Closed-Loop Model-Based Design of Experiments for Kinetic Model Discrimination and Parameter Estimation: Benzoic Acid Esterification on a Heterogeneous Catalyst

Abstract

An autonomous reactor platform was developed to rapidly identify a kinetic model for the esterification of benzoic acid with ethanol with the heterogeneous Amberlyst-15 catalyst. A five-step methodology for kinetic studies was employed to systematically reduce the number of experiments required to identify a practical kinetic model. This included (i) initial screening using traditional factorial designed steady-state experiments, (ii) proposing and testing candidate kinetic models, (iii) performing an identifiability analysis to reject models whose model parameters cannot be estimated for a given experimental budget, (iv) performing online Model-Based Design of Experiments (MBDoE) for model discrimination to identify the best model from a list of candidates, and (v) performing online MBDoE for improving parameter precision for the chosen model. This methodology combined with the reactor platform, which conducted all kinetic experiments unattended, reduces the number of experiments and time required to identify kinetic models, significantly increasing lab productivity.