Acoustic on-line monitoring of solution crystallization process in pure and impure media
Résumé
We show that acoustic emission (AE) is a very attractive non intrusive technique for monitoring crystallization processes. AE has been successfully applied in many fields of material sciences and it was also used in the pharmaceutical industry for monitoring various chemical engineering processes including fluidized bed granulation, fluidized bed coating, powder compaction, etc. However, few studies deal with the use of AE to monitoring crystallization processes. The objective of this work is to evaluate the potential for using acoustic emission to monitor polythermal batch crystallization in the absence and presence of impurities. The basic concept behind AE monitoring of crystallization processes is that the phase transitions occurring during crystallization in solution induce physicochemical changes in the suspension. Such changes release energy and therefore generate acoustic elastic waves propagating in the liquid medium. Furthermore, as crystal particles are generated, the elastic properties of the dispersed phase also change. The latter changes affect the acoustic emission caused by the particle collision impacts and inter-particles and/or particles-wall frictions. The elasticity of crystals and their kinetic energy are also affected by many other properties such as size, shape, hardness, density, uniformity of composition which obviously depend on the presence of impurities during the process. We report preliminary batch solution cooling experiments obtained with the model system Ammonium Oxalate/water (AO) in the presence of Nickel Sulfate as impurity. The experiments are monitored using AE, ATR FTIR measurement of supersaturation and CSD analysis performed thanks to in situ image acquisition. Complex but promising information is obtained thanks to AE monitoring.
Domaines
Génie des procédés
Origine : Fichiers produits par l'(les) auteur(s)
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