AbstractCarbon dioxide (CO2) capture technologies are crucial for mitigating climate change, with post‐combustion capture (PCC) using chemical absorption being a leading method. However, the energy‐intensive solvent regeneration process presents a significant challenge, consuming up to 50% of the total energy in carbon sequestration. Despite extensive research on absorption, desorption studies remain limited. This study focuses on the desorption analysis through experimental runs in a pilot‐scale tray column with varying flow rates, validating an Aspen Plus model. The research compares the impact of the number of stages, feed stage position, column pressure, and reflux ratio between equilibrium and rate‐based models. The findings reveal enhanced desorption efficiency through optimized operational conditions, including reduced flow rates, additional equilibrium stages, feeding stage positioning closer to the condenser, elevated pressures, and lower reflux ratios. © 2024 Society of Chemical Industry and John Wiley & Sons, Ltd.