Synthesis of cerium (IV) oxide by means of room temperature precipitation method was carried out. The effect of preparation variables such as synthesis time, calcination temperature and pH of the solution on resulting CeO 2 properties was discussed. Moreover, the comparison of CeO 2 samples prepared in a static and rotation mode of synthesis is presented. The solid catalysts were characterized by means of X-ray powder diffraction, scanning electron microscopy, transmission electron microscope, nitrogen physisorption, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy using pyridine as a probe molecule and temperature programmed desorption of CO2. Significant variations in physico-chemical properties of CeO2 by varying the preparation conditions were observed. Furthermore, the catalytic performances of CeO 2 catalysts were compared in the synthesis of diethyl carbonate starting from ethanol and CO2 using butylene oxide as a dehydrating agent. The dependence of CeO2 properties on its catalytic activity is evaluated in detail.