In situ monitoring, control and optimization of a liquid-liquid phase separation crystallization
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- 作者：D. Duffy ; N. Cremin ; M. Napier ; S. Robinson ; M. Barrett ; Hongxun Hao ; Brian Glennon
- 关键词：Crystallization ; Process control ; Particulate processes ; Phase change ; Oiling out ; Supersaturation
- 刊名：Chemical Engineering Science
- 出版年：2012
- 出版时间：30 July, 2012
- 年：2012
- 卷：77
- 期：Complete
- 页码：112-121
- 全文大小：1433 K
文摘
The oiling out and crystallization behavior of a pharmaceutical compound from acetone and water was studied using a range of in-situ tools to qualitatively describe the oiling out phenomenon. Using a single peak height in the IR spectral region, the liquid phase concentration could be tracked during the liquid-liquid phase separation and also during the subsequent crystallization. This allowed the oiling out region of the system to be properly understood at a mechanistic level and also allowed for the implementation of a control technique that would control the particle size over regular seeding and maintain supersaturation at a constant level.