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PAT-based design of agrochemical co-crystallization processes: a case-study for the selective crystallization of 1:1 and 3:2 co-crystals of p-toluenesulfonamide/triphenylphosphine oxide

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posted on 04.07.2016, 10:38 authored by Keddon Powell, D.M. Croker, Chris RiellyChris Rielly, Zoltan NagyZoltan Nagy
In this study, the selective crystallization and characterization of the stoichiometric forms of the p-toluenesulfonamide/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.

History

School

  • Aeronautical, Automotive, Chemical and Materials Engineering

Department

  • Aeronautical and Automotive Engineering

Published in

Chemical Engineering Science

Volume

152

Pages

95 - 108

Citation

POWELL, K.A. ... et al, 2016. PAT-based design of agrochemical co-crystallization processes: a case-study for the selective crystallization of 1:1 and 3:2 co-crystals of p-toluenesulfonamide/triphenylphosphine oxide. Chemical Engineering Science, 152, pp.95-108

Publisher

© Elsevier Ltd.

Version

AM (Accepted Manuscript)

Publisher statement

This work is made available according to the conditions of the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International (CC BY-NC-ND 4.0) licence. Full details of this licence are available at: https://creativecommons.org/licenses/by-nc-nd/4.0/

Publication date

2016

Notes

This paper was accepted for publication in the journal Chemical Engineering Science and the definitive published version is available at http://dx.doi.org/10.1016/j.ces.2016.06.005

ISSN

0009-2509

Language

en