a-a'azobisisobutyronitrile initiated radical polymerization of MMA in presence of naphthaleneiodine charge transfer complex in DMSO at 65 ± 0.10C for 2 hours under a nitrogen blanket, follows ideal kinetics. Dilatometric technique is used to prepare the polymer. The overall activation energy and average value of kp 2/kt are 32.37 kJ and 1.14 x 10–2 l mol–1s–1 respectively. The polymer has a viscosity -average molecular weight between 23741-65285.The FTIR spectrum of the polymer shows the presence of band at 3010 cm-1 and 1735 cm-1 for the phenyl group of the complex and ester stretchings of MMA respectively. 1H-NMR spectrum shows the peak at 7.8 d ppm and 3.7 dppm due to phenyl protons and ester group of MMA respectively. The thermal properties of the polymer were investigated by TGA technique. The TGA spectrum shows the stability of polymer upto 2500C.