Industrial batch crystallization of a plate-like organic product. In situ monitoring and 2D-CSD modelling. Part 2: Kinetic modelling and identification
Résumé
The batch seeded cooling solution crystallization of a fine organic material, exhibiting a platelet-like habit, was investigated and a model of the time variations of the crystal size distribution (CSD) was designed using two-dimensional population balance equations. Activated surface secondary nucleation and attrition secondary nucleation mechanisms were considered, coupled with growth mechanisms of two main dimensions of the crystal, resulting in a set of eight kinetic parameters. The model relates the effects of the main batch operating conditions: seeding temperature, cooling rate and total area of the seed particles, on both the supersaturation profile and bi-dimensional CSD. Surface secondary nucleation occurs first since it is promoted by the introduction of seeds and remains active as long as the relative supersaturation exceeds a threshold value of about 16%. It vanishes below which could be expected as we deal with an activated mechanism. Contact secondary nucleation occurs later when the concentration of solid is sufficient. It is spread over time until supersaturation disappears at the end of the batch process. This contact secondary mechanism is assumed to be the dominant nucleation mechanism as it generates about two-thirds of the final crystal number. Sharp desupersaturation profile following the introduction of seeds, which was observed experimentally, is shown to be quantitatively described through the growth of seed particles. The termination of the batch process is more difficult to represent. Due to crystal attrition, distinct growth rates between initial and secondary crystals or growth rate dispersion might explain such difficulty.