Industrial batch crystallization of a plate-like organic product. In situ monitoring and 2D-CSD modelling: Part 1: Experimental study
Industrial batch crystallization of a plate-like organic product. In situ monitoring and 2D-CSD modelling: Part 1: Experimental study
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DOI：
10.1016/j.ces.2006.08.077
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发表时间：
2007-02
影响因子：
4.7
通讯作者：
M. Oullion;F. Puel;G. Févotte;S. Righini;P. Carvin
中科院分区：
文献类型：
--
作者：
M. Oullion;F. Puel;G. Févotte;S. Righini;P. Carvin
给出了一种细小有机物在乙醇水溶液中间歇冷却溶液结晶的实验结果。通过在线、原位ATR FTIR光谱确保了过程监测，提供了连续的溶质浓度估计。还进行了离线图像分析，以产生对小板样颗粒的2D晶体尺寸分布(CSD)的离散时间测量。通过对所选批次的定性分析，特别关注种子的大小和重量，强调了二次成核对过饱和过程和CSD过程的决定性作用。至少有两种形核机制可以解释实验结果：晶种的引入导致表面形核的显著爆发，冷却过程的持续，通过产生连续的过饱和，允许发生激活的二次形核。
Experimental results obtained during the batch cooling solution crystallization of a fine organic compound in aqueous ethanol solvent are presented. The process monitoring was ensured through in-line, in situ ATR FTIR spectroscopy, providing continuous solute concentration estimates. Off-line image analysis was also performed to yield discrete-time measurements of the 2D-crystal size distribution (CSD) of the platelet-like particles. The decisive effect of secondary nucleation on both the course of supersaturation and CSD was highlighted through the qualitative analysis of selected batch runs, particular attention being focused on the seeds size and weight. At least two nucleation mechanisms allow explaining the experimental results: the introduction of seeds causes a significant burst of surface nucleation and the continuation of the cooling process, through the generation of continuous supersaturation, allows activated secondary nucleation to take place.