| Summary: | In the present work, a series of catalysts based on aluminum and zirconium oxides was studied for the transformation of glucose into 5-hydroxymethylfurfural. These catalysts were characterized by using experimental techniques, such as X-ray diffraction, N<sub>2</sub> adsorption–desorption at −196 °C, X-ray photoelectron spectroscopy, temperature-programmed desorption of NH<sub>3</sub> and CO<sub>2</sub>, and scanning transmission electron microscopy. The catalytic behavior in glucose dehydration was evaluated in a water-methyl isobutyl ketone biphasic system, in the presence of CaCl<sub>2</sub>, in order to minimize losses due to unwanted secondary reactions. High glucose conversion and 5-hydroxymethylfurfural (HMF) yield values were obtained in the presence of an Al(Zr)O<sub>x</sub> catalyst with an Al:Zr molar ratio of 7:3, reaching 97% and 47%, respectively, at 150 °C after 120 min. Under tested conditions, this catalyst retained most of its catalytic activity for four reuses.
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