The separation of manganese from cobalt sulfate solutions is crucial in the field of spent lithium-ion battery recycling. A membrane-based microreactor is used to reveal required mass transfer characteristics as is diffusion and chemical reaction. The dependence of di-(2-ethylhexyl)phosphoric acid (D2EHPA) concentration, pH, and metal ion concentration on the extraction efficiency are investigated. A back-reaction term is introduced giving a significant influence on the effective extraction rate even at small metal complex concentrations as initial extraction rates proved to be inaccurate to describe the system. It is shown that the extraction of manganese at a pH of 3.0 is mainly diffusive while the cobalt extraction is strongly kinetically controlled. At a separating pH of 3.9 a good agreement between the model and experimental data is only given if the equilibrium back-extraction rate is considered (deviation less than 5%).