Accelerated analysis of the electrochemical production route for biomass-derived adiponitrile

The electrochemical transformation of biomass feedstocks offers a promising route for the sustainable production of fuels and chemicals, enhancing integration with renewable energy sources. Adiponitrile, a key intermediate in nylon 6,6 production, is mainly produced through thermochemical processes or methods relying on fossil fuel feedstocks. Alternatively, it can be produced through the Kolbe coupling of biomass-derived 3-cyanopropanoic acid, with its practical implementation hinging on understanding and controlling factors that dictate reaction selectivity. In this study, we establish relationships between electrolyte composition, electrochemical conditions, and performance metrics in this approach, achieving a maximum faradic efficiency of 40% toward adiponitrile at current densities up to 500 mA cm⁻². Implementing a semi-autonomous high-throughput electrochemical workflow, we tested hundreds of reaction conditions, accelerating the exploration of reaction parameters. Limitations and guidelines obtained from this study apply to a range of electrochemical decarboxylation reactions, and the accelerated research approach shows potential for speeding up the development of sustainable electrochemical processes.