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Abstract: Detemplation of zeolite MCM-56 was successfully realized by controlled oxidation of the template using H2O2 at 363 K. The resulting material (denoted as MCM-56(H2O2)) shows larger surface area (micropore and external), higher micropore volume, more Lewis acid and Brønsted acid sites in comparison with the sample detemplated by calcination (denoted as MCM-56(C)). Moreover, two Mo-containing catalysts of Mo/H-MCM-56(H2O2) and Mo/H-MCM-56(C) were prepared, and their catalytic properties for the reaction of methane aromatization were investigated. Compared with Mo/H-MCM-56(C), the sample of Mo/H-MCM-56(H2O2) shows higher conversion of methane and yield of benzene, with lower selectivity to benzene and higher selectivity to coke. The relatively high benzene yield might be mainly assigned to the existence of more 10-ring channels, while the high selectivity of coke should be due to the presence of large amounts of 12-ring pockets and acid sites exposed to the crystal exterior over Mo/H-MCM-56(H2O2). [Copyright &y& Elsevier]