The
experimental realization of a continuous preferential crystallization
process, consisting of two mixed-flow crystallizers coupled via crystal-free
liquid exchange streams and with only the liquid phases operating
continuously, is addressed. Experiments in triplicate, using the conglomerate-forming
system of dl-asparagine monohydrate in water, were conducted,
and the achievement of nearly racemic composition of the liquid phase
in the crystallizers was verified. An experiment was also carried
out using seed crystals of a smaller average particle size than used
in the reference experiments. Successful enantioseparation by crystal
growth, with the repeatability being within ±10% deviation, was
obtained. However, slow crystal growth, due to a low surface integration
rate, led to a negligible consumption of the desired enantiomer added
in the feed solution, resulting in low productivities. Productivities,
yields, and purities of solid products were influenced by the morphological
differences in the seed crystals. Due to irregularly shaped seed crystals,
increase in the productivities and yields were achieved in the L-Tank.
Lower purities of solid products from the L-Tank compared to purities
of the solid products from the D-Tank were obtained. This could be
due to surface nucleation of d-asparagine monohydrate, ascribed
to the surface structure of the seeds of l-asparagine monohydrate
supplied. Improvements in productivity, yield, and purity in the L-Tank,
for the same process duration, were realized using seed crystals of
lower average particle size having a smoother surface structure. The
main advantages compared to other separation processes are low capital
cost, high crystal purity and yield, ease of upscaling, increased
safety, and reduced environmental impact due to reduction in the amount
of solvent used. The application is currently limited to conglomerate-forming
systems, but the separation concept may open new possibilities for
process improvements regarding enantioseparation of racemic compound-forming
systems as well.