Monitoring a batch crystallization process by acoustic emission

Crystallization is regarded as an important unit operation for separation and purification, as well as the production of solid particles with specified end-use properties. However, it is still difficult to control or to optimize the crystallization process due to the complexity of the coupled phenomena taking place simultaneously in the liquid and solid phases. In order to overcome such drawback, different analytical technologies have been implemented in the literature for monitoring (in situ, at best) the key crystallization parameters, e.g. solute concentration and crystal size distribution, which in turn enhances the comprehension about this operation. In our work, a multi-probe monitoring system composed of acoustic emission, ATR-FTIR and imaging probes was applied to the crystallization of a model system (an aqueous solution of adipic acid) in a semi-batch crystallizer. The crystallization was carried out under two different feed rates and under vacuum or atmospheric pressure. The goal was to demonstrate the usefulness of the multi-probe system for monitoring the crystallization process and to study the influence of the process (stirring rotation speed, cooling speed, etc.) on the acoustic emission. As a matter of fact, the multi-probe system tracked information about the dissolved adipic acid in the liquid phase with the ATR-FTIR spectrometry, while the crystal size, shape and number were monitored with the help of the imaging probe (with image treatment methods). The acoustic emission probes were used to detect the beginning of crystallization and the phenomena of crystal growth and agglomeration