High Throughput Multidimensional Kinetic Screening in Continuous Flow Reactors

Abstract

An automated high throughput multidimensional reaction screening platform based on an inline Fourier‐transform infrared spectroscopy (FT‐IR) is presented. By combining flow chemistry, machine automation and inline analysis, the platform is able to screen reactions in multidimensions (residence time, monomer concentration, degree of polymerization, reaction temperature and monomer conversion) rapidly and efficiently way. Kinetic data libraries associated with high data precision (absolute error < 4 %), high reproducibility and high data density are built with ease from the platform. To test the method, we screened the RAFT polymerization of methyl acrylate in unmatched detail, and the ring opening metathesis polymerization of methyl‐5‐norbornene‐2‐carboxylate. The method we introduce is a key step in providing ‘big data’ for data driven research in the future, and already at present allows for precise prediction of reaction outcomes within the high‐dimensional chemical parameter space that is screened.

Dynamic experiments in flow accelerate reaction network definition in a complex hydrogenation using catalytic static mixers

“…12–15 Dynamic experiments have been developed and demonstrated by various groups, but, thus far, used exclusively for homogeneous reactions. 16–24 Application of this technique to heterogeneously-catalyzed gas–liquid reactions, however, has not yet been investigated.…”

Bayesian optimization of radical polymerization reactions in a flow synthesis system

“…[39][40][41] Recent developments in microchemistry have led to the investigation of polymerization through flow synthesis, initially facilitated by micromixer-based systems. [42][43][44][45][46][47] Flow synthesis offers several benefits, including homogeneous mixing, efficient heat exchange, precise residence time control and scalability [48][49][50] , making it a suitable candidate for integration with machine learning techniques. [51][52][53][54][55][56][57] Warren et al previously developed a polymer synthesis and analysis platform that allowed RAFT polymerization to be automated and used this system to explore the trade-off between molar mass dispersity and monomer conversion 58 .…”

Optimization of heterogeneous continuous flow hydrogenation using FTIR inline analysis: a comparative study of multi-objective Bayesian optimization and kinetic modeling

“…Kinetic modeling, grounded in a comprehensive understanding of chemical processes, represents a classical and crucial strategy for reaction optimization, especially for heterogeneous hydrogenation reactions. [14][15][16][17] For instance, Su et al demonstrated the application of kinetic modeling in the heterogeneous flow hydrogenation of hexafluoroacetone trihydrate, revealing an adsorption-desorption mechanism with competitive adsorption of H2 dissociation. [18] Similarly, Yu et al conducted a continuous hydrogenation study of 2-(4-nitrophenyl) butanoic acid and kinetics study in a micropacked-bed reactor, employing kinetic analysis to elucidate the impacts of internal and external diffusion, as well as salt formation.…”