Perovskite-type catalysts show a good prospect in the field of pollutant degradation. Bimetallic doping can regulate the structure of perovskite and improve its performance. A series of Ni-substituted LaCoxNi1-xO3 (x = 1, 0.75, 0.5, 0.25, 0) catalysts were prepared to degrade reactive brilliant red X-3B by activating H2O2. SEM and XRD analyses revealed that Ni was successfully incorporated into the LaCoO3 material, and the B-site substituted material exhibited an increased number of active sites. The experimental results showed that the Ni substitution at the B-site could effectively enhance the Fenton-like degradation performance of LaCoO3. B-site doping can accelerate charge transfer, thereby enhancing catalytic efficiency. LaCo0.5Ni0.5O3 exhibited an optimal degradation efficiency of 76.5%, which was 1.26 and 1.48 times higher than those of LaCoO3 and LaNiO3, respectively. Free radical capture and electron paramagnetic experiments showed that LaCoxNi1-xO3 could activate H2O2 to produce ·OH, ·O2- and other free radicals. This work may offer a new insight for enhancing the Fenton-like degradation performance of LaCoO3 by another metal substitution at B-site.

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