Cerium oxide (Ce100), molybdenum oxide (Mo100), and a material containing Ce and Mo (CeMo) were synthesized by the Pechini method, using glycerol as a polyol. These materials were applied for fructose conversion in an aqueous medium. The characterization results show the formation of cerium molybdate (Ce2(MoO4)3) for CeMo. Ce100 presented good thermal stability, and Mo100 sublimation of MoO3 and polymolybdates was verified. CeMo exhibited a mass loss of 19%, associated with the sublimation of MoO3 and polymolybdate species. Additionally, the existence of Bronsted and Lewis acid sites was confirmed, and the addition of Mo to Ce was an efficient strategy to increase the acidity. Regarding the catalytic activity (150 °C and 0.5 to 6 h), Ce100 exhibited low conversions and high selectivity to 5-hydroxymethylfurfural (5-HMF). For Mo100, high conversions, with a significant formation of insoluble materials, were detected. For CeMo, beyond the high activity, a lower formation of insoluble materials was noted. In this case, selectivity toward products from the retro–aldolic route and 5-HMF were obtained. These results indicate that the main factor influencing fructose conversion is an adequate combination of the acid sites. Recycling experiments were carried out, and stability was observed for four cycles, confirming the robustness of this system.

Pure and mixed oxides were synthesized using three methods, namely, coprecipitation, hydrothermal treatment using CTAB and Pechini treatment using glycerol, and investigated for the transformation of fructose, aiming to determine the influence of textural, structural, and acid-base properties on conversion and selectivity. All systems led to fructose conversion in an aqueous medium, and the factors that influenced the transformation were the textural and structural properties, as well as the number of acid sites present in the catalysts. The best conversions were observed using mixed oxides, highlighting SnNb (CTAB) and SnNb (GLY), showing the importance of the modulation of properties using the synthesis method. All systems were selective mainly for 5-HMF (5-hydroxymethylfurfural) and, to a lesser extent, for the products of the retro-aldolic route, and this selectivity was preserved, regardless of the catalytic system used.