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In this work, the thermogravimetry–Fourier transform infrared spectroscopy (TG–FTIR) and gas chromatography–mass spectrometry (GC–MS) techniques are used to investigate the thermal degradation behavior of polypropylene (PP) with 20 wt.% diatomite (DM). The initial decomposition temperature of these blends was 17 °C lower than that of pristine PP, and more olefin degradation products were formed during the pyrolysis process under Ar atmosphere. These results could be attributed to the catalytic effects of DM on the degradation of PP and the changes of PP chain scission pathways around the particles (more β scission happened via the secondary radical transfer). These olefins could be caught by DM through the Si–O–C bond formed during the heat–treatment around 400~500 °C. The formation of the cross–linked structure could facilitate the growth of graphene during a high–temperature graphitization process.