Separation Units and Equipment for Lab-Scale Process Development

Abstract

For complete chemical processes, downstream operation steps are essential, but on a miniaturized scale, they are not so far developed as the microreactors. This contribution presents three different unit operations for phase and component separation. Liquid-liquid extraction is often performed in columns, which were miniaturized for higher separation efficiency and flow rates suitable for processes in flow chemistry. Two-phase mass transfer processes in capillaries benefit from rapid final phase separation, which can be performed in an in-line phase splitter based on different surface wetting behavior. Crystallization is often a final purification step, which is performed in a continuously operated helical tube setup with narrow residence time distribution. For all unit operations, design criteria are shown with typical applications. The methodology of downscaling of known equipment and employing typical microscale phenomena such as good flow control, laminar flow, or dominant surface forces leads to successful equipment design.

Entwurf und Betrieb eines Rohrreaktors mit enger Verweilzeitverteilung

“…Eli Lilly für eine Hydrierung mit ca. 12 h Verweilzeit ; d) Wendelrohrreaktor mit jeweils zwei Wicklungen und 180°‐Umlenkungen der Arbeitsgruppe Prof. Röder, Hochschule Mannheim ; e) CFI in Zickzack‐Aufbau für eine Kühlungskristallisation , ; f) Glasreaktor in CFI‐Design , , g) modularer Aufbau eines CFI in Kastenform .…”

Flow chemistry—Microreaction technology comes of age

“…Liquid–liquid extraction is particularly useful as it consumes less energy and requires lower temperatures than distillation. Mixer settlers and columns can provide a high number of equilibrium stages, but designs capable of handling small volumes are rare due to the presence of complex moving parts . Conventional gravity based liquid–liquid separation has been automated and implemented in small scale .…”

Continuous Downstream Processing of Amino Acids in a Modular Miniplant

“…Considering downstream processes in the fine‐chemical and pharmaceutical industry, crystallization from solution and subsequent solid/liquid (SL) separation are common unit operations for purification and final product isolation . Hence, slurry and solids handling become crucial when dealing with continuous processing of such products , .…”