1. Influence of Liquid-Liquid Phase Separation on the Crystallization of L -Menthol from Water
- Author
-
Marco Mazzotti and Ian de Albuquerque
- Subjects
Materials science ,General Chemical Engineering ,Analytical chemistry ,02 engineering and technology ,General Chemistry ,010402 general chemistry ,021001 nanoscience & nanotechnology ,01 natural sciences ,Industrial and Manufacturing Engineering ,0104 chemical sciences ,law.invention ,Suspension (chemistry) ,Condensed Matter::Soft Condensed Matter ,Solvent ,symbols.namesake ,Cooling rate ,law ,symbols ,Liquid liquid ,L menthol ,Crystallization ,0210 nano-technology ,Raman spectroscopy ,Phase diagram - Abstract
The crystallization of L-menthol in water was investigated, with the intent of understanding the effect that liquid-liquid phase separation (LLPS) has on the properties of product crystals. First the binary phase diagram was measured, comprising both solid-liquid and liquid-liquid equilibrium regions. Subsequently, a calibration for the online monitoring of solid and liquid-liquid suspension densities was performed using Raman spectroscopy, thus enabling the detection of LLPS and crystallization. By using the obtained phase diagram, an initial composition lying within the LLPS region, was selected to perform cooling crystallization. Crystallization was monitored online using Raman spectroscopy, and after crystallization occurred the solution was filtered, solids were air dried, ground, and subsequent offline characterization was performed using DSC, XRD, and Karl-Fisher. It was shown that crystallization followed by LLPS led to the formation of the most stable polymorphic form, yet those solids contained solvent inclusions. The initial amount of inclusions was shown to be a function of operating conditions, namely cooling rate and suspension density.
- Published
- 2017