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In this paper, CuO and CeO 2 were screened as co-catalyst components for Fe 2 O 3 /attapulgite (ATP) catalyst, and three new catalysts (CuO-Fe 2 O 3 /ATP, CeO 2 -Fe 2 O 3 /ATP and CuO-CeO 2 -Fe 2 O 3 /ATP) were prepared for degradation of methylene blue (MB). The three catalysts' characteristics were determined by BET, XRD, FT-IR, SEM and XPS. MB degradation in different systems and at different pH values was also studied. Under the conditions of H 2 O 2 concentration of 4.9 mmol L -1 , catalyst dosage of 5 g L -1 , pH of 5, reaction temperature of 60 °C and MB initial concentration of 100 mg L -1 , the as-synthesized catalysts showed much greater reaction rate and degradation efficiency of MB than Fe 2 O 3 /ATP catalyst. In addition, the reusability of the as-prepared composites was evaluated. The intermediate products of MB degradation were identified by LC-MS and the possible degradation process of MB was put forward., Competing Interests: There are no conflicts to declare., (This journal is © The Royal Society of Chemistry.)