Abstract

A recently developed continuous enantioseparation process utilizing two coupled fluidized bed crystallizers is systematically investigated to identify essential correlations between different operation parameters and the corresponding process performance on the example of asparagine monohydrate. Based on liquid phase composition and product crystal size distribution data, it is proven that steady state operation is achieved reproducibly in a relatively short time. The process outputs at steady state are compared for different feed flow rates, supersaturations, and crystallization temperatures. It is shown that purities >97% are achieved with productivities up to 40 g/L/h. The size distribution, which depends almost exclusively on the liquid flow rate, can be easily adjusted between 260 and 330 µm (mean size) with an almost constant standard deviation of ±55 µm.

Highlights

  • Continuous crystallization has again become the focus of many research activities.Efforts have been made to develop design rules based on comparing it with the corresponding batch process [1,2] or to elucidate basic mechanisms, for example, the impurity incorporation and carryover [3]

  • Based on liquid phase composition and product crystal size distribution data, it is proven that steady state operation is achieved reproducibly in a relatively short time

  • Novel concepts, applying to example slug-flow [4], oscillatory baffled [5,6], Couette-Taylor [7,8] or fluidized bed crystallizers [9,10,11,12], as well as columns with static mixers [1] or coiled flow inverters [13], have been developed lately. These concepts exploiting tubular crystallizers in general are not superior nor applicable for every substance system or separation problem. They have specific benefits and drawbacks [1] compared to the well-known mixed-suspension, mixed-product removal (MSMPR) concept but have given new input to the topic of continuous crystallization and have widened the field of application for the food, agriculture, and pharmaceutical industries

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Summary

Introduction

Continuous crystallization has again become the focus of many research activities.Efforts have been made to develop design rules based on comparing it with the corresponding batch process [1,2] or to elucidate basic mechanisms, for example, the impurity incorporation and carryover [3]. Novel concepts, applying to example slug-flow [4], oscillatory baffled [5,6], Couette-Taylor [7,8] or fluidized bed crystallizers [9,10,11,12], as well as columns with static mixers [1] or coiled flow inverters [13], have been developed lately. These concepts exploiting tubular crystallizers in general are not superior nor applicable for every substance system or separation problem. All of these studies aimed at a full conversion of the pollutant ions in the liquid phase to form a salt and utilized afterward the surface of fluidized, inert particles to collect the fine precipitate

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