Two-Phase Flow in a Coiled Flow Inverter: Process Development from Batch to Continuous Flow

Abstract

The transfer of batch processes to continuous flow is a major driver for the application of microreactors. Here, we present a methodology for the transfer of (bio)chemical reactions in batch mode to two-phase continuous flow. For our purposes, the coiled flow inverter (CFI) is a promising reactor design providing enhanced heat and mass transfer, narrow residence time distribution, and rapid mixing. First, this methodology is used for current development of a droplet-based reaction screening system, which was first tested with a Paal−Knorr pyrrole synthesis as model reaction. The reaction was successfully performed in the automated screening system. The yields compared to the batch mode revealed enhanced mass transfer of the product into the continuous phase. Second, we investigated the biocatalyzed oxidation of ABTS by the enzyme laccase in a straight capillary for process development in a CFI. Because of its high flexibility regarding substrate specificity, laccase oxidizes many substrates with a colored product. Hence, an optical evaluation method for determination of reaction rate is used. We compare the Michaelis−Menten kinetic of the batch reaction and the continuous reaction in a capillary. The results show that the batch reaction can be mapped to the capillary setup. However, the capillary in continuous operation enables higher screening capacity of different reaction conditions and simple scale-up procedure.

Reaction Optimization of a Suzuki‐Miyaura Cross‐Coupling Using Design of Experiments

“…Nevertheless, it was shown that screening of chemical reaction with the help of the software tool and in combination with lab automation can be rapidly performed to gain first insight into influencing effects. As an outlook, the software tool will be applied on a continuous automated screening system [13] compatible with the presented lab robot and a closed loop system with self-optimization should lead to a faster reaction optimization. Experiments with more data points should show the possibility to gain quantitative knowledge about kinetic data of chemical reactions.…”

Continuous flow technology-a tool for safer oxidation chemistry

“…295 Kockmann and co-workers reported the laccase catalyzed oxidation of chromogenic substrates 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) and syringaldazine (SAz) in a two-phase flow system in a coiled flow inverter (CFI). 296 The flow pattern in the CFI is redirected in the 90° bend to increase radial mixing which results in enhanced mass transfer.…”

P50 - Künstliche Intelligenz (KI)-basierte optische Sensorik für flüssig-flüssig Systeme

“…Für weitere Details sei hierzu ebenfalls auf Referenz [7] In Zukunft ist geplant die Tropfen erkennende KI ebenfalls anzuwenden um Tropfen in Schläuchen analysieren. Da Schläuche, beispielsweise als Coiled Flow Inverter (CFI), ein vielversprechendes Reaktordesign bieten, um Batch-Prozessen auf kontinuierliche Prozesse zu übertragen [9] kann auch hier eine automatisierte optische Prozessüberwachung einen Mehrwert bieten. Eine auf der KI-basierten optische Prozessüberwachung aufbauende Regelungsstrategie mittels Reinforcement Learning wird an der Extraktionskolonne ebenfalls realisiert, sodass die Kolonne komplett autonom betrieben werden kann.…”