ABSTRACT Constructing sulfur vacancies (S v ) on monolayer MXene to modulate the valence states of metal sites, elucidating the underlying mechanisms responsible for the multiphase Fenton‐like catalytic process, is of critical importance. Motivated by this inspiration, we pathbreakingly applied elemental regulation and defect engineering on monolayer MXene, with CoS collaboration, aiming to construct S v to modulate the valence of Co sites in CoS and thereby enhance the catalytic performance toward PMS activation. Monolayer MXene incorporation effectively suppressed CoS aggregation, while sulfidation followed by calcination at 300°C created S v on the MXene surface, denoted as S v ‐CM. This regulation significantly boosted PMS activation and promoted the formation of highly reactive high‐valent metal‐oxo species (HVMS). Achieving complete bisphenol A (BPA) degradation within 5 min, the S v ‐CM/PMS system outperforms most previously reported heterogeneous catalyst/PMS systems. This highly efficient catalytic oxidation process converts BPA into low‐toxicity products via HVMS. Furthermore, the S v ‐CM/PMS system demonstrated excellent durability, maintaining 100% BPA removal over 72 h of continuous operation. This study provides valuable insights into the rational design of S v ‐CM and paves the way for its practical implementation for the Fenton‐like catalytic process and water purification.
He et al. (Sat,) studied this question.