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Mesoporous Co-Al₂O₃ catalysts were prepared by one-pot synthesis and, for the first time, used in the partial oxidation of methane to synthesis gas. Compared with the catalysts prepared by impregnation methods, the catalysts prepared by one-pot synthesis showed superior catalytic performance for this reaction. The results showed that mesoporous Co-Al₂O₃ catalysts have high surface areas, large pore volumes, and an ordered hexagonal mesostructure. In the catalysts, Co species are highly dispersed, resulting in high dispersion of the metal after reduction. A confinement effect, provided by the mesopores, on metal nanoparticles could effectively enhance resistance to metal sintering.