Novel attapulgite (ATP)/Ce1-xZrxO2 nanocomposite was prepared by a facile homogeneous deposition method using hexamethylenetetramine as precipitator. The catalytic activity of ATP/Ce1-xZrxO2 was investigated by oxygenating methylene blue dye wastewater using O-3 as oxidant. HRTEM. XRD, FT-IR, Raman and H-2-TPR data reveal significant interactions between Ce-Zr-O oxides and ATP support, the evolution of textural, structural and oxidation state as a function of the composition, and the formation of more oxygen vacancies in Ce1-xZrxO2. The molar fraction of Zr4+ demonstrates considerable influence on the degradation rate of the methylene blue. Compared with pure ATP and ATP/CeO2, the ATP/Ce1-xZrxO2 composite remarkably enhances catalytic activity, and a maximum degradation rate of methylene blue at 99% is achieved when the molar fraction x is 0.2. (C) 2012 Elsevier B.V. All rights reserved.