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[Display omitted] • Anchoring cobalt on sandwich-like 2D MXene shows synergistic effect on PAA activation. • Highly efficient degradation of 2,4-DCP is observed at neutral condition. • Ti 3 C 2 T x MXene substrate accelerates recycling of ≡ Co(III)/≡ Co(II). • Acetylperoxyl radical is primarily responsible for contaminant degradation. • The Co@MXenes/PAA process was unaffected by water matrices. A novel Co@MXenes catalyst with unique structure was prepared through randomly anchoring cobalt on 2D sandwich-like MXenes to activate peracetic acid (PAA) for water decontamination. Compared to the conventional Co 3 O 4 nanomaterial, the Co@MXenes catalyst exhibits superior performance for PAA activation under neutral condition. In-depth investigation revealed that the Ti 3 C 2 T x MXene substrate triggered the ≡ Co(III)/≡ Co(II) cycle, which greatly enhanced the activation of PAA. The XPS and ICP techniques further demonstrated that Co@MXenes was highly stable with extremely low cobalt ion leaching and hence a superior reusability was obtained. Moreover, acetylperoxyl radical (CH 3 CO 3 ) was identified as the primary radical species responsible for organic micropollutants degradation, exhibiting high selectivity towards contaminants containing electron-rich groups. The novel technology exhibited a high tolerance of Cl− and good performance in real wastewater treatment. This work provides a promising effective catalyst for PAA activation and will facilitate PAA application in wastewater decontamination. [ABSTRACT FROM AUTHOR]