Electrochemical Hydrogen Production From Biomass-Derived Molecules Using Tio2-Coated Stainless Steel Electrodes

The development of sustainable alternatives for hydrogen production has attracted increasing attention due to the environmental limitations of fossil-based processes. In this study, electrochemical hydrogen production was evaluated using biomass-derived substrates, including formic acid and glycerol, as well as shale wastewater as a potential reaction medium. In addition, TiO 2 films were applied to metallic electrodes as a strategy to reduce the energy demand of the process. The TiO 2 films were synthesized via the Pechini method and characterized by X-ray diffraction, confirming the formation of the anatase phase. Electrochemical experiments were conducted over 120 min, and hydrogen production was quantified by gas analysis. Under optimized conditions, the system produced approximately 0.035 mol of hydrogen using a mixture of 80% formic acid and 20% glycerol. The results showed that hydrogen production strongly depended on the composition of the reaction medium, with better results obtained in the absence of shale wastewater. The presence of shale wastewater, characterized by dissolved metals and organic compounds, led to a decrease in the current generated on chronoamperometry, suggesting an inhibitory effect associated with its complex composition. In addition, although TiO 2 -coated electrodes enabled hydrogen production, scanning electron microscopy revealed partial film detachment after electrolysis, indicating limited coating stability under operating conditions. These findings demonstrate the potential of biomass-derived substrates for electrochemical hydrogen production, while highlighting the challenges associated with complex waste matrices and the need to improve electrode coating stability and overall system performance. • TiO₂ films with anatase phase were synthesized by the Pechini method • TiO₂-coated stainless steel electrodes were applied to hydrogen production • Waste-derived electrolytes (formic acid and glycerol) enabled hydrogen generation • An optimized 80% formic acid/20% glycerol mixture yielded 0.035 mol of H₂ • SEM and Raman analyses revealed partial TiO₂ film detachment after electrolysis