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We further developed previous work on MXene materials prepared using molten salt methodology. We substituted single, with mixed salts, and reduced the melting point from >724 °C to <360 °C. Cobalt (Co) compounds were simultaneously etched and doped while the MXene material was created using various techniques in which Co compounds occur as Co3O4. The synthesized Co3O4/MXene compound was used as a peroxymonosulfate (PMS) activator that would generate free radicals to degrade antibiotic ornidazole (ONZ). Under optimal conditions, almost 100% of ONZ (30 mg/L) was degraded within 10 min. The Co3O4/MXene + PMS system efficiently degraded ONZ in natural water bodies, and had a broad pH adaptation range (4–11), and strong anion anti-interference. We investigated how the four active substances were generated using radical quenching and electron paramagnetic resonance (EPR) spectroscopy. We identified 12 ONZ intermediates by liquid chromatography-mass spectrometry and propose a plausible degradative mechanism.