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Rapid optimisation of API crystallisation in a segmented flow reactor with a continuous, variable temperature gradient

Robertson, Karen; Seeberger, Peter H.; Gilmore, Kerry

Rapid optimisation of API crystallisation in a segmented flow reactor with a continuous, variable temperature gradient Thumbnail


Authors

Peter H. Seeberger

Kerry Gilmore



Abstract

The reproducible crystallisation of small molecules can be difficult due to the myriad of factors influencing crystallisation events and growth as well as the inhomogeneity of traditional approaches. While continuous flow approaches can increase reproducibility in sensitive chemical processes, the controlled formation of solids in flow is technically challenging due to issues with fouling. Further, while one of the simplest means of inducing crystallisation is the slow decrease of temperature, smooth temperature gradients across a long distance have not been achievable in flow reactors. Herein we disclose a segmented flow reactor employing a controlled continuous temperature gradient that allows for continuous crystallisation at temperature profiles ranging from 80 to 15 °C. The temperature gradient can be altered (input and output temperatures independently) during operation to rapidly optimise crystallisation conditions. Fine control of crystallisation conditions for the reproducible growth of single paracetamol crystals serves to illustrate the potential of this continuous crystallisation method.

Citation

Robertson, K., Seeberger, P. H., & Gilmore, K. (2022). Rapid optimisation of API crystallisation in a segmented flow reactor with a continuous, variable temperature gradient. Reaction Chemistry and Engineering, https://doi.org/10.1039/d2re00183g

Journal Article Type Article
Acceptance Date Sep 20, 2022
Online Publication Date Sep 21, 2022
Publication Date Sep 21, 2022
Deposit Date Oct 26, 2022
Publicly Available Date Oct 26, 2022
Journal Reaction Chemistry and Engineering
Print ISSN 2058-9883
Electronic ISSN 2058-9883
Publisher Royal Society of Chemistry (RSC)
Peer Reviewed Peer Reviewed
DOI https://doi.org/10.1039/d2re00183g
Keywords Fluid Flow and Transfer Processes; Process Chemistry and Technology; Chemical Engineering (miscellaneous); Chemistry (miscellaneous); Catalysis
Public URL https://nottingham-repository.worktribe.com/output/12036109
Publisher URL https://pubs.rsc.org/en/content/articlelanding/2022/RE/D2RE00183G

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