Allyl methacrylate, AMA was polymerized in CCl4 solution by α,α′‐azoisobutyronitrile at 50°C. The thermal degradation mechanism of PAMA was characterized by MS, TGA‐FT‐IR and FT‐IR‐ATR methods. The mass spectrum and TGA thermogram showed two stage degradation. The first stage of degradation was mostly linkage type degradation for the fragmentation of pendant allyl groups at 225–350°C. In the second stage, at 395–515°C, the degradation is random scission and depolymerization types. This was also supported by direct thermal pyrolysis of polymer under vacuum.
