Microwave‐Aided Triacetin Synthesis Using CeO ₂ ─Gd ₂ O ₃ Catalyst and Crude Bio‐Oil Extract Glycerol

ABSTRACT Facile synthesis of glycerol acetins using crude glycerol obtained from bio‐oil conversion offers a sustainable route for waste utilization and green chemistry. In this study, the catalytic acetylation of glycerol with aliphatic and aromatic acids was investigated using a cerium (CeO 2 ) and gadolinium (Gd 2 O 3 ) mixed oxide system as heterogeneous catalysts. The mixed oxide was synthesized by a coprecipitation method assisted by microwave irradiation and characterized using BET surface area, XRD, SEM, and FTIR techniques. The catalytic activity of the samples was evaluated under optimized reaction conditions to maximize the yields of monoacetin, diacetin, and triacetin. The addition of Gd 2 O 3 to the CeO 2 system increased the total acidity, with strong Lewis acidity arising from enhanced oxygen mobility, which favored selective triacetin formation and broader conversion profiles. A synergistic effect was observed, resulting in high glycerol conversion (>90%) and triacetin selectivity (>60%) under mild conditions. The catalysts also demonstrated good reusability over multiple cycles with minimal loss of activity. These findings highlight the potential of rare‐earth metal oxides in developing efficient and environmentally benign catalytic systems for glycerol upgrading.