Effect of dilution on the performance of ionic liquids in milliflow solvent extraction applications: Towards integration of extraction, scrubbing and stripping operations with in-line membrane-based phase separation

Abstract

The combination of ionic liquids (ILs) and millifluidic reactors is often suggested as a form of process intensification. The high viscosity of ILs has, however, raised concerns about hydrodynamics, mass-transfer enhancement and the ability to integrate several millifluidic operations. In the present study the performance of a quaternary ammonium hydrogensulfate IL, [A336][HSO4], in a millifluidic solvent extraction (SX) process was evaluated and compared with various, lower viscosity solutions of the IL in a diluent. Dilution of [A336][HSO4] significantly improved the slug flow hydrodynamics by reducing the film thickness, avoiding the loss of secondary recirculations inside the plugs and improving stability at elevated flow rates. The overall mass-transfer performance of the system was also improved upon dilution by a balancing of mass-transfer and reaction limitations. It was also observed that dilution reduced reagent consumption and improved the extraction selectivity. In addition, the decrease of the viscosity of the IL upon dilution facilitated the use of an in-line membrane-based phase separator. An integrated millifluidic set-up containing an extraction, scrubbing and stripping reactor was built using these in-line phase separators and applied to the SX purification of germanium from a synthetic zinc refinery residue leachate. The integrated reactor system was operated using a 30 vol% [A336][HSO4] dilution in p-cymene and successfully run for 4 h without any loss in separation performance or stability.