Epoxy/silsesquioxane organic-inorganic hybrids: Sol-gel synthesis of inorganic precursors containing amino and phenyl groups

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 catalysi...

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Bibliographic Details
Published in:Polymer engineering and science 2012-01, Vol.52 (1), p.52-61
Main Authors: Farias, M.A., Coelho, L.A.F., Pezzin, S.H.
Format: Article
Language:English
Subjects:
Applied sciences
Catalysis
Chemical compounds
Chemical properties
Chemical reactions
Chemical synthesis
Composition
Epoxy resins
Ethyl alcohol
Exact sciences and technology
Glass transition temperature
Inorganic and organomineral polymers
Mechanical properties
Methods
Oligomers
Phenyls
Physicochemistry of polymers
Polymer industry, paints, wood
Precursors
Preparation
Production processes
Properties and testing
Silicon compounds
Sol gel process
Synthesis
Technology of polymers
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Summary: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 29Si nuclear magnetic resonance (29Si NMR) analysis indicated that T3 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 (Tg) 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 Tg 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
ISSN:0032-3888
1548-2634
DOI:10.1002/pen.22044