This research focuses on deducing the kinetic mechanism for biodiesel production catalyzed by a CaO nanocatalyst derived from waste cockle shells via thermal hydration–dehydration treatment. In addition, the CaO nanocatalyst preparation method via thermal hydration–dehydration-related parameters (hydration duration, recalcination temperature, and recalcination duration) was studied and optimized. The transesterification reaction catalyzed by the CaO nanocatalyst followed the Langmuir–Hinshelwood kinetic mechanism with surface reaction as the rate-limiting step. The relatively low activation energy (3786.7 J/mol) for a transesterification reaction offered by the CaO nanocatalyst enhanced the reaction rate to 27.3% FAME yield/hr. The optimal conditions for the thermal hydration–dehydration treatment used to develop the nano CaO catalyst were 6 h of hydration duration, 650 °C of recalcination temperature, and 3 h of recalcination duration. Of biodiesel yield, 94.13% was obtained at a moderate temperature of 60 °C and 3 h reaction time during the transesterification of palm oil catalyzed by the nano-CaO. SEM, BET, and TPD results proved that the CaO nanocatalyst had a large surface area (13.9113 m2/g) and high pore volume (0.0318 cm3/g) that were rich in active sites (1046.46 μmol CO2/g), and the pore diameter (33.17 nm) was accessible to reactants and products.
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