Separation of chiral mixtures in real SMB units: The FlexSMB-LSRE®

Authors

  • Pedro Sá Gomes,

    1. Laboratory of Separation and Reaction Engineering, Associate Laboratory LSRE/LCM, Dept. of Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal
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  • Miriam Zabkova,

    1. Laboratory of Separation and Reaction Engineering, Associate Laboratory LSRE/LCM, Dept. of Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal
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  • Michal Zabka,

    1. Laboratory of Separation and Reaction Engineering, Associate Laboratory LSRE/LCM, Dept. of Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal
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  • Mirjana Minceva,

    1. Laboratory of Separation and Reaction Engineering, Associate Laboratory LSRE/LCM, Dept. of Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal
    Current affiliation:
    1. Lehrstuhl für Thermische Verfahrenstechnik der Universität Erlangen-Nürnberg, Egerlandstr. 3, D-91058 Erlangen, Germany
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  • Alírio. E. Rodrigues

    Corresponding author
    1. Laboratory of Separation and Reaction Engineering, Associate Laboratory LSRE/LCM, Dept. of Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal
    • Laboratory of Separation and Reaction Engineering, Associate Laboratory LSRE/LCM, Dept. of Chemical Engineering, Faculty of Engineering, University of Porto, Rua Dr. Roberto Frias, 4200-465 Porto, Portugal
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Abstract

In this work, a procedure for the separation of a racemic mixture of guaifenesin onto a chiral stationary phase (Chiralpak AD), by means of Simulated Moving Bed (SMB) technology, is presented in four major steps: (1) search for the suitable stationary and mobile phases; (2) determination of sorption parameters and validation by frontal analysis; (3) modeling and design of the SMB unit; and (4) operation and demonstration. A major emphasis is given to the common deviations that “real” SMB units present when compared with the theoretical apparatus (due to tubing and equipment dead volumes, switching time asymmetries and delays, pumps flow rates variations). These deviations are analyzed before and after the design and construction of the FlexSMB-LSRE® unit, a new flexible unit, hereby presented. A detailed model that takes into account tubing and equipment dead volumes, as well as switching time asymmetries and delay, was used to study and compare different dead volumes design and compensating strategies. It is shown that all these approaches can be converged into a switching time compensating strategy. This approach served to predict the experimental operating conditions and run a classical SMB experiment, which afterwards was compared with the simulated profiles obtained for the FlexSMB-LSRE® unit. The result of the separation was guaifenesin enantiomers with purities above 98% and a productivity value of 23 genantiomer/(dm3 CSP day). © 2009 American Institute of Chemical Engineers AIChE J, 2010

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