Non-hydrolytic sol-gel synthesis of epoxysilane-based inorganic-organic hybrid resins

A silica-based inorganic-organic hybrid resins (IOHR) were synthesized by non-hydrolytic sol-gel process from 3-glycidoxypropyltrimethoxyrsi lane (GLYMO) and diphenylsilanediol (DPSD) at a fixed amount of (20 mol%) phenyltrimethoxysilane using barium hydroxide as a catalyst. The confirmation of condensation reaction in the IOHR was done by liquid state Si-29 NMR (Nuclear Magnetic Resonance) spectroscopy, measurement of viscosity as well as weight average molecular weight (W-m) of the IOHR. The W-m of the IOHR was varied from 1091 to 2151, depending upon the DPSD content. Fourier transform infrared (FTIR) spectroscopic measurements were performed to investigate the details of vibrational absorption bands in the IOHR. It was seen that up to 50 mol% of DPSD there were no absorption peaks in the region of 3000-3600 cm(-1) responsible for O-H groups and it reappeared at 60 mol% of DPSD due to some unreacted OH groups present in the resin. The IOHR at all the compositions was oily transparent liquid, miscible with various organic solvents like toluene, cyclohexanone, chloroform, tehrahydrofuran (THF), etc., and also commercial epoxy resins but immiscible with water. The color of the IOHR was pale yellow, which lightened with increasing DPSD content. The IOHR having 40-50 mol% ofDP5D were storable. The refractive index at 632.8 nm of the resin films varied from 1.556 to 1.588, depending upon the resin composition. Physico-chemical properties such as the thermal stability, visible transparency, etc. after curing were investigated as a function of the chemical composition. (C) 2008 Elsevier B.V. All rights reserved.