| Summary: | Catalytic combustion is an efficient and economic technology for eliminating volatile organic compounds (VOCs) in industrial environments. This study evaluated the synergistic catalytic properties of bimetallic oxides, viz., CoM/γ-Al<sub>2</sub>O<sub>3</sub> (M = Cu, Fe, or Ni), for improving the combustion efficiency of toluene. The CoM/γ-Al<sub>2</sub>O<sub>3</sub> catalysts were prepared by an impregnation method and characterized by using advanced techniques. Among the bimetallic catalysts, CoCu/γ-Al<sub>2</sub>O<sub>3</sub> exhibited the best performance. The findings revealed that owing to the strong synergistic interaction between Cu, Co, and the γ-Al<sub>2</sub>O<sub>3</sub> support, the active species in the CoCu/γ-Al<sub>2</sub>O<sub>3</sub> catalyst were effectively stabilized, and they significantly enhanced the redox performance and acidity of the catalyst, demonstrating superior catalytic activity and sulfur resistance. Conversely, the CoFe/γ-Al<sub>2</sub>O<sub>3</sub> catalyst performed poorly, exhibiting a significant decline in its activity owing to sulfur poisoning. The insights from this study provide theoretical support for designing efficient, sulfur-resistant catalysts that are crucial to reducing industrial VOC emissions.
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