An extensive set of experimental data on multicomponent distillation with non-ideal systems in structured packed columns is presented to fill the gap of such data in literature. Experimental composition profiles along the column height obtained by distillation experiments with nonideal systems, methanol-2-propanol-water, methanol-acetonitrile-water, and acetone-methanol-2-propanol-water are reported. The distillation columns and the sampling technique are discussed in detail. An example how to use these data is shown by comparing the experimental data with simulation results when applying different mathematical models.