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Abstract Ethylene glycol is a widely utilized commodity chemical, the production of which accounts for over 46 million tons of CO₂emission annually. Here we report a paired electrocatalytic approach for ethylene glycol production from methanol. Carbon catalysts are effective in reducing formaldehyde into ethylene glycol with a 92% Faradaic efficiency, whereas Pt catalysts at the anode enable formaldehyde production through methanol partial oxidation with a 75% Faradaic efficiency. With a membrane-electrode assembly configuration, we show the feasibility of ethylene glycol electrosynthesis from methanol in a single electrolyzer. The electrolyzer operates a full cell voltage of 3.2 V at a current density of 100 mA cm⁻², with a 60% reduction in energy consumption. Further investigations, using operando flow electrolyzer mass spectroscopy, isotopic labeling, and density functional theory (DFT) calculations, indicate that the desorption of a *CH₂OH intermediate is the crucial step in determining the selectively towards ethylene glycol over methanol. 

Abstract Electrochemical oxygen reduction to hydrogen peroxide (H 2 O 2 ) in acidic media, especially in proton exchange membrane (PEM) electrode assembly reactors, suffers from low selectivity and the lack of low-cost catalysts. Here we present a cation-regulated interfacial engineering approach to promote the H 2 O 2 selectivity (over 80%) under industrial-relevant generation rates (over 400 mA cm −2 ) in strong acidic media using just carbon black catalyst and a small number of alkali metal cations, representing a 25-fold improvement compared to that without cation additives. Our density functional theory simulation suggests a “shielding effect” of alkali metal cations which squeeze away the catalyst/electrolyte interfacial protons and thus prevent further reduction of generated H 2 O 2 to water. A double-PEM solid electrolyte reactor was further developed to realize a continuous, selective (∼90%) and stable (over 500 hours) generation of H 2 O 2 via implementing this cation effect for practical applications.