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Peroxymonosulfate (PMS) activation has gained increasing attention for its water remediation. In this work, carbon nanotube-supported FeCo₂O₄ nanoparticles (FeCo₂O₄/CNT) were prepared and showed tremendous potential as a catalyst for PMS activation. The synergistic effect between FeCo₂O₄ and CNT in FeCo₂O₄/CNT promotes its better catalytic performance than individual CNT or FeCo₂O₄. The synthesized FeCo₂O₄/CNT could reach 100% phenol removal with a <i>k</i> value of 0.30 min⁻¹ within 15 min ([PMS] = 0.3 g L⁻¹, [FeCo₂O₄/CNT] = 0.3 g L⁻¹). FeCo₂O₄/CNT can adapt well to a wide pH range (4–9) and a complex water component (with inorganic ions or organic matter). Moreover, the catalytic mechanism investigation suggested that both radical and non-radical pathways are accountable for the efficient removal of phenol.