Characterization and scale-up of transport phenomena in miniaturized, stirred-pulsed extraction columns

液-液萃取是最重要的分离过程之一，并且在处理复杂混合物（例如来自生物技术生产过程）中获得重要性。工艺工程师拥有大量现有的设备，这些设备在过去几十年中没有进一步发展。研究活动主要集中在流体动力学，传质，以及在已知和现有设备的建模改进。为了设计萃取柱，诸如分散、聚结和返混的工艺参数是重要的，并且必须在针对每个物理化学系统的广泛的中试工厂实验中确定。最近开发的小型化和搅拌脉冲萃取柱（公称直径15 mm，DN 15）的分离性能几乎是传统搅拌柱的两倍。然而，在强化塔中的传输现象的一些细节还没有得到很好的理解，以转移的高性能到更大的塔。本研究项目的目的是获得更好的理解，如停留时间，传质，和分离性能在不同直径的塔（DN 15，32和50）的重要现象。除了标准化的测试系统（EFCE系统甲苯/丙酮/水和乙酸正丁酯/丙酮/水）外，具有不同内部构件的色谱柱将通过分离复杂混合物（对映异构体和异构体）来表征。利用这些结果，可以在从实验室到中试规模的不同规模上开发和操作强化萃取塔。在该项目内，应实现三个主要目标：i）改进对在各种脉动模式下搅拌脉冲萃取柱中的传输现象的理解（振幅、频率和相移）、内部构件和搅拌器速度，ii）在不同搅拌器和板几何形状和脉动、搅拌器速度、负载和化学系统的变化下的分离性能的表征和建模，以及在具有适当分散和脉动的柱内的调节的停留时间，iii）将结果转移到内径为32 mm的较大色谱柱并进行测试/验证（小型工厂）和50 mm内径（中试规模），并将自己的数据与列日和凯泽斯滕的数据进行比较。该项目的上级目标是提高对小型化搅拌脉冲萃取柱的理解，该萃取柱具有优化的搅拌单元尺寸和几何形状以及脉动和搅拌器速度。高分离性能和可调节的可转移性，长停留时间允许液-液萃取的新应用。因此，可以预期萃取柱更广泛应用的新动力以及现有和已安装设备的新机会。

Liquid-liquid extraction is one of the most important separation process and gains importance in the treatment of complex mixtures e.g. from biotechnology production processes. The process engineer has a multitude of existing apparatuses, which were not further developed in the last decades. Research activities are focused on fluid dynamics, mass Transfer, and modeling improvements in known and existing equipment. To design an extraction column, process parameters such as dispersion, coalescence, and back mixing are important and have to be determined in extensive pilot plant experiments for each physico-chemical system. The recently developed, miniaturized, and stirred-pulsed extraction column (nominal diameter 15 mm, DN15) has nearly twice as high separation performance compared to conventional stirred columns. However, some details of transport phenomena in the intensified column are not well understood to transfer the high performance to larger columns.This research project aims to gain a better understanding for important phenomena such as residence time, mass transfer, and separation performance in columns with different diameters (DN15, 32 and 50). Beside standardized test systems (EFCE-systems toluene/acetone/water and n-butyl acetate/acetone/water) the columns with different internals will be characterized by separation of complex mixtures (enantiomers and saccharides). With these results intensified extraction columns can be developed and operated on different scales from laboratory to pilot scale. Within the project three major goals should be achieved:i) the improved understanding of transport phenomena in the stirred-pulsed extraction column under various pulsation modes (amplitude, frequency, and phase shift), internals, and stirrer speed, ii) the characterization and modeling of the separation performance under different stirrer and plate geometries and variation of pulsation, stirrer speed, loading, and chemical systems, as well as adjusted residence times within the column with appropriate dispersion and pulsation,iii) the transfer and testing/validation of the results to larger columns with 32 mm inner diameter (miniplant) and 50 mm inner diameter (pilot scale) together with comparison of own data with them of groups in Liège and Kaiserslautern. Superior goal of the project is the improved understanding of the miniaturized, stirred-pulsed extraction column with optimized stirred cell size and geometry together with pulsation and stirrer speed. The transferability of the high separation performance and adjustable, long residence time allow for new applications of liquid-liquid extraction. Hence, new momentum for wider application of extraction columns can be expected as well as new opportunities for existing and installed equipment.