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Two hierarchical Y and ZSM5 zeolites were prepared with a surfactant-mediated desilication method. Both the conventional and hierarchical forms were used to prepare NiCu-zeolites via the ion-exchange method. All samples were characterised using different techniques. For the hierarchical materials, N 2 physisorption and TEM analyses confirmed the appearance of mesoporosity. Transition metal-containing zeolites were used as novel electrocatalysts for the glycerol electrochemical oxidation reaction (GEOR) in the form of modified electrodes. Cyclic voltammetry was used to investigate the surface properties of the modified electrodes and their activity toward GEOR at different pH provided by different supporting electrolyte solutions, indicating alkaline conditions as the most promising ones. The hierarchical forms showed a remarkable higher activity compared to the conventional ones, together with appreciable yields towards partially oxidized products of industrial interest. Noteworthy, a stable current higher than 10 mA was generated, which is interesting to produce H 2 by coupling GEOR and hydrogen evolution reaction. [Display omitted] • Hierarchical Y and ZSM5 zeolites prepared via surfactant-mediated desilication. • Non precious metal-containing zeolites prepared by ion-exchanging Ni and Cu. • Electrodes modified with the metal-containing zeolites as electrocatalysts for GEOR. • Good yields of valuable oxidation products obtained using hierarchical zeolites. • Stable and high-intensity current possibly useable for simultaneously producing H 2. [ABSTRACT FROM AUTHOR]