Abstract
Self-optimisation constitutes a very helpful tool for chemical process development, both in lab and in industrial applications. However, research on the application of model-free autonomous optimisation strategies (based on experimental investigation) for complex reactions of high industrial significance, which involve considerable intermediate and by-product formation, is still in an early stage. This article describes the development of an enhanced autonomous microfluidic reactor platform for organolithium and epoxide reactions that incorporates a successive combination of inline FT-IR spectrometer and online mass spectrometer. Experimental data is collected in real-time and used as feedback for the optimisation algorithms (modified Simplex algorithm and Design of Experiments) without time delay. An efficient approach to handle intricate optimisation problems is presented, where the inline FT-IR measurements are used to monitor the reaction’s main components, whereas the mass spectrometer’s high sensitivity permits insights into the formation of by-products. To demonstrate the platform’s flexibility, optimal reaction conditions of two organic syntheses are identified. Both pose several challenges, as complex reaction mechanisms are involved, leading to a large number of variable parameters, and a considerable amount of by-products is generated under non-ideal process conditions. Through multidimensional real-time optimisation, the platform supersedes labor- and cost-intensive work-up procedures, while diminishing waste generation, too. Thus, it renders production processes more efficient and contributes to their overall sustainability.Graphical abstract
Highlights
When industrial production processes are not conducted under ideal conditions, labor- and cost-intensive work-up procedures become necessary to fulfill product quality requirements
Spectroscopy and online mass spectrometry, two different optimisation studies were compared: In the first study, selfoptimisation was only based on inline FT-IR measurements, aiming at maximisation of main product yield
Regarding the optimisation procedure based exclusively on FT-IR measurements, a modified Simplex algorithm and Design of Experiments were implemented as optimisation strategies
Summary
When industrial production processes are not conducted under ideal conditions, labor- and cost-intensive work-up procedures become necessary to fulfill product quality requirements. Several optimisation strategies exist for this purpose [1, 2]. Their high significance for chemical process development, both in lab and in industrial applications, has been demonstrated by the extant literature [3–11]. Process optimisation often proceeds through one-by-one optimisation [12, 13] instead of a more efficient multidimensional approach [14, 15]. In academic research, such systematic, multidimensional optimisation strategies have been studied in detail [16–28]. They have been proven to constitute a valuable tool for process optimisation, especially when being integrated into fully-automated microreactor platforms [29–35]. Inline FT-IR spectroscopy and online mass spectrometry constitute promising analysis techniques that enable rapid quantification of reactants (analysis duration
Sign-in/Register to view highlights & summary Sign-in/Register to access full text options 
Talk to us
Join us for a 30 min session where you can share your feedback and ask us any queries you have
Schedule a call
