In this study, 2-methacryloxyethyl phenyl phosphate (MEPP), a phosphorus-containing flame retardant, was synthesised via the esterification of phenyl dichlorophosphate (PDCP) with 2-hydroxyethyl ethylene methacrylate (HEMA), followed by hydrolysis. A two-stage bulk polymerisation process prepared MEPP/methyl methacrylate (MEPP/MMA) copolymers containing various amounts of MEPP. The condensed-phase and volatized products produced at various temperatures during the thermal degradation of MEPP/MMA copolymer were monitored by Fourier transform infrared (FT-IR) spectroscopy and thermogravimetric analysis with Fourier transform infrared spectroscopy (TGA/FT-IR). Finally, we propose the possible mechanisms for the thermal degradation of MEPP/MMA copolymer according to the analytical results of the condensed-phase and volatilized products. Crown Copyright (C) 2009 Published by Elsevier Ltd. All rights reserved.