The integration of flow chemistry into continuous manufacturing
requires efficient, controllable, and continuous methods for the concentration
of diluted solutions on relatively small scales. The design and application
examples of a new continuous solvent removal process are presented.
The continuous stripping method employing dense carbon dioxide is
based on the formation of homogeneous mixtures of dilute organic solutions
of the target molecules with a large excess of carbon dioxide at temperatures
as low as 35 °C and pressures around 10 MPa. Subsequent pressure
reduction results in the quick release of carbon dioxide and vaporization
of a significant fraction of the organic solvent. The concentration
of the solute in the separated liquid phase can be up to 40 times
higher than in the feed. Among the many controllable process parameters,
the most significant ones are the mass–flow rate ratio of carbon
dioxide to the feed and the temperature of the phase separator. By
careful setting of the operational parameters, the degree of concentration
enhancement may be accurately controlled. The new apparatus—despite
consisting of laboratory equipment and being built in a fume hood—could
easily support pilot-scale synthetic flow chemistry, being a continuous,
efficient alternative to thermal concentration methods.