A novel nickel‐based metal organic framework (MOF) [Ni(FDC)(CH3OH)1.5(H2O)0.5](H2O)0.35 (UOW‐6) utilizing biomass‐derived 2,5‐furan dicarboxylate (FDC) as a ligand is reported as an electrocatalyst for anodic ethylene glycol oxidation with cathodic hydrogen evolution. The MOF structure was analyzed using single crystal X‐ray‐diffraction, TGA and thermodiffractometry, to establish its structure and verify phase purity. The material was dropcast on carbon fiber paper as a catalyst, and by using a three‐electrode system, UOW‐6 requires only 1.47 V to attain a current density of 50 mAcm‐2. During oxidation of the ethylene glycol (EG), UOW‐6 shows unprecedented selectivity towards formic acid with a Faradaic efficiency of 94% and remarkable stability over 20 days. The combination of electrochemical measurements and in situ Raman confirmed in situ formed NiOOH at the surface of UOW‐6 as the catalytically active sites for EG oxidation. This work not only presents a pioneering application of FDC‐based MOFs for polyethylene terephthalate (PET) upcycling but also underscores the potential of electrocatalysis in advancing sustainable plastic valorization strategies.
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