Synthesis of CoO–NiO promoted sulfated ZrO2 super-acid oleophilic catalyst via co-precipitation impregnation route for biodiesel production

This study focuses on the synthesis of a novel heterogeneous CoO–NiO promoted sulfated ZrO2 (CN/SZ) catalyst and investigating its catalytic efficiency as a transesterification reagent. Catalytic performance has also been compared with two reference catalysts viz., sulfated ZrO2 (SZ) and pure ZrO2 (Z). Prepared materials were characterized using X-ray diffraction (XRD) technique, N2- adsorption/desorption study, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDAX), Raman, Fourier Transformed Infrared (FTIR), and X-ray photoelectron (XP) spectroscopy techniques. Surface acidity and basicity were assessed by NH3 and CO2 temperature-programmed desorption (TPD) respectively that established high surface acidity and basicity of CN/SZ nanocatalyst. The reagent has shown supreme catalytic performance as only 0.2 wt% catalyst loading amount has provided 98.8% of biodiesel yield with 3:1 MeOH:Oil molar ratio at 65 °C for 2 h. Also, the reusability study has proved the efficacy of CN/SZ nanocatalyst that it can successfully be reused in five consecutive reaction cycles displaying promising results and the reactivated catalyst provided remarkably high biodiesel yield of 96.8%. Further, the mechanistic pathway of the simultaneous catalytic esterification of free fatty acid and transesterification of triglyceride occurring on catalyst surface has also been explored.