Synergistic pulsed electrocatalysis enables green and efficient synthesis of nylon monomer adipic acid.

Adipic acid (AA), a pivotal monomer, is produced via high-temperature nitric acid oxidation of cyclohexanone-cyclohexanol mixture (KA oil); a NO2-intensive process with a large carbon footprint. Electricity-powered electro-oxidative upgrading of KA is appealing, but impractical due to poor O2 utilization, oxygen evolution, and rapid catalyst passivation under potentials, causing an activity-stability-selectivity trade-off. We present an integrated electrocatalytic platform combining an α-FeOOH/NiFe layered double hydroxide (NiFe-LDH) heterojunction catalyst with pulsed electrolysis (PE) for green, efficient AA production. The heterointerface directs electron bridging between α-FeOOH and NiFe-LDH, lowering energy barriers for C-C scission, and creating surface sites for selective AA. PE mode decouples electro-oxidation from catalytic-site regeneration, cyclically refreshing poisoned centers to prevent intermediate accumulation. This strategy achieves 6.73 mmol h-1 cm-2 AA yield with 90.06% Faradaic efficiency over 300 h. Moreover a flow electrolyzer coupling anodic AA synthesis with cathodic CO2-to-formate conversion at 300 mA cm-2 enables scalable, sustainable nylon-monomer production.