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Improving the efficiency and stability of heterogeneous catalysts is essential for effectively utilizing peroxymonosulfate activation in industrial wastewater treatment. Perovskite ABO3catalysts with high structural flexibility have gained considerable attention in the peroxymonosulfate activation for the removal of hazardous organic compounds from wastewater. However, there is still considerable potential for catalytic enhancement due to the ease of tailoring its composition and structure. Herein, we introduce a scalable method to synthesize LaCo0.2Mn0.8O3with the aim of improving the catalytic performance. Interestingly, LaCo0.2Mn0.8O3with abundant oxygen vacancies and improved dispersion stability exhibited enhanced catalytic degradation of carbamazepine compared to the LaMnO3and LaCoO3catalysts in the peroxymonosulfate activation system. The partial substitution of manganese by cobalt in LaMnO3leading to the LaCo0.2Mn0.8O3+peroxymonosulfate system maintains a relatively high performance over repeated usage. Furthermore, the LaCo0.2Mn0.8O3catalyst exhibited excellent catalytic performance and stability across a broad pH range (3–9). Electron paramagnetic resonance and radical quenching experiment tests demonstrated singlet oxygen (1O2) as the primary active species for carbamazepine degradation in the LaCo0.2Mn0.8O3+ peroxymonosulfate system, while free radicals, such as sulfate radicals (⁠SO4•–), hydroxyl radicals (•OH), and superoxide radicals (O2•–), played a minor role in the carbamazepine removal. Taken together, this research provides significant insight into the effect of B-site substitution on the catalytic performance of perovskite catalysts.