(701e) An Autonomous Microreactor Platform for the Rapid Identification of Kinetic Models for Fast Liquid/Liquid Reactions

One of the most complex topics for design of multiphase liquid/liquid processes is the development of reliable and accurate kinetic models, since reaction kinetics and mass transfer are both controlling the process.^[1] In order to develop intrinsic kinetic models, a researcher needs to ensure that the reaction rate is not limited by mass transfer phenomena, identify the model structure that can best describe the reaction chemistry and obtain precise kinetic parameters.

This work shows the workflow for obtaining reliable and accurate kinetic models for fast liquid/liquid reactions by developing a close-loop experimental system. A reactive chemical system of interest is the heterogeneous nitration of 2-nitrotoluene (2-MNT), since it is a very fast reaction,^[2] highly exothermic,^[3] and reaction products, 2,4-dinitrotoluene (2,4-DNT) and 2,6-dinitrotoluene (2,6-DNT), are important intermediates in fine chemical industries.^[4] In this work, we utilize an autonomous flow platform equipped with continuous flow micromixers to achieve efficient mixing and ensure process safety. Work-up steps are performed in-line and phases are separated based on membrane separation. Organic phase passes through a benchtop NMR for quantification of reaction products and data are processed by an MBDoE algorithm to design the next experiment with the objective of achieving a precise estimation of kinetic parameters for a pre-selected kinetic expression.^[5]

References: [1] React. Chem. Eng., 2019, 4, 235, [2] React. Chem. Eng., 2022, 7, 111-122, [3] Beilstein J. Org. Chem., 2014, 10, 405-24, [4] Phys. Chem. Chem. Phys., 2021, 23, 4658–4668, [5] Chem. Eng. J., 2019, 377, 120346