In this investigation, polymethyl methacrylate (PMMA) was mixed with cyclic olefin copolymer (COC) because of its hardness, strength, and transparency properties. The results of thermal analysis through TGA and DTG showed that the thermal properties of the alloy are improved using 40% cyclic olefin copolymer. Kinetics of thermal degradation (pyrolysis) of polymers have been studied and analyzed and thermal pyrolysis of polymethyl methacrylate and cyclic olefin copolymer thermoplastic polymer was conducted. The computation of kinetic analysis is measured along with the different methods used to study the kinetics. The activation energy (E) of degradation of studied materials was estimated using Ozawa Flynn and Wall (OFW), Starink and Kissinger’s methods, and evaluation of three kinetic parameters taken appropriate kinetic model in terms of percent change for both types of polymers have been proposed, and finally, simulated curves were compared with the experimental curves. Both mechanisms of degradation for COC and PMMA under nitrogen atmosphere will reflect intramolecular transfer and random scission of the main chain.