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A series of Fe–rich palygorskite supported manganese oxide (X%Mn–Pal) catalysts were prepared by co-precipitation method and used as catalysts for toluene oxidation. The components and structure of the as-prepared catalysts were characterized by XRD, Raman, TEM, XPS, and in situ DRIFTS. The results showed that the 15%Mn–Pal catalyst exhibited the highest catalytic activity (T₉₀ = 227 °C) and excellent cycling stability for the oxidation of toluene compared with other catalysts. The characterization results indicated that remarkable activity of the 15%Mn–Pal catalyst for toluene oxidation should be ascribed to the abundant surface oxygen vacancies. In situ DRIFTS results elucidated that benzoate was the main intermediate, which can be further oxidized into H₂O and CO₂. The objectives of this study are to (i) investigate the synergistic effect between Fe and Mn for toluene oxidation, (ii) develop an efficient catalyst for toluene abatement with high activity and low–cost, and (iii) promote the application of natural Fe–rich palygorskite in the control of VOCs.