The Kolbe electrolysis is a promising reaction to combine the usage of electrons as reagents and the application of renewable generated carboxylic acids as raw materials producing value added chemicals. Within this study, the electrolysis was conducted in a specially developed concept electrochemical microreactor and draws the particular attention to continuous operation and reuse of the aqueous electrolyte as well as of the dissolved unreacted feedstock. The electrolysis was conducted in alkaline aqueous solution using n‐octanoic acid as model substance. Platinized titanium as anode material in an undivided cell setup was shown to give Kolbe selectivity above 90 %. During the technically relevant conditions of current densities up to 0.6 A cm −2 and overall electrolysis times of up to 3 h, a high electrode stability was observed. Finally, a proof‐of‐concept continuous operation and the numbering up potential of the ECMR could be demonstrated.

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