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A study of the hydrodynamic and mass transfer performance for Karr reciprocating plate extraction columns has been presented for a range of operating conditions and column diameters of 50, 100, and 450 mm. Although the use of Karr columns has been widespread for many years for a range of important applications, the need for more reliable methods for predicting the performance and scale-up of such columns continues to be a matter of significant importance. The present study has examined the hydrodynamic performance in terms of the dispersed phase hold up and droplet size distribution and mass transfer performance which has incorporated the effects of backmixing in the continuous phase. Work was initially carried out in a 50 mm diameter laboratory scale Karr column using the system 10 v/v% tributyl phosphate/kerosene (continuous)−phenol−water (dispersed) where hydrodynamic and mass transfer performance was analyzed for both directions of mass transfer. Using these data, models were investigated and developed to predict performance over a range of operating conditions. An alternative system consisting of an organic solvent (continuous)−phenolic alkaloid−aqueous caustic (dispersed) was also studied, using both 100 and 450 mm diameter Karr columns. These data were used to validate the hydrodynamic and mass transfer performance models developed for the phenol system in the 50 mm diameter column. Dispersed phase holdup data were found to fit the correlation presented by Kumar and Hartland [Ind. Eng. Chem. Res. 1995, 34, 3925−3940], and the drop size distribution also agreed with the relationship presented by Kumar and Hartland [Ind. Eng. Chem. Res. 1996, 35, 2682−2695] within reasonable accuracy. The mass transfer performance results indicated that the continuous phase controlled the mass transfer rate, and thus, column design was simplified by assuming that the overall mass transfer coefficient can be obtained using a standard mass transfer correlation for the continuous phase. The current mass transfer results were found to be best predicted by a refitted form of the overall mass transfer coefficient correlation developed by Harikrishnan et al. [Chem. Eng. J. 1994, 54, 7−16].