Influence of introduction devices on crystallisation kinetic parameters in a supercritical antisolvent process

摘要

Supercritical CO_2 antisolvent processes developed in this work are based on two different introduction devices: the Concentric Tube Antisolvent Reactor (a capillary centred in a larger tube) and the Impinging Jet Technology (organic solution and supercritical CO_2 impinging face to face). Griseofulvin pharmaceutical compound is chosen to test those two processes. The different experimental results indicate the same trends as classical supercritical antisolvent process for the evolution of particle size and particle size distribution with process parameters (mainly concentrations and flow rates). The second and main part is dedicated to the use of these experimental results for deriving modelling evaluation. Concerning this part, it is first shown that, in a first approximation, these processes can be represented by a continuous, mixed suspension and mixed product removal crystallizer. This allows modelling the mass particle size distribution. It also allows giving some numerical data on kinetics parameters (nucleation and growth). Secondly, general kinetic laws are derived for each process. In particular in the case of the impinging jet technology, the energy dissipated in the medium by the flow rates must be included in the crystallisation kinetic law.