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The control of antisolvent crystallization is a perplex that has not been resolved yet. To date, the process relies on the addition of downstream processing units such as grinding. Membranes, on the contrary, have the ability to control the transport of the antisolvent and provide excellent mixing that inhibit the formation of local supersaturations that are responsible for the random properties of the resulting crystals. In a previous work, we demonstrated that membranes can indeed provide in one step, a narrow crystal size distribution and a uniform shape; also, membrane properties like hydrophobicity, thickness and porosity play an important role in controlling the crystal size, and crystal size distribution [1-2]. We noticed that the flow rate had an impact on the hydrodynamics of the crystallizing solution, so this begs the question, what other operating conditions impact the crystallization process? This work investigated – besides the impact of flow rate – the impact of antisolvent composition, the temperature and gravity. Results were impressive such that in any condition, membranes were consistent in providing a narrow CSD. The prism-like shape of glycine crystals was maintained as well, but slightly altered when operating at a temperature of 35 °C. Finally, for the crystal size and the crystalline structure, it was demonstrated that the size does not change significantly ca. 5 um, and the monoclinic form was perfectly maintained in all conditions. The study shows that membrane is indeed a robust technology that can offer one-step uniform crystal properties. Most of all, it demonstrates from a kinetic perspective, that operational time can be extended given a specific combination of the four factors —flow rate, antisolvent composition, temperature or gravity. This membrane function is much-needed for the formation of organic compounds overall, particularly heat-sensitive ones as in pharma- and agro-industries, saving energy, time and footprint.
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Chergaoui, S., Debecker, D., Leyssens, T., & Luis Alconero, P. (2022). Intensification of antisolvent crystallization process using membrane technology. Euromembrane 2022, Sorrento, Italy. https://hdl.handle.net/2078.5/103358