ISBN 978-3-8439-0982-2

978-3-8439-0982-2, Reihe Verfahrenstechnik

Elisabeth Anna Hopmann
Development of a Centrifugal Partition Chromatographic Separation: from Molecule to Process

133 Seiten, Dissertation Universität Erlangen-Nürnberg (2013), Softcover, A5

Zusammenfassung / Abstract

This work presents new guidelines for the development of a continuous centrifugal partition chromatographic (CPC) separation. CPC is a support-free liquid chromatographic technique in which the mobile and the stationary phases are liquid. This work is divided into two parts.

The first part focuses on the thermodynamics and the selection of the biphasic solvent system (i.e. the mobile and stationary phase) and the second part covers the process level of the technology and focuses on the selection of the operating parameters of a continuous CPC unit.

In the first part, the a-priori conductor-like screening model for real solvents (COSMO-RS) is used for the first time to select a suitable biphasic solvent system in CPC. Furthermore, COSMO-RS is implemented in a general approach for the selection of the most appropriate biphasic solvent systems for a particular separation task. Besides the partition coefficient, the approach includes further selection criteria relevant for preparative applications such as: sample solubility, physical properties of the solvent system, environmental and economic considerations. The advantage of the presented systematic approach is the minimization of the experimental effort normally needed to select solvent systems and the potential of the development of possible new solvent systems by the incorporation of alternative solvents. Moreover, the use of an ionic liquid based biphasic solvent system, alcohol/[EMIM][NTf2]/water, as alternative solvent system is investigated.

The second part of this thesis deals with a novel continuous cyclic liquid-liquid chromatographic separation technology called sequential centrifugal partition chromatography (sCPC). The concept of sCPC is proven experimentally in the first commercially available sCPC unit. A procedure for the selection of the sCPC unit operating parameters for the theoretically complete separation of a binary feed mixture is presented. Additionally, the sCPC process is modeled successfully using the stage model and operating parameter studies are performed by experiments and simulation to analyze the separation performances. A general scheme for optimization of the unit operating parameters is presented including the proposed procedure for the selection of the unit operating parameters and process simulations. The sCPC process could be of high value for purification/fractionation of natural products.