1,2,3,4-Tetraphenylcyclopentadiene triphenyl stibonium ylide initiated radical polymerization of n-butyl methacrylate (n-BMA) in dioxane at (60 +/- 0.2)degrees C for 90 min under nitrogen atmosphere has been carried out. The system follows nonideal kinetics, i.e., R-p alpha [ylide](0.2) [n- BMA](1.8). The value of k(p)(2)/k(t) and overall energy of activation have been computed as 0.133 x 10(-2) L mol(-1) s(-1), 33 kJ/mol, respectively. The FTIR spectrum shows a band at 1745 cm(-1) due to acrylate group of n-BMA. The H-1 NMR spectrum shows a peak of two magnetically equivalent protons of methylene group at 2.1 delta ppm. The DSC curve shows glass transition temperature (T-g) as 41 degrees C. The presence of six hyperfine lines in ESR spectrum indicates that the system follows free radical polymerization and the initiation is brought about by phenyl radical. (c) 2006 Wiley Periodicals, Inc.