This study introduces a novel metallic-MOF composite, MIL-100@ZIF-67, anchored on MXene nanosheets, designated as MIL-100@ZIF-67@MXene, for the enhanced degradation of carbamazepine (CBZ) and activation of peroxymonosulfate (PMS). The efficacy of the composite in CBZ degradation and the underlying reaction parameters and mechanisms were thoroughly investigated. Remarkably, the MIL-100@ZIF-67@MXene/PMS system achieved a 95% reduction of CBZ within 30 minutes under neutral pH conditions. Scavenger experiments and electron paramagnetic resonance (EPR) analysis confirmed that a combination of radicals (SO4•−, •OH) and non-radicals (1O2, O2•−, and high-valent metal-oxo species) contributed to the degradation process, with singlet oxygen (1O2) identified as the predominant active species. Additionally, the composite exhibited superior performance in the hydrogen evolution reaction (HER), generating 130 µmol L-1 mg-1 min-1 of dissolved hydrogen under alkaline conditions (pH 10) and a potential of -1.2 V. This research demonstrates the potential of bimetallic MOFs combined with carbon materials for effective antibiotic removal and PMS activation. Furthermore, it highlights their promising capability in HER, offering a multifaceted approach to addressing environmental pollution and promoting energy sustainability.

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