Journal
CHEMICAL ENGINEERING SCIENCE
Volume 152, Issue -, Pages 95-108Publisher
PERGAMON-ELSEVIER SCIENCE LTD
DOI: 10.1016/j.ces.2016.06.005
Keywords
Co-crystallization; Co-crystal; Stoichiometric; Process analytical technologies
Categories
Funding
- EPSRC [EP/I033459/1]
- Centre for Continuous Innovation in Continuous Manufacturing and Crystallization (CMAC)
- European Research Council under the European Union's Seventh Framework Programme (FP7)/ERC Grant [280106-CrySys]
- National Science Foundation (NSF), USA
- Science Foundation Ireland (SFI)
- Engineering and Physical Sciences Research Council [EP/I033459/1] Funding Source: researchfish
- EPSRC [EP/I033459/1] Funding Source: UKRI
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In this study, the selective crystallization and characterization of the stoichiometric forms of the p-to-luenesulfonamide/triphenylphosphine oxide (p-TSA-TPPO) co-crystal system in acetonitrile (MeCN) is demonstrated using batch and semi-batch crystallizers. In the batch study, both 1:1 and 3:2 p-TSA-TPPO were successfully isolated as pure forms. However, process variability was observed in a few experimental runs. To address the batch process variability issue, a control strategy was implemented using temperature cycling, aided by in situ process analytical technologies (PAT) to convert from 3:2 to 1:1 p-TSA-TPPO. In the semi-batch co-crystallization studies, the two molecular co-formers, p-TSA and TPPO, were dissolved in MeCN and pumped separately to the crystallizer. Changing the flow rates of the respective active ingredients allowed control over the co-crystallization outcome, and presents as a promising opportunity for development of a continuous co-crystallization process. (C) 2016 Published by Elsevier Ltd.
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