Polymethyl methacrylate/hydroxylated multi-walled carbon nanotubes (PMMA/MWCNT-OH) nanocomposites were prepared by solution blending by adding 1, 2, 3, and 4 wt-% MWCNT-OH. The thermal degradation mechanism and thermal life of PMMA/MWCNT-OH in nitrogen and oxygen atmospheres were investigated in detail. When MWCNT-OH content was 3 wt-%, the maximum thermogray-weight temperature (Tm) was 11.5°C and 61.4°C higher than that of PMMA in nitrogen and oxygen atmospheres. Three-dimensional diffusion reaction and level 1.5 chemical reaction in nitrogen atmosphere and one-dimensional diffusion reaction and level 1 chemical reaction chemical reaction in oxygen atmosphere by Achar method and Coats–Redfern method were the possible mechanisms of PMMA and PMMA/MWCNT-OH nanocomposites. When the weight loss rate of 30% was taken as the thermal life end point of the composites, the thermal life first increased and then decreased with the content of MWCNT-OH increased by Kissinger method and Dakin equation.
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