A morphological strategy consisting of nanocasting synthesis of nickel aluminate spinel precursor was addressed. Two nanocasted catalysts were synthesized involving different template‑removal procedures (i.e., Teflon-assisted calcination vs. NaOH washing) for spinel recovery. As a reference, spinel NiAl2O4 supported by SBA-15 and bare nickel aluminate spinel were selected. The obtained solids were characterized in detail, examining their textural, acid–base, structural and compositional characteristics, either in the calcined or reduced forms. The as-obtained catalysts’ performance was evaluated in the aqueous-phase reforming of glycerol at 235 °C and 35 bar. Exhausted samples were also characterized to enlighten changes in catalyst properties during the aqueous-phase reaction. NiAl/SBA-15 and NiAl-NCF catalyst showed very poor catalytic performance for the glycerol transformation. NiAl-NCN catalyst presented improved activity with respect to NiAl, with a 20% higher hydrogen production rate but, as a drawback, higher methane formation for a whole range of glycerol conversions. Exhausted catalyst indicated nickel oxidized in liquid phase reaction.
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