The increasingly severe antibiotic pollution has become one of the most critical issues. In this study, a zinc peroxide/peroxymonosulfate (ZnO₂/PMS) double-oxidation system was developed for tetracycline (TC) degradation. A small amount of ZnO₂ (10 mg) and PMS (30 mg) could effectively degrade 82.8% of TC (100 mL, 50 mg/L), and the degradation process could be well described by the pseudo-second-order kinetic model. Meanwhile, the ZnO₂/PMS double-oxidation system showed high adaptability in terms of reaction temperature (2–40 °C), initial pH value (4–12), common inorganic anions (Cl⁻, NO₃⁻, SO₄²⁻ and HCO₃⁻), natural water source and organic pollutant type. The quenching experiment and electron paramagnetic resonance (EPR) characterization results confirmed that the main reactive oxygen species (ROS) was singlet oxygen (¹O₂). Moreover, three possible pathways of TC degradation were deduced according to the analyses of intermediates. On the basis of comparative characterization and experiment results, a synergistic activation mechanism was further proposed for the ZnO₂/PMS double-oxidation system, accounting for the superior degradation performance. The released OH⁻ and H₂O₂ from ZnO₂ could activate PMS to produce major ¹O₂ and minor superoxide radicals (•O₂⁻), respectively.

Microwave-assisted processing has shown tremendous promise in accelerating chemical reactions and reducing energy consumption through targeted dielectric heating. This study develops MOF-derived Mn-Co and Ce-Co oxide catalysts for energy-efficient benzene oxidation via microwave catalysis. The MnCo spinel oxides (particularly MnCo11-400) exhibit superior microwave absorption and catalytic activity due to enhanced oxygen mobility and tailored dielectric properties. Microwave irradiation enables rapid benzene mineralization over the MnCo11-400 catalyst, achieving 78% conversion at 30 W and complete conversion at 50 W, demonstrating exceptional energy efficiency at low power inputs. Microwaves significantly lower the reaction temperature compared to conventional thermal catalysis (ΔT = 100–250 °C). Stability tests confirm robustness over repeated power cycling (80% conversion retained after 3 × 1 h on/off cycles). Furthermore, an adsorption–microwave oxidation synergistic strategy is demonstrated: pre-adsorbed low-concentration benzene (1.15 mmol) at ambient temperature undergoes complete mineralization within 20 min under 30 W microwave irradiation. The intermittent microwave operation achieves equivalent benzene removal to continuous thermal processing while significantly reducing energy demand. This work establishes MOF-derived spinel oxides as high-performance microwave catalysts for low-temperature VOC abatement.