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Extractive Distillation: Recent Advances in Operation Strategies Open Archive TOULOUSE Archive Ouverte ( OATAO ) OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible. This is an author-deposited version published in : http://oatao.univ-toulouse.fr/ Eprints ID : 15857 To link to this article : DOI : 10.1515/revce-2014-0031 URL : https://www.degruyter.com/view/j/revce.2015.31.issue-1/revce-2014-0031/revce-2014-0031.xml To cite this version : Shen, Weifeng and Benyounes, Hassiba and Gerbaud, Vincent Extractive distillation: recent advances in operation strategies . (2014) Reviews in Chemical Engineering, vol. 31 (n° 1). pp. 13-26. ISSN 0167-8299 Any correspondence concerning this service should be sent to the repository administrator: [email protected] Weifeng Shen , Hassiba Benyounes and Vincent Gerbaud * Extractive distillation: recent advances in operation strategies Abstract : Extractive distillation is one of the efficient 1 Introduction techniques for separating azeotropic and low-relative- volatility mixtures in various chemical industries. This In most separation systems, the predominant nonideality paper first provides an overview of thermodynamic occurs in the liquid phase because of molecular interac- insight covering residue curve map analysis, the appli- tions. Azeotropic and low-relative-volatility mixtures are cation of univolatility and unidistribution curves, and often present in the separating industry, and their sepa- thermodynamic feasibility study. The pinch-point anal- ration cannot be realized by conventional distillation. ysis method combining bifurcation shortcut presents Extractive distillation is then a suitable widely used tech- another branch of study, and several achievements have nique for separating azeotropic and low-relative-volatility been realized by the identification of possible product cut mixtures in the pharmaceutical and chemical industries. under the following key parameters: reflux ratio, reboil Given an azeotropic mixture A-B (with A having a lower ratio, and entrainer-feed flow rate ratio. Process opera- boiling temperature than B does), an entrainer E is added tion policies and strategy concerning batch extractive to interact selectively with the original components and distillation processes are summarized in four operation alter their relative volatility, thus enhancing the original steps. Several configurations and technological alterna- separation. Extractive distillation differs from azeotropic tives can be used when extractive distillation processes distillation by the fact that the third-body solvent E is fed take place in a continuous or batch column, depending continuously in another column position than the feed on the strategy selected for the recycle streams and for mixture. Extractive distillation has been studied for many the main azeotropic feeds. decades, with a rich body of literature. Some main sub- jects studied include column with all possible configu- Keywords: batch; bifurcation theory; continuous; extrac- rations; process operation polices and strategy; process tive distillation; operation strategies; thermodynamic design, synthesis, and optimization; determination of analysis. separation sequencing; entrainer design and selection; feasibility studies; and so on. Among these topics, feasi- DOI 10.1515/revce-2014-0031 bility is always a critical issue, as it is necessary to assess process feasibility before making design specifications. Feasibility studies also contribute to a better understand- ing of complex unit operations such as batch extractive distillation (BED). 2 Thermodynamic topologic *Corresponding author: Vincent Gerbaud, Universit é de Toulouse, insights INP, UPS, LGC (Laboratoire de G é nie Chimique), 4 all é e Emile Monso, F-31432 Toulouse Cedex 04, France, e-mail: [email protected]; and CNRS, LGC (Laboratoire The design of distillation processes is connected to thermo- de G é nie Chimique), F-31432 Toulouse Cedex 04, France dynamics, in particular to the boiling point of each com- Weifeng Shen: Universit é de Toulouse, INP, UPS, LGC (Laboratoire pound and azeotrope. The initial feasibility study relates de G é nie Chimique), 4 all é e Emile Monso, F-31432 Toulouse Cedex to well-known design tools: residue curve map (RCM) 04, France ; CNRS, LGC (Laboratoire de G é nie Chimique), F-31432 analysis and liquid phase diagrams, since they represent Toulouse Cedex 04, France ; and Chemical and Biomolecular Engineering, Clarkson University, Potsdam, NY, USA close approximations to actual equilibrium behavior and Hassiba Benyounes: U.S.T. Oran, Laboratoire de Chimie Physique can be used to predict composition changes in separation des Mat é riaux, Catalyse et Environnement, Oran, Alg é rie processes under infinite reflux ratio conditions. 2.1 Residue curve map offering a visual representation over the whole compo- sition space and assisting the engineer to detect separa- The RCM technique is considered as a powerful tool for tion constraints. Pham and Doherty (1990) conducted an flow-sheet development and preliminary design of con- RCM analysis for ternary heterogeneous mixtures to aid ventional multicomponent separation processes. RCM is in the sequencing of heterogeneous distillation columns. a collection of the liquid residue curves in a simple one- However, distillation runs under finite reflux ratio (reboil stage batch distillation originating from different initial ratio in reverse extractive distillation) conditions, to compositions. Using the theory of differential equations, determine which products are achievable and the loca- the study of the topological properties of RCMs is summa- tion of the suitable feed composition region, are more rized in two published articles ( Hilmen et al. 2003 , Kiva complicated ( Wahnschafft et al. 1992 , Poellmann and et al. 2003 ). The simple RCM was modeled by the follow- Blass 1994 ) because the dependency of the composition ing differential equation: profile on the reflux ratio (reboil ratio) needs to be con- dx sidered. This affects the range of composition available * i =x -y (1) to each section profiles due to the occurrence of pinch dh i i points, which differ from the singular points of the RCM ( Doherty and Caldarola 1985 , Levy et al. 1985 , Bausa et al. where h is a dimensionless time describing the relative 1998 , Urdaneta et al. 2002 ). loss of the liquid in the still-pot, x i is the mole fraction of species i in the liquid phase, and y i is the mole fraction of species i in the vapor phase. The y values are related with i 2.2 Unidistribution curve and relative the xi values using equilibrium constant Ki . The singular points of the differential equation are checked by comput- volatility ing the associated eigenvalues. Within a nonreactive RCM, The distribution coefficient and relative volatility are well- a singular point can be a stable or an unstable node or a known characteristics of the vapor-liquid equilibrium. saddle, depending on the sign of the eigenvalues related The distribution coefficient K is defined by: to the residue curve equation. For nonreactive mixtures, i there are three stabilities: unstable node, stable node, and y i K = (2) saddle point ( Figure 1 A). The residue curves move away i x i from the unstable node to the stable node with increas- ing temperatures. Some residue curves move away from Ki characterizes the distribution of component i between = a saddle point with decreasing temperatures, and others, the vapor and liquid phases in equilibrium. Ki 1 defines with increasing temperatures (Figure 1B). the unidistribution curve. The vapor is enriched with com- > A past review article ( Fien and Liu 1994 ) presented ponent i if Ki 1 and is impoverished with component i if < the use of ternary diagrams including RCMs for feasibil- Ki 1 compared to the liquid. The higher the Ki , the greater ity analysis, flow sheet development, and preliminary the driving force (yi -xi ) is given and the easier the distil- design of both homogeneous and heterogeneous azeo- lation will be. The ratio of the distribution coefficient of tropic system separation processes. RCMs of reactive components i and j gives the relative volatility. The relative and extractive distillation units were used by Jim é nez volatility is a very convenient measure of the ease or dif- et al. (2001) for a simultaneous analysis. This graphical ficulty of separation in distillation. The volatility of com- technique reveals the sensitivity of design options by ponent i relative to component j is defined as A B B [Srcm]50°C Residue Tmin azeoAB curve [UNrcm]30°C Stable node Unstable node Saddle E (heavy) A [SNrcm]60°C [Srcm ]40°C Figure 1 Features of (A) singular point and (B) RCM. y / x α = i i (3) ij y / x j j The relative volatility characterizes the ability of com- ponent i to transfer (evaporate) into the vapor phase com- pared to the ability of component j. Component i is more α > α < volatile than component j if ij 1 and less volatile if ij 1. For ideal and nearly ideal mixtures, the relative volatili- ties for all pairs of components are nearly constant in the whole composition space. The situation is different for nonideal and in particular azeotropic mixtures where the composition dependence can be complex. Unidistribution and univolatility line diagrams can be used to sketch the VLE (vapor–liquid equilibrium) dia- grams and represent the topologic features of the simple phase transformation trajectories. The qualitative char- acteristics of the distribution
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