A heterogeneous catalyst was prepared by anchoring spinel cobalt ferrite nanoparticles on porous activated carbon (SCF@AC). The catalyst was tested to activate hydrogen peroxide (HP) in the Fenton degradation of metronidazole (MTZ). SCF nanoparticles were produced through the co-precipitation of iron and cobalt metal salts in an alkaline condition. Elemental mapping, physico-chemical, morphological, structural, and magnetic properties of the as-fabricated catalyst were analyzed utilizing EDX mapping, FESEM-EDS, TEM, BET, XRD, and VSM techniques. The porous structure of AC enhanced the catalytic activity of SCF by a significant decrease in the agglomeration of SCF nanoparticles. The effectiveness of SCF@AC in Fenton degradation improved substantially when UV light and ultrasound (US) irradiations were induced, most likely due to the strong synergistic effect between the catalyst and these irradiation sources. The photo-Fenton system was more efficient than the Fenton, sono-, and sono-photo-Fenton processes eliminating both MTZ and TOC. It was found that AC not only dispersed SCF nanoparticles and improved the stability of the catalyst, but also provided a high adsorption capacity of MTZ, resulting in a faster degradation. After 60 min of the photo-Fenton reaction, the elimination efficiencies of MTZ (30 mg L−1) and TOC were 97 and 42.1% under optimum operational conditions (pH = 3.0, HP = 4.0 mM, SCF@AC = 0.3 g L−1, and UV = 6 W). SCF@AC showed excellent stability with low leaching of metal ions during the reaction. Radical and non-radical (O2•–, HO•, and 1O2 species), alongside adsorption and photocatalysis mechanisms, were responsible for MTZ decontamination over the SCF@AC/HP/UV system. A comprehensive study on the HP activation mechanism and MTZ degradation pathway was obtained through scavenging tests. The findings demonstrate that SCF@AC is an effective, reusable, and environmentally sustainable catalyst for advanced oxidation processes that can effectively remove organic pollutants from wastewater. This study offers valuable insights into the feasibility of employing SCF@AC catalysts in Fenton-based processes for the degradation of MTZ.
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