Abstract
Fast chemical process development is inevitably linked to an optimized determination of thermokinetic data of chemical reactions. A miniaturized flow calorimeter enables increased sensitivity when examining small amounts of reactants in a short time compared to traditional batch equipment. Therefore, a methodology to determine optimal reaction conditions for calorimetric measurement experiments was developed and is presented in this contribution. Within the methodology, short-cut calculations are supplemented by computational fluid dynamics (CFD) simulations for a better representation of the hydrodynamics within the microreactor. This approach leads to the effective design of experiments. Unfavourable experimental conditions for kinetics experiments are determined in advance and therefore, need not to be considered during design of experiments. The methodology is tested for an instantaneous acid-base reaction. Good agreement of simulations was obtained with experimental data. Thus, the prediction of the hydrodynamics is enabled and the first steps towards a digital twin of the calorimeter are performed. The flow rates proposed by the methodology are tested for the determination of reaction enthalpy and showed that reasonable experimental settings resulted.Graphical abstractA methodology is suggested to evaluate optimal reaction conditions for efficientacquisition of kinetic data. The experimental design space is limited by thestepwise determination of important time scales based on specified input data.
Highlights
Operated processes feature higher yields and selectivity, facilitate process automation, reduce the ecological footprint and offer shorter process development times [1,2,3]
The experimental settings are transferred via Open Platform Communications (OPC) Unified Architecture (UA) to the programmable logic controller (PLC), which controls the whole experimental setup
The control commands for the calorimeter are executed automatically using the PLC and subsequently, the measured values are evaluated
Summary
Operated processes feature higher yields and selectivity, facilitate process automation, reduce the ecological footprint and offer shorter process development times [1,2,3]. J Flow Chem evaluation of microreactor performance for fast and exothermic reactions has already been shown by Asano et al [13]. A methodology is developed for the selection of experiments in a continuous flow calorimeter during chemical process development aiming a time and cost-efficient acquisition of thermokinetic data. The methodology enables choosing the optimal reaction conditions out of the entire possible range of experimental parameters of the calorimeter rather than performing full factorial design of experiment. Optimal designs of experiments are determined, which offer maximal information gain with minimal effort. The proposed experimental settings are tested for the determination of the reaction enthalpy of a test reaction
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