Abstract: The glycerol market is currently experiencing a surplus due to increased biodiesel production,mcreating a demand for innovative approaches for its optimal utilization. Electrochemical valorization, particularly electro-oxidation, emerges as a promising solution for transforming excess glycerol into valuable products. Here, we report the use of carbon microfibers with ultralow nickel content (<5 wt %) to catalyze glycerol oxidation reaction (GOR), coupled with continuous gas-phase CO2 electroreduction to obtain formate. The humidified CO2-fed membrane electrode assembly electrolyzer, devoid of noble metals, efficiently produces oxidized products like lactate at concentrations of 0.144 g L-1 from glycerol and formate solutions reaching up to 100 g L-1 from CO2, surpassing previous methods employing commercial Pt-based materials. This novel approach not only enhances glycerol conversion efficiency but also contributes to sustainable carbon utilization, leading to the production of valueadded products.

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