Environmentally benign production of biodiesel using heterogeneous catalysts is an important issue that requires the preparation of catalysts with high activity and reusability by a simple procedure. In this study, pure alumina and zinc oxide-and copper oxide-modified alumina were tested for the esterification of oleic acid to its methyl ester. The microwave-assisted solution combustion (MSC) method was used to prepare the catalyst samples that were characterized by X-ray diffraction (XRD), Fourier transform infra-red (FTIR), Brunauer-Emmett-Teller (BET) surface area measurement, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The spinel-type zinc aluminate was successfully synthesized, but CuO-modified alumina particles were clearly observed. Whereas in the alumina, much lower activity was observed than the doped alumina, zinc aluminate showed higher activity than copper oxide-alumina due to its smaller particle size, higher BET surface area, larger average pore size, and higher acidity. Finally, after the reaction conditions for the conversion of oleic acid were optimized for the case of spinel ZnAl2O4 as nanocatalyst, a yield of higher than 94% was obtained at 180 degrees C, 9 methanol/oleic acid molar ratio, 3 wt% of catalyst for 6 h. Furthermore, the catalyst deactivation was not observed after four reaction cycles at the optimal reaction conditions, indicating the feasibility of the proposed method for the preparation of industrial catalysts.