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Free-form shape optimization techniques are investigated to improve the separation efficiency of structured packings in laboratory-scale distillation columns. A simplified simulation model based on computational fluid dynamics (CFD) for the mass transfer in the distillation column is used and a corresponding shape optimization problem is formulated. The goal of the optimization is to increase the mass transfer in the column by changing the packing's shape, which has been previously used as criterion for increasing the separation efficiency of the column. The computational shape optimization yields promising results, with an increased mass transfer of nearly 20 %. For validation, the resulting optimized shape is additively manufactured using 3D-printing and investigated experimentally. The experimental results are in good agreement with the performance improvement predicted by the computational model, yielding an increase in separation efficiency of around 20 %.