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Droplet formation in oiling-out crystallization has important implication forseparation and purification of pharmaceutical active ingredients by using anantisolvent. In this work, we report the crystallization processes ofoiling-out droplets on surfaces during solvent exchange. Our model ternarysolution is beta-alanine dissolved in isopropanol and water mixture. As theantisolvent isopropanol displaced the alanine solution pre-filled in amicrochamber, liquid-liquid phase separation occurred at the mixing front. Thealanine-rich subphase formed surface microdroplets that subsequentlycrystallized with progression of solvent exchange. We find that the flow rateshave significant influence on the droplet size, crystallization process, andgrowth rate, and final morphology of the crystals. At fast flow rates thedroplets solidified rapidly and formed spherical-cap structures resembling theshape of droplets, in contrast to crystal microdomains or thin films formed atslow flow rates. On a highly hydrophilic surface, the crystals formed thin filmwithout droplets formed on the surface. We further demonstrated that by thesolvent exchange crystals can be formed by using a stock solution with a verylow concentration of the precursor, and the as-prepared crystals can be used asseeds to trigger crystallization in bulk solution. Our results suggest that thesolvent exchange has the potential to be an effective approach for controllingoiling-out crystallization, which can be applied in wide areas, such asseparation and purification of many food, medical, and therapeutic ingredients.

Oiling-out Crystallization of Beta-Alanine onSolid Surfaces Controlled by Solvent Exchange