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.

生物质原料的电化学转化为燃料和化学品的可持续生产提供了一条有前途的途径，增强了与可再生能源的整合。己二腈是尼龙6,6生产的关键中间体，主要通过热化学工艺或依靠化石燃料原料的方法生产。或者，它可以通过生物质衍生的 3-氰基丙酸的 Kolbe 偶联来生产，其实际实施取决于对决定反应选择性的因素的理解和控制。在这项研究中，我们通过这种方法建立了电解质成分、电化学条件和性能指标之间的关系，在高达 500 mA cm ^-2的电流密度下，己二腈的最大法拉第效率达到 40% 。通过实施半自主的高通量电化学工作流程，我们测试了数百种反应条件，加速了反应参数的探索。这项研究获得的局限性和指南适用于一系列电化学脱羧反应，加速研究方​​法显示了加速可持续电化学过程发展的潜力。