In this paper, a simple and economic route for the preparation of CuAl2O4 is proposed. The method was developed with the objective of obtaining a material with greater surface area, when compared to the spinel prepared by conventional combustion method (CCM). The catalytic properties of CuAl2O4 spinel prepared by CCM are compared with the one prepared microwave combustion method (MCM). Nano-sized CuAl2O4 were synthesized by both CCM and MCM using Opuntia dillenii haw as the plant extract, and were characterized by X-ray diffraction analysis (XRD), high resolution scanning electron microscopy (HR-SEM), N2 adsorption/desorption isotherms, and diffuse reflectance spectroscopy (DRS). Oxidation to their corresponding carbonyl compounds, high selectivity, and inexpensive precursors make this catalytic system a useful oxidation method for benzyl alcohol. The XRD results confirmed the formation of a cubic CuAl2O4. The formation of CuAl2O4 nanorices and nanorods structures were confirmed by HR-SEM. Through MCM method, CuAl2O4 (sample B) with a high specific surface area of was obtained. The band gap values of the (2.30 and 2.35 eV) for the obtained oxides are due to the nanometric dimensions of the nanostructures. The effect of the solvent, temperature, and oxidant on the oxidation of benzyl alcohol is reported. © 2014 Elsevier B.V. All rights reserved.