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Fe0/Fe3C/Fe3O4 nanoparticles wrapped in graphite shells (CC-Fe/C) were synthesized via pyrolyzing MIL-88B(Fe) at 700, 800, and 900 °C. CC-Fe/C-800 prepared at 800 °C exhibited the best performance for activating peroxymonosulfate with complete removal of bisphenol A at 10 mg/L in 20 min, attributing to the synergistic effect of multiple active sites (Fe0, Fe3C, and Fe3O4) on its surface. Mechanism study suggested that SO4∙−, ∙OH, 1O2, and O2−∙ were involved in the degradation. Fe0 cores could act as cocatalysts to promote the regeneration of Fe2+, enhancing the catalytic activity. Finally, CC-Fe/C-800 showed good reusability and practicability.