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A novel and efficient α‐MnO2‐N/C@active carbon (AC) catalyst was proposed and synthesized through a surface modification method based on imprinting process. Uniformly dispersed α‐MnO2 and N/C sites were constructed simultaneously and the competitive adsorption of metal precursors with nonmetal precursors was avoided. Conformational relationship of α‐MnO2‐N/C@AC revealed that α‐MnO2 and graphite N were the main active sites, cleverly forming synergistic catalytic effect, which results in a good degradation effect for two actual printing and dyeing wastewater. The removal rate of chemical oxygen demand (COD) could reach 78% and 58% within 60 min, respectively, and it maintained stable after 20 repetitions without leaching of metal ions. Mechanistic investigation demonstrated that N/C sites rapidly adsorbed ozone to generate ·O2− and synergistically catalyzed with adjacent α‐MnO2 sites to further produce ·OH, significantly facilitating the generation of ·OH. This work provides a promising strategy to synthesize novel and efficient catalysts for ozone catalytic oxidation process.

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