Molybdate inserted layered double hydroxides (LDHs) were prepared by anion exchange in their aging step of synthesis under hydrothermal conditions. These materials were characterized by X-ray diffraction, chemical analysis, N2 physisorption, DR UV-vis and Raman spectroscopy. The solids as prepared showed interesting chemical, structural and textural properties. They proved high catalytic activity for the oxidation of sulfur-containing organic molecules and anthracene by hydrogen peroxide under gentle reaction conditions. The results were compared to those obtained over Mo-containing LDHs prepared by conventional ion exchange. (C) 2012 Elsevier B.V. All rights reserved.