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The presence of amines in reactive CO2 capture introduces additional interfacial complexity through the formation of amine–CO2 adducts whose speciation, charge, and transport properties directly govern electrocatalytic performance. Here, we show that the solvent environment controls the nature of these adducts and, consequently, their reactivity and selectivity at solid–liquid interfaces. Using monoethanolamine (MEA) in dimethyl sulfoxide (DMSO), we demonstrate a shift from ionic carbamate–ammonium pairs in aqueous media to predominantly neutral carbamic acid species in nonaqueous electrolyte. This transition reduces electrostatic screening by ammonium ions, enhances accessibility of the reactive CO2 intermediate at the interface, and suppresses competing proton-coupled reactions such as hydrogen evolution. As a result, selective CO formation is achieved with Faradaic efficiencies up to ~78% using earth-abundant catalysts under pure CO2 feeds, and ~35–43% at current densities near 100 mA cm-2 under oxygen-rich conditions representative of flue gas (17% CO2, 17% O2). Stability tests over tens of electrochemical cycles show minimal loss in selectivity, indicating the robustness of the nonaqueous capture–conversion system. Collectively, these results establish solvent-controlled amine speciation as a key design parameter for engineering reactive capture electrolytes under industrially relevant conditions.
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