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Investigation of agglomeration in the presence of oiling out in the antisolvent crystallization process

journal contribution
posted on 15.04.2021, 13:51 by Liping Wang, Ying Bao, Zhuang Sun, Valerie PinfieldValerie Pinfield, Qiuxiang Yin, Huaiyu YangHuaiyu Yang
Oiling out during the crystallization process often generates agglomeration. This research is focused on the control of agglomeration in the antisolvent crystallization of the propylparaben-ethanol-water system in the presence of oiling out, that is, the liquid-liquid phase separation phenomenon. Crystallization trajectories were designed to start from a homogeneous solution with different initial concentrations of propylparaben in ethanol, crossing the liquid-liquid phase separation region in the ternary phase diagram by adding the antisolvent of water. A combination of process analytical technology tools, such as focused beam reflectance measurement, particle visual monitoring, and attenuated total reflectance ultraviolet/visible, enabled the detection of the different stages of the oiling out crystallization process, including the droplet formation of the dispersed phase, prenucleation, nucleation, and crystal growth both in the liquid-liquid phase-separated system and in the homogeneous solution. The crystals tended to form normally at higher initial concentrations of propylparaben while tending to agglomerate at a lower initial concentration. Crystallization experiments were also performed with the addition of sonication, with variation in sonication start time, duration, and power. The results showed that ultrasound could reduce the agglomeration dependent on the initial application time. The mechanism of crystallization and agglomeration in oiling out was discussed.

Funding

China Scholarship Council, National Natural Foundation of China (No. 21576187 and No. 21776203)

Tianjin Municipal Natural Science Foundation (No. 18JCYBJC21100)

Regenerative BioCrystallisation

Engineering and Physical Sciences Research Council

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History

School

  • Aeronautical, Automotive, Chemical and Materials Engineering

Department

  • Chemical Engineering

Published in

Industrial & Engineering Chemistry Research

Volume

60

Issue

10

Pages

4110 - 4119

Publisher

American Chemical Society (ACS)

Version

AM (Accepted Manuscript)

Rights holder

© American Chemical Society

Publisher statement

“This document is the Accepted Manuscript version of a Published Work that appeared in final form in Industrial & Engineering Chemistry Research, copyright © American Chemical Society after peer review and technical editing by the publisher. To access the final edited and published work see https://doi.org/10.1021/acs.iecr.1c00491

Acceptance date

18/02/2021

Publication date

2021-03-03

Copyright date

2021

ISSN

0888-5885

eISSN

1520-5045

Language

en

Depositor

Dr Valerie Pinfield. Deposit date: 12 April 2021