Mn/Cu co‐doping of amorphous Ni ( OH ) x accelerates C α H activation for efficient adipic acid electrosynthesis

Adipic acid (AA) is a key nylon feedstock, but conventional nitric‐acid production is energy‐intensive and environmentally burdensome. Electrochemical synthesis offers a sustainable alternative, but inefficient C α  H activation limits reaction kinetics. Here, we developed an amorphous Mn/Cu co‐doped Ni(OH) x electrocatalyst on nickel foam via one‐step pulsed electrodeposition. Under optimized conditions, it achieved an AA production rate of 1448.8 μmol h −1 cm −2 and a Faradaic efficiency of 83.0%, outperforming most reported catalysts. Spectroscopic analyses, isotope‐labeling experiments, and theoretical calculations reveal that Mn/Cu co‐doping synergistically tunes the electronic structure of Ni active sites, lowers the activation barrier for the key C α  H activation step, and promotes reactive intermediates along the AA‐forming pathway. In a scale‐up flow electrolyzer, the catalyst delivered 60.79 mmol h −1 at 300 mA cm −2 , demonstrating promising scalability and economic potential. This work establishes Mn/Cu co‐doping as an effective strategy for accelerating AA electrosynthesis.