Abstract
Electrochemical transformation of biomass feedstocks offers a promising route for 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 fossil fuel feedstocks. Alternatively, it can be produced through 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 Faradaic efficiency of 40% towards 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 the development of sustainable electrochemical processes.