The growing demand for flexible and compact separation technologies has promoted the application of high‐gravity technology, like rotating packed beds (RPBs). Mass transfer characterization and packing design play an important role in the development of this technology. This article provides a systematic approach towards the evaluation of packing and the development of advanced packing design for distillation in RPBs. For the latter, an additive manufacturing approach is used to develop a new Zickzack packing for RPBs. The new packing provides better mass transfer at reduced pressure drop compared to available conventional packings, while being competitive in terms of mass transfer with the industrially applied rotating zigzag bed at significantly reduced pressure drop.