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Membrane-assisted antisolvent crystallization (MAAC) is a crystallization technique in which the transport of antisolvent is controlled through a membrane either in the liquid or vapour form. As the antisolvent reaches the crystallizing solution, it changes its composition, so solubility decreases and the solute crystallizes; thereby, MAAC can be used as an efficient technique to control crystallization kinetics (Curcio et al., 2020). This work investigates the potential of MAAC, over conventional antisolvent crystallization, using flat-sheet porous hydrophobic membranes — Polyvinylidene fluoride and polypropylene. Amino acid crystallization in water, with the controlled addition of the antisolvent ethanol, was chosen as the model system for the study of MAAC. Amino acids are small molecules that form the elementary basis of peptides and proteins crucial for life; on the other hand, the amino acid-water-ethanol system allows us to evaluate the sole impact of the membrane process itself in controlling the increase of supersaturation. The resulting Crystal Size Distribution (CSD), crystal morphology, and crystalline form were evaluated for various flow conditions, correlating with the transmembrane flux of the antisolvent and its mixing on both sides of the membrane, affecting supersaturation directly. It was observed that with the increase of the crystallizing solution flow rate, the transmembrane antisolvent flux decreased. This resulted in a higher concentration of the dissolved solute in the feed solution, hence higher supersaturation, eventually a narrower CSD. The resulting crystal properties differed according to the difference in antisolvent-solute-membrane interactions. The physicochemical characteristics of the membranes, such as porosity and surface energy, influence the kinetics of crystallization significantly (Chergaoui et al., 2022). These results show the potential of using MAAC to intensify crystallization processes for various applications including polymorph selection, variation of crystal morphology, or narrower crystal size distribution. MAAC is particularly advantageous over conventional crystallizers in potentially purifying challenging reactions or developing thermally sensitive nanoparticles (metal-organic frameworks, catalysts, active pharmaceutical ingredients ...).
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Chergaoui, S., Leyssens, T., Debecker, D., & Luis Alconero, P. (2022). Membrane-assisted antisolvent crystallization: which factors control crystal properties? 9th World Congress on Particle Technology, Madrid, Spain. https://hdl.handle.net/2078.5/106208