Synthesis of Phosphorus-Containing Polyhedral Oligomeric Silsesquioxanes via Hydrolytic Condensation of a Modified Silane

A simple route to synthesize a new type of phosphorus-containing polyhedral oligomeric silsesquioxanes (DOPO-POSS) in high yield, by the hydrolytic condensation of a modified silane, is reported. The starting material was a phosphorus-containing triethoxy silane (DOPO-VTES), which was synthesized by addition reaction between 9,10-dihydro-9-oxa-10-phosphaphenanthrene10- oxide (DOPO) and vinyl triethoxy silane (VTES). This product was subjected to hydrolytic condensation using an HCl catalyst in methanol. The new types of phosphorus-containing POSS were obtained and characterized using H-1, C-13, Si-29-NMR, MALDI-TOF MS, XRD, DSC, and FTIR. All of these results suggested that the DOPO-POSS were amorphous mixtures of T-8, T-9(OH), and TGA curve of DOPO-POSS shows that the cage-like compound has high thermal stability. (C) 2011 Wiley Periodicals, Inc. J Appl Polym Sci 122: 3383-3389, 2011