3D Printed Microreactors for the Continuous Non‐Kolbe Electrolysis

Abstract

In the renaissance of organic electrochemistry, 150‐year‐old Kolbe chemistry offers a sustainable pathway to liquid energy carriers and commodities. Herein, easy‐access design methods for electrochemical microreactors employing 3D printing and simple post processing techniques are presented. The continuous Non‐Kolbe electrolysis of monomethyl succinic acid is studied as a test reaction for the production of an industrially relevant, green monomer. In a semi‐batch setup, methyl acrylate is produced with a maximum yield of 34 %, similar to results from a thoroughly optimized batch reaction in a prior study. In single‐pass experiments, a comparable faradaic efficiency of 54 % is achieved.

Scalable Microreactor Concept for the Continuous Kolbe Electrolysis of Carboxylic Acids Using Aqueous Electrolyte

“…Electrochemical conversion of levulinic acid to 2,7-octanedione and the non-Kolbe electrolysis of monomethyl succinic acid to methyl acrylate in single-pass and semi-batch mode were studied in electrochemical flow cells. [25] 3D printing techniques show a high potential for cost efficient and customizable manufacturing of electrochemical microreactors (ECMR) or flow cells that can be used to study the transformation from batch electrolysis into flow processes.…”

Electrochemical nitration for organic C–N bond formation: a current view on possible N-sources, mechanisms, and technological feasibility

“…115 For the rapidprototyping of electrochemical reactors, additive manufacturing techniques recently gain importance. [116][117][118][119][120] Such 3Dprinted reactors are also tested in CO2RR, although different challenges like chemical tolerance of the materials or tightness occur. 118,121 Therefore, to start, reliable catalytic activity should be demonstrated in an analytical H-cell reactor configuration.…”

“…[116][117][118][119][120] Such 3Dprinted reactors are also tested in CO2RR, although different challenges like chemical tolerance of the materials or tightness occur. 118,121 Therefore, to start, reliable catalytic activity should be demonstrated in an analytical H-cell reactor configuration. The electrosynthesis can then directly be transferred to a flow electrolyser allowing the use of GDEs.…”

LABS: Laboratory Automation and Batch Scheduling – A Modular Open Source Python Program for the Control of Automated Electrochemical Synthesis with a Web Interface

“…A review article for high‐throughput screening in electro‐organic synthesis was compiled by J. C. Vantourout and co‐workers [10] . With regards to electrochemical flow cells, methods like 3D printing allow prototyping and miniaturization to speed up development [11] . Additional reaction parameters for electrolysis in flow, such as flow rate, can complicate the optimization.…”

“…[10] With regards to electrochemical flow cells, methods like 3D printing allow prototyping and miniaturization to speed up development. [11] Additional reaction parameters for electrolysis in flow, such as flow rate, can complicate the optimization. This challenge can be overcome systematically by methodological approaches such as design of experiments or Bayesian optimization.…”