Abstract: The present work aimed to investigate the law of the conversion of glycerol with diethyl carbonate (DEC) over the highly efficient Ce–NiO catalyst prepared by co-precipitation method. The thermodynamic and kinetics parameters of this reaction for glycerol carbonate synthesis were studied. The reaction equilibrium constants were investigated experimentally in the temperature region of 338–358 K, and the standard molar properties (at 298 K) were obtained (△H0= 115.71 kJ mol−1, △G0= 13.523 kJ mol−1, △S0= 0.343 kJ mol−1). Effects of various experimental conditions including stirring speed, reaction temperature, catalyst amount, reactant mole ratio on the reaction kinetics were also studied. Different order kinetic equations were used to simulate law of the transesterification process. The result shows a three-order equation of glycerol (two orders) and DEC (one order) was more appropriate to interpret the law of glycerol transesterification with diethyl carbonate. The activation energy of this reaction was obtained with 87.90 kJ mol−1. Finally, the microstructure and physicochemical properties of the Ce–NiO samples were studied by XRD, SEM, TEM, and CO2-TPD. One-pot catalytic conversion of glycerol into glycerol carbonate over Ce–NiO catalyst.