<p>In this study, FeOOH/BiOI composite materials were successfully synthesized using simple precipitation method. The samples were systematically characterized using various techniques, including XRD, SEM, EDS, XPS, and UV–Vis–DRS. A visible light-assisted FeOOH/BiOI activation system, mediated by different oxidants (Peroxydisulfate, PDS and hydrogen peroxide, H₂O₂), was constructed to achieve efficient degradation of antibiotic wastewater. It was discovered that the FeOOH/BiOI photocatalyst activated by PDS and H₂O₂ significantly improved the degradation efficiency of norfloxacin (NOR). The effects of composition ratios, pH, and dosage on NOR removal were also investigated. The degradation efficiency of 0.5-FeOOH/BiOI composites for NOR was 57.3% in PDS system and 66.9% in H₂O₂ system. Importantly, a working mechanism for the visible light-assisted FeOOH/BiOI activation system with PDS and H₂O₂ was proposed. The synthesis of the FeOOH/BiOI composite material effectively promoted the separation of photogenerated electrons and holes, generating more active substances in the system. These active substances attacked the NOR molecules adsorbed on the catalyst surface or diffused into the solution to degrade the NOR molecules in the solution, ultimately achieving efficient degradation of NOR. This finding holds significant implications for guiding the application of visible light-assisted advanced oxidation technology in the field of antibiotic wastewater treatment.</p>