Photocatalytic degradation is a sustainable technique for reducing the environmental hazards created by the overuse of antibiotics in the food and pharmaceutical industries. Herein, a layer of MoS2/g-C3N4 nanocomposite is introduced to zirconium oxide (ZrO2) nanoparticles to form a “particle-embedded-layered” structure. Thus, a narrow band gap (2.8 eV) starts developing, deliberated as a core photodegradation component. Under optimization, a high photocatalytic activity of 20 mg/L TC at pH 3 with ZrO2@MoS2/g-C3N4 nanocomposite was achieved with 94.8% photocatalytic degradation in 90 min. A photocatalytic degradation rate constant of 0.0230 min–1 is determined, which is 2.3 times greater than the rate constant for bare ZrO2 NPs. The superior photocatalytic activity of ZrO2@MoS2/g-C3N4 is due to the dual charge-transfer channel between the MoS2/g-C3N4 and ZrO2 nanoparticles, which promotes the formation of photogenerated e–/h+ pairs. Charge recombination produces many free electron–hole pairs, which aid photocatalyst reactions by producing superoxide and hydroxyl radicals via electron–hole pair generation. The possible mechanistic routes for TC were investigated in-depth, as pointed out by the liquid chromatography–mass spectrometry (LC–MS) investigation. Overall, this work shows that photocatalysis is a feasible sorbent approach for environmental antibiotic wastewater treatment.

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