Fatty-acid-adsorbed γ-alumina was regenerated via transesterification using methanol with sulfuric acid as a catalyst. The fatty acids adsorbed on γ-alumina were converted to fatty acid methyl esters (FAME) and desorbed from the γ-alumina during the acid-catalyzed methanol regeneration process. A series of experiments studied the effect of the operating parameters (temperature, amount of sulfuric acid (wt%), methanol-solution-to-γ-alumina weight ratio, and regeneration time) on the acid-catalyzed methanol regeneration process. The chemically adsorbed fatty acids were desorbed effectively above 100 °C when the amount of sulfuric acid was 3 wt%, the methanol-solution-to-γ-alumina weight ratio was higher than 5 : 1, and the regeneration time was longer than 30 min. This new approach provides an ecofriendly process that operates at much lower temperatures than other methods of regeneration (thermal and supercritical methanol) while producing a renewable fuel.