Determining local concentrations of the analytes in state of the art microreactors is essential for the development of optimized and safe processes. However, the selective, parallel monitoring of all relevant reactants and products in a multianalyte environment is challenging. Electrochemical microsensors can provide unique information on the reaction kinetics and overall performance of the hydrogen peroxide synthesis process in microreactors, thanks to their high spatial and temporal resolution and their ability to measure in situ, in contrast to other techniques. We present a chronoamperometric approach which allows the selective detection of the dissolved gases hydrogen and oxygen and their reaction product hydrogen peroxide on the same platinum microelectrode in an aqueous electrolyte. The method enables us to obtain the concentration of each analyte using three specific potentials and to subtract interfering currents from the mixed signal. While hydrogen can be detected independently, no potentials can be found for a direct, selective measurement of oxygen and hydrogen peroxide. Instead, it was found that for combined signals, the individual contribution of all analytes superimposes linearly additive. We showed that the concentrations determined from the subtracted signals correlate very well with results obtained without interfering analytes present. For the first time, this approach allowed the mapping of the distribution of the analytes hydrogen, oxygen, and hydrogen peroxide inside a multiphase membrane microreactor, paving the way for online process control.

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A microstructured membrane reactor has been developed to overcome the safety and productivity challenge of the direct synthesis of hydrogen peroxide. A single membrane is employed for separate, continuous dosage of the gaseous reactants hydrogen and oxygen to the solid catalyst present in the aqueous solvent. Using a custom OpenFOAM® model, the impact of catalyst‐coated static mixers with different mixer geometries is studied. It is demonstrated that the custom fluid guiding elements outperform the investigated commercial static mixer under the flow conditions relevant to this application.

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