Great effort has been applied to model and simulate the dynamic behavior of the reactive distillation as a successful process intensification example. However, very little experimental work has been carried out in transient conditions. The work presents a series of experiments for the production of ethyl acetate from esterification of acetic acid and ethanol in a reactive distillation pilot column. The steady-state approach performed experiments with both excess of alcohol and stoichiometric feed configuration. Predicted and measured results show good agreement and reveal a strong dependency of the structured packing catalyst activity on the pilot geometry and its operating conditions. The transient process behavior of the heterogeneously catalyzed system was deeply investigated and continuous and dynamic data were collected for an equilibrium model validation, after different perturbations on parameters. The experimental validation is shown to be essential to provide realistic hydrodynamic parameters, to understand the sensitive parameters such as heat losses and to adapt values for the catalyst holdup as a function of the system. (C) 2013 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.