PREDICTION OF MASS TRANSFER COEFFICIENTS IN REGULAR PACKED COLUMNS

Developments in the area of packed columns, particularly structured packed columns, are ongoing, specifically in the area of liquid-liquid extractions. Accurate predictions of mass transfer coefficients lead to more accurate design of columns. In the present study, mass transfer coefficients were measured experimentally for packed columns of different heights to study the effect of packing height and specific area. Two experimental pilot regular packed extraction columns were examined using toluene/acetic acid/water and n-butyl acetate/acetic acid/water systems. Based on the results, a novel model for prediction of effective diffusivity has been proposed that is a function of column height and specific area. The mass transfer coefficients obtained by this prediction were compared with other models. The results of this new model are in good agreement with the experimental data. Therefore, this new model can be used to design better regular packed columns.     

CONTROL OF A PULSED LIQUID-LIQUID EXTRACTION COLUMN BASED ON A MULTILEVEL SYSTEM OF AUTOMATA

This paper presents the real-time application of the learning control theory to the control of a chemical pilot plant: a pulsed liquid-liquid extraction column.

The behaviour of an agitated liquid-liquid extraction column can be related to random mechanisms such as the phenomena of droplets breakage and coalescence. Previous studies on hydrodynamic and mass transfer aspects showed that a pulsed liquid-liquid extraction column had an optimal behaviour for operating conditions close to flooding. These results led to choose the following strategy to control the column in its optimal behaviour zone:

- the measure of the conductivity of the liquid medium below the distributor which gives a good information about flooding, is the controlled variable

-the pulse frequency is the control action.

The learning control algorithm is based on a multilevel system of automata which operates in a random environment. By means of an evaluation unit of the performances of the column which generates either penalty (inaction) or reward on the basis of heuristic rules, the automaton chooses a value of the pulse frequency. This approach is essentially connected to artificial intelligence in so far as human knowledge on the plant is included in these rules.

This algorithm has been implemented on a microcomputer for control purposes. The experimental results presented show the good performances of the approach.     

Liquid-liquid extraction in a reciprocating screen plate column

A novel reciprocating-plate liquid-liquid extraction column is proposed. It features a simple design that utilizes as the plates mesh screens with a fractional free area larger than 64%. A hydrodynamic and mass transfer study of the column was carried out in which the existence of a uniform liquid-liquid dispersion throughout the column at relatively low speeds of plate reciprocation was confirmed. Experimental results show that in comparison with other reciprocating columns, the present column has these desirable qualities: (1) large dispersed phase holdup and overall mass transfer coefficient, (2) low power requirements, (3) high flow capacity. A correlation of the dispersed phase holdup data based on slip and drop characteristic velocities is presented. The drop characteristic velocity for the screen plate column is empirically related to the power dissipation rate and system properties. On propose une nouvelle colonne d'extraction liquide-liquide munie de plateaux réciproques. Il s'agit d'une conception simple qui utilise comme plateaux des tamis à mailles avec une zone libre fractionnelle supérieure à 64%.     

萃取塔数学模型及过程强化的若干研究进展

萃取塔因生产能力大、占地面积小、密闭性好等优点，在石油、化工、生物、医药和环境工程等多领域被广泛应用。本文从以下几个方面介绍了萃取塔近些年的研究进展：综述了传统萃取塔（脉冲萃取塔、转盘塔与Kühni塔等）的水力学、轴向扩散与传质模型的发展，分析比较了表面张力、传质方向、放大效应等因素对模型的影响；介绍了计算流体动力学（CFD）在萃取塔中单液滴、单相流模拟、液-液两相流模拟、外加能量模拟、与群体平衡模型（PBM）耦合模拟中的应用进展；介绍了国内外设计开发的新型萃取塔，包括改变传统塔的内构件和引入多种外场能量等方式来强化相间传质。研究表明，将先进实验研究方法、准确经验模型和可靠理论计算相结合，将会是萃取塔研究的重要手段和方向。     

THE RECIPROCATING PLATE COLUMN—DEVELOPMENT AND APPLICATIONS

Reciprocating plate columns (RPCs) were first proposed in 1935 but most of the development has occurred in the past 30 years. Three types of RPC are in use in industry for liquid-liquid extraction, in diameters up to about 1·5  m: The Karr column (U.S.A. and Europe), the VPE column (Eastern Europe) and the vaned-perforation plate (KRIMZ and GIAP) columns developed in the U.S.S.R. All types of RPC operate on common principles, but their design characteristics differ, and basic knowledge must be supplemented by engineering tests with the system of interest. The RPC appears to have promise as a gas-liquid contactor and recent research has suggested possible design modifications for this application.     

An application of a cascaded self tuning regulator to a karr solvent extraction column

An application of a cascaded Clarke-Gawthrop self tuning regulator (STR) to a Karr liquid-liquid solvent extraction column is presented. The Karr column, a reciprocating plate column, exhibits nonlinear asymmetric responses which are complex functions of the operating conditions and requires adaptive control in order to prevent instability. The outer loop of this cascade scheme controls the extract concentration of the continuous phase while the inner loop controls the hydrodynamic holdup in the column and prevents flooding. The manipulated variable was the frequency of reciprocation. The STR-STR cascade arrangement is compared with a fixed parameter Proportional plus Integral (PI) controller in the outer loop and an STR in the inner loop.     

Zum Flutpunkt in Flüssig/Flüssig-Gegenstromkolonnen

Flooding point of liquid-liquid countercurrent columns . Calculation of the column diameter for given volumetric flow rates of the raffinate and the extract phases requires a knowledge of the flooding point. A simple flooding point diagram is presented which contains the rise or fall rate of an individual drop as intermediate quantity. The principal experimental results from the literature obtained in countercurrent columns with and without introduction of energy by rotation and pulsation are compared with the flooding point diagram.     

Efficient Shortcut Method for Determining the Process Window in Stirred-Pulsed Extraction Columns

Recent studies showed the superior separation performance of stirred-pulsed columns of different diameters in liquid-liquid extraction processes. Here, an efficient shortcut method will be presented, which is time and resource-efficient as well as cost-effective to determine the operational window of these columns for industrial separation tasks. Savings in time of less experiments and costs of materials consumption can be estimated with up to 30 %. The presented method is particularly suitable before the application of new chemical systems, which are particularly cost-intensive and scarce in material supply.     

填料特性对鼓泡填料萃取塔性能影响

填料的结构与表面性能对鼓泡填料萃取塔性能有直接影响。利用空气 煤油 (苯甲酸 ) 水体系 ,测定了未装填料和分别装填板波填料、丝网填料、压延孔环填料的鼓泡萃取塔水力学性能和传质性能。实验表明 ,对未装填料和装有填料的萃取塔 ,气相搅拌都可以显著提高液液两相的接触与传质性能 ;液泛速度随表观气速的增大而下降 ;流道设计合理的规整填料传质性能明显高于散装填料 ;表面光滑的填料分散相滞存率低 ,因而液泛速度较高 ;填料的作用有利于降低轴向返混 ,明显提高萃取塔传质性能。     

GRAVITY SETTLING OF DISPERSED PHASE DROP SWARMS IN EXTRACTION COLUMNS IN ABSENCE OF MASS TRANSFER

Taking into account the effect of velocity profiles of the continuous phase in interstices of drops,dragcoefficient and relative motion correlations for dispersed liquid-liquid two-phase flow in absence of mass transferwere developed in terms of the pseudo-fluid concept based on the simple similarity criteria and the mixtureviscosity model suggested by Ishii and Zuber.The present model was compared with the experimental data fromfive(different sources and also with seven other pertinent correlations available in literature.Fairly goodpredictions were obtained under wide ranges of the dispersed phase holdup and Reynolds number.The validity ofthe present model has also been checked against the experimental slip velocity data and holdup data obtained ina Karr reciprocating plate extraction column by the author of the present paper and satisfactory agreement isachieved、The results show that the equations of the motion of a multi-droplet system can be formulated in aform identical with those for a single dr     

气体搅动的筛板萃取塔性能实验研究

在筛板萃取塔中引入气体搅动,既能明显提高装置的传质效率,又能大幅提高装置处理能力。筛板塔的通量随气速的变化规律与填料塔有显著区别,其性能研究有重要意义。利用煤油(苯甲酸)-水-空气体系,考察了气体搅动和筛孔直径对萃取塔流体力学和传质性能的影响。结果表明,随着表观气速的增加,气含率、分散相含率、液泛速率和传质效率均明显增加。但过高的气速也会导致分散相的过于分散和乳化,传质性能下降,直至液泛。不同直径的筛孔相比,较小的筛孔使分散相停留时间延长,分散相含率和传质效率提高,但液泛速率和处理能力降低。     

空气搅动的填料萃取塔性能实验研究

引　言气体搅动是一种外加能量的萃取方法 .与机械搅拌相比 ,气体搅动的萃取塔内无运动部件 ,操作稳定 ,结构简单 ,能耗低 .过去已有数篇关于气体搅动的混合 -澄清槽[1] 、喷洒塔[2～ 4 ] 、多级连续萃取器[5] 等无填料的萃取过程水力学性能和传质性能的文献报道 .而在填料塔萃取过程中加入气体搅动技术 ,一方面继承了填料可以有效地降低轴向返混的优越性能 ;另一方面 ,通过外加能量进一步强化液 -液两相接触与传质 ,提高传质系数 ,综合了外加能量的萃取技术和填料萃取技术的优点 .关于这方面的内容目前少有报道[6] .1　实验装置与实验方法…     

Performance Map for the Design of Liquid‐Liquid Extraction Columns

For the fast approximation of liquid‐liquid extraction column designs via HETS (height equivalent of a theoretical stage) values and flooding points, a population balance model was developed. The model requires only one pilot‐scale column experiment to fit a coalescence parameter. The comparison of experimental data with simulations shows good agreement for a stirred extraction column. With the model, the operation domain of the column is simulated and visualized in a performance map, showing the holdup, the distance to the flooding point and HETS values.     

Modelling of liquid-liquid extraction columns: Use of published model correlations in design

Design of several liquid-liquid extraction columns — packed, pulsed-packed, pulsed-plate, Oldshue-Rushton columns and the rotating disc contactor — was attempted utilizing available correlations for drop size, holdup of dispersed phase, flooding velocities, mass transfer coefficients and axial mixing coefficients. Correlations in many cases were vaguely defined and often based on very limited data. Results indicated that for given flow rates and extraction efficiency, the height of a packed or Oldshue-Rushton column must be considerably greater than the predicted minimum heights of the other three columns, which were comparable considering the limited data utilized in the developed correlations. A critical evaluation of the correlations should be carried out to guide the further experimental effort required to confirm the utility of the axial dispersion model in liquid-liquid extraction column design. Extension of the theory to include drop size variation is highly desirable.     

萃取柱内液-液两相流CFD-PBM模拟研究进展

对萃取柱内CFD-PBM模拟研究进行了较详细的综述,包括其基本理论、不同的求解方法及模拟研究现状等. CFD-PBM模拟的基本方程包括流动方程和群体平衡方程,其相互耦合,群体平衡方程涉及破碎与聚并2个关键模型. 群体平衡模型的求解方法包括直接离散化方法、矩量法、正交矩量法、直接正交矩量法、分段正交矩量法等,对这些方法的原理、优点和缺点进行了综述. 目前国际上关于萃取柱内CFD模拟采用较多的是简单的欧拉-欧拉两相流模拟,考虑液滴尺寸分布和进一步的浓度分布的群体平衡模型应用较少. 完善伴随传质的液-液分散体系的群体平衡模型,并将其应用于不同类型的萃取柱中,是萃取分离学科的重要任务.     

Flow phenomena and flooding limitations in a phase transition extraction column

The flooding limitations of liquid-liquid countercurrent two-phase flow in a phase transition extraction (PTE) column were investigated both experimentally and theoretically. The solvents used in the PTE process are partially miscible and posses a critical point of miscibility. In the experiments, the effect of the settlers’ inclination on the onset of flooding in non-isothermal PTE column was investigated. It was found that flooding conditions in the column can be postponed by using off-horizontal settlers. This led to the development of a novel structure of a PTE column with improved throughputs.A model is suggested for predicting flooding conditions in the PTE column. It combines a recently developed two-fluid model with improved theory-based closure relations for laminar stratified flow, with a non-isothermal model for evaluating the composition in the mixing section and the internal streams in the column. The results of the combined model favorably predict the experimental flooding flow rates.     

Simulation of hydrodynamics in RDC extraction columns using the simulation tool “ReDrop”

ReDrop is a simulation tool which can predict the behaviour of pulsed extraction columns on pilot-plant scale. Because it follows a certain number of drops during their entire lifetime in an extraction column, it can be seen as a Monte-Carlo solution of drop-population balances. ReDrop is based on single-drop models which have system-specific parameters. These parameters are determined from lab-scale experiments with single drops. In this study, ReDrop is extended to RDC extraction columns and simulations are carried out for the standard test systems toluene (d) + water (c) + acetone (c → d) and n-butyl acetate (d) + water (c). The calculated hold-up and Sauter mean diameter show good agreement with the experimental data obtained in pilot-plant scale experiments.     

STUDIES ON FLOODING POINT AND HOLD-UP IN A SOLVENT EXTRACTION COLUMN WITH RECIPROCATING SIEVE PLATES

The flooding point and hold-up of the dispersed phase in an extraction column with reciprocating-sieve plates of 32 mm inside diameter and 1960 mm effective column height have been investigated under thefollowing conditions:Percent perforation of the plates 40%,53.5% and 63.7%,diameters of perforatedholes 7.8,9.0 and 9.8 mm,and distances between plates 20 and 40 mm respectively.Experiments werecarried out with three different liquid-liquid systems covering a rather wide range of physical properties.The relative velocity of the two phases passing through the perforations of the plates is consideredin the present work to be related to the work done by the oscillating plates in the column on unit massof liquid in unit time.Therefore the flooding velocity and hold-up in extraction column with reci-procating sieve plates should be related to A~2F~3 instead of AF as reported before.Equations weredeveloped to correlate the experimental data of flooding point and hold-up respectively.