification was observed, and the most significant value was an increase of 13°C in T g obtained with the hybrid produced with silsesquioxane oligomers synthesized by sol–gel for 18 h. From thermogravimetric analyses (TGAs), it was observed an increase on the residual masses for the hybrids and a decrease in their degradation rates, suggesting an improvement of thermal stability. These results indicate the formation of a new organic–inorganic hybrid material with potential applications for high performance coatings and structural components. POLYM. ENG. SCI., 2012. © 2011 Society of Plastics Engineers