A high pressure single-pass high-conversion electrochemical cell for intensification of organic electrosynthesis processes

Abstract

The anode oxidation of 4-methoxytoluene (4-MT) to 4-methoxybenzyl dimethylacetal (4-MBDMA) in methanol is used as a test reaction for the study of a microchannel electrochemical reactor operated continuously in a single-pass high-conversion mode. The cell consists of two stainless steel cathodes, grooved with 100μm deep channels surrounding a flat glassy carbon anode. Pressures up to 20 bars are applied in the cell in order to reduce the volumetric flow rate of the cathodically produced hydrogen. Both the narrow gap and the operation under pressure lead to an enhancement of the electrolytic conductivity of the cell and make it possible to operate with concentrated solutions, with high current densities and with a very low supporting electrolyte concentration (i.e. 0.01M KF).The cell performance is discussed in terms of cell voltage, reactant conversion, material and current efficiency and finally selectivity in 4-MBDMA. The effect of inlet reagent concentration, pressure, flow-rate and temperature are investigated. Best performance is obtained with 0.5M 4-MT at 5 bars and 45°C: for a 90% conversion, selectivity and current efficiency attain, respectively, 92% and 85%. The high pressure, single-pass high-conversion cell exhibits in this case a space time yield 5–10 times higher than the current industrial process, with a significantly lower concentration of the supporting electrolyte.