Zinc hexacyanoferrate nanocubes have been synthesized following an extremely simple method and characterized by elemental analysis, thermal analysis, infrared spectroscopic and X-ray diffraction techniques. Field emission scanning electron microscopic image showed that it consisted of sharp Cubic particles With size ranging from 83 to 164 nm. Catalytic activity of nanocubic Zinc hexacyanoferrate has been studied for solvent-free oxidation of benzyl alcohol using H2O2 as oxidant under the optimum conditions of certain parameters such as benzyl alcohol to H2O2 molar ratio, the amount of catalyst, reaction time and temperature. (C) 2009 Elsevier B.V. All rights reserved.