A new macroporous ZnO/MoO3/SiO2 hybrid was synthesized by a method involving sol-gel technology and biomimetic synthesis. It was characterized by Elemental analysis, Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), X-ray photoelectron spectrum (XPS) and scanning electron microscopy (SEM). Chemical degradation of 0.3 g/L Safranin T (ST) by air oxidation over macroporous ZnO/MoO3/SiO2 hybrid was studied. It was found that the decolorization efficiency and the chemical oxygen demand (COD) removal of ST reached above 95.3% and 93.2%, respectively, within 25 min at room temperature and atmospheric pressure. And the organic pollutant was mineralized to simple inorganic species such as HCO3-, Cl- and NO3-, while the total organic carbon (TOC) decreased 95.4%. The structure and morphology of the catalyst were still stable after six cycling runs and the leaching test showed negligible leaching effect. (C) 2011 Elsevier B.V. All rights reserved.