Electrocatalytic oxidation of glycerol to glyceric acid over dealloyed <scp>PtCu</scp> catalyst

Abstract Electrocatalytic upcycling of low‐value crude glycerol (GLY; ~0.17 US$/kg) to high‐value glyceric acid (GLA; ~7.5 US$/kg) can reduce biodiesel costs but is limited by low activity and selectivity. Herein, we developed a PtCu‐Act electrocatalyst by electrochemically dealloying surface Cu from PtCu alloy, forming a Pt‐enriched surface that strengthens GLY adsorption and accelerates OH* generation, delivering 0.24 mmol cm −2 h −1 GLA productivity with 56% selectivity at 0.8 V vs. RHE. We further introduce the photoassisted strategy, boosting GLA productivity and selectivity to 0.31 mmol cm −2 h −1 and 71%. Using crude GLY derived from waste cooking oil, this system co‐produces GLA and green hydrogen. Moreover, we designed an open‐loop flow battery (OLFB) integrating PtCu‐Act enables co‐generation of GLA and electricity during discharge and green hydrogen during charge, enabling carbon‐neutral biorefineries. This work couples surface reconstruction, photoassisted strategy, and OLFB integration to enable scalable GLY valorization with clean energy co‐production.