The electrification of the production of fine chemicals has received increased interest in combating petrochemical routes with a high carbon footprint. Oxidising biomass from waste streams with concomitant hydrogen production, such as the transformation of lignin to vanillin, would be a great asset. Here, we show the combination of activity screening using a scanning droplet cell on a thin‐film Ni−Fe library and performance testing in a flow‐through cell with pulse electrolysis. The identified optimal Ni−Fe material composition was prepared on Ni foam with a polymer/metal precursor spray method. Full factorial and Doehlert matrix designs were employed to better comprehend each parameter‘s effects on the complex system. The best conditions for the electrooxidation of Kraft lignin at room temperature were at E1st=1.36 V vs RHE, t1st=1 s for the first pulse and E2nd=1.60 V vs RHE and t2nd=15 s for the second pulse, leading to the significantly improved production of 2.15 μmols of vanillin at room temperature. Pulsed chronopotentiometry was demonstrated to be a cost‐effective and robust technique with a simple setup for the valorisation of Kraft lignin. Combined with a subsequent thermolysis step, 8.05 μmols of vanillin were obtained.

中文翻译：

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基于实验设计的脉冲电解和热解法优化硫酸盐木质素香草醛产量

精细化学品生产的电气化在应对高碳足迹的石化路线方面引起了越来越多的关注。氧化废物流中的生物质并同时生产氢气，例如将木质素转化为香草醛，将是一笔巨大的财富。在这里，我们展示了在薄膜 Ni-Fe 库上使用扫描液滴池进行活性筛选和在流通池中使用脉冲电解进行性能测试的组合。确定的最佳 Ni−Fe 材料成分是通过聚合物/金属前驱体喷涂方法在泡沫镍上制备的。采用全因子和 Doehlert 矩阵设计来更好地理解每个参数对复杂系统的影响。硫酸盐木质素室温电氧化的最佳条件为 E第一名=1.36 V vs RHE, t第一名=1 s 第一个脉冲和 E第二名=1.60 V vs RHE 和 t第二名=第二个脉冲 15 秒，导致室温下 2.15 μmol 香草醛的产量显着提高。脉冲计时电位法被证明是一种经济有效且稳健的技术，具有简单的设置，可用于硫酸盐木质素的增值。结合随后的热解步骤，获得 8.05 μmol 香草醛。