AbstractThe composite Fenton catalyst was prepared by attaching MgCo2O4 to the surface of g‐C3N4 using a one‐pot method after preparing MgCo2O4 through co‐precipitation. The microstructure of the composites was analyzed using X‐ray diffraction (XRD) and other characterization methods. The catalytic activity of the composites towards tetracycline (TC) was studied, and a possible catalytic mechanism was proposed. The experimental results indicate that the degradation of TC by MgCo2O4@g‐C3N4 reached almost 99.0 % within 30 min in the presence of PMS and visible light. The combination of MgCo2O4 and g‐C3N4 improved the absorption of visible light, and the energy level‐matched heterojunction facilitated the separation of photogenerated electrons and holes, accelerating the redox cycle of ≡Co3+/≡Co2+. The free radical quenching experiment confirmed that the main active substances were free radical ⋅O2− and 1O2. The one‐step synthesis of composite catalysts exhibits high catalytic performance and good stability, offering a potential solution for the efficient treatment of tetracycline wastewater.