In the present work, the activated carbon was prepared from agricultural waste by an activation method using sodium hydroxide as an activating agent. The prepared AC-CC has been characterized by N₂ adsorption–desorption isotherms, thermogravimetric analysis (TGA-DTA), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and temperature-programmed desorption (TPD). The porous carbon was thus obtained with a specific surface area of 13.901 m² g⁻¹ and a total pore volume of 0.011 cm³ g⁻¹. The catalytic activity of the activated carbon has been studied for the ketalization of glycerol and provides maximum glycerol conversion of 72.12% under optimum conditions. The activity of the AC-CC also did not change appreciably for three consecutive batch reaction sequences. The spent catalyst was further analysed for elemental composition using XPS and surface morphology was studied using SEM. There was little deformation in the structure although the percentage of carbon remains almost same (∼72%) as that of the original catalyst, which contributes to the reduction of conversion efficiency of glycerol to solketal by 5% in the 3^rd consecutive reaction. Thus, AC-CC obtained from Zea mays L. cob could be a very promising renewable catalyst for glycerol conversion into solketal as a fuel-additive.