Simultaneous Electrochemical Upgrading of Biomass and CO₂ Utilization Using Fe/Ni‐Derived Carbon Nanotubes Derived from CO₂

Abstract Fossil fuel consumption has caused petroleum shortages and increased carbon emissions; thus, utilizing renewable resources in biorefineries for biomass‐derived chemical synthesis is promising. Among them, 2,5‐furandicarboxylic acid (FDCA) is a key alternative to terephthalic acid (PTA) for sustainable polyester production. In this work, we demonstrate an efficient approach for the simultaneous production of FDCA while utilizing carbon dioxide (CO₂) via an electrochemical approach. Complete electrooxidation of hydroxymethylfurfural (HMF) at the anode yields FDCA, while CO₂ reduction at the cathode produces valuable compounds such as carbon monoxide (CO). This concurrent HMF electrooxidation and CO₂ electroreduction strategy enables high‐value chemical production at mild conditions. In addition, we developed efficient single catalysts, FeNi metals supported on CO₂‐derived multi‐walled carbon nanotubes deposited on nickel foam (FeNiCNTs/NF) as both the anode and the cathode for HMF oxidation and CO 2 reduction, respectively. Remarkably, faradaic efficiencies reached 99.60% for FDCA (FE FDCA ) at the anode and 96.25% for CO (FE CO ) at the cathode. This study highlights the effective use of synthesized non‐noble metals supported on CO₂‐derived CNTs for integrated biorefinery and CO₂ utilization.