A process consisting in a cyclic combination of crystallization, milling, and dissolution stages is investigated by means of a dedicated experimental campaign. A specifically designed experimental rig, consisting of two jacketed batch crystallizers and a continuous rotor-stator wet mill, is used to carry out the tests. Experiments are performed in order to investigate the effect of the most relevant operating conditions, namely the number of cycles, the milling intensity, and the amount of mass dissolved during the heating stage. The conditions chosen to perform the experiments have been identified by means of a specifically designed mathematical model, whose results also constitute the basis for the analysis of the experimental data. An optimal experiment, identified heuristically with the help of process simulations, is performed to assess the performance of the newly developed combined cycles. Finally, for a comprehensive characterization study, two experiments, namely a single cooling stage with or without milling, are carried out to evaluate the benefits granted by the 3-stage process over more conventional techniques.