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Multigraphene was prepared via a one-pot pyrolysis method using polypropylene (PP) as the carbon source and diatomite (DM) as the catalyst. The obtained graphene had 4–6 layers and a D/G intensity ratio of 0.70 and a 2D/G intensity ratio of 0.72, indicating a high degree of graphitization. When the pyrolysis temperature was higher than 850 °C under argon, the graphene yield was greatly dependent on the DM content. The highest graphene yield of 25.86% was obtained by pyrolysis of PP with 30 wt.% DM at the temperature of 1000 °C. A catalytic effect of DM and infusible cross-linking structure formation were proposed to explain the possible mechanism of graphene growth during the pyrolysis of the DM/PP composites.