In this work, the potential-controlled electrochemical aldol reaction of acetone to diacetone alcohol is studied in a standard batch electrolysis set-up as well as in an electrochemical continuous flow microfluidic reactor. In the batch set-up the influence of a number of parameters such as electrolyte composition, electrode material and electrolysis potential is described. Starting with pure acetone and a quaternary ammonium salt as support electrolyte, a maximum concentration of 15 m% diacetone alcohol is obtained after 2 h electrolysis in a divided set-up with a platinum electrode at -2.5 V [1, 2]. These results are taken into account in the optimisation towards maximum space-time yield and diacetone alcohol selectivity in the electrochemical micro flow reactor. Employing a flow cell system has important benefits which allows for a more efficient reaction such as a high surface-to-volume ratio of the electrode area to the reaction volume and close proximity of the electrodes. In addition optimization of the flow rate and cell height allows high yields of product in continuous operation. Incorporating a membrane in the reactor prevents cross-over of products which is detrimental for the yield.
[1] D. Pauwels, B. Geboes, J. Hereijgers, D. Choukroun, K. De Wael, T. Breugelmans, The application of an electrochemical microflow reactor for the electrosynthetic aldol reaction of acetone to diacetone alcohol, Chemical Engineering Research and Design, 128 (2017) 205-2013.
[2] D. Pauwels, J. Hereijgers, K. Verhulst, K. De Wael, T. Breugelmans, Investigation of the electrosynthetic pathway of the aldol condensation of acetone, Chemical Engineering Journal, 289 (2016) 554-561.
Figure 1: Exploded view of the electrochemical microreactor. 1: Electrode material 2: PEEK housing with hole for the electrode (2a: WE, 2b: CE), 3: POM spacer with serpentine reaction channel. 4: Aluminium parts with holes for the in- and outlet tubing, hole for the reference electrode (4a only) and holes for the electrode connections.