Extending Batch Extractive Distillation Thermodynamic Feasibility Insights to Continuous for Class 1.0-2 Case A

The feasibility of batch and continuous extractive distillation analysis for the separation azeotropic mixtures is addressed. Based on batch feasibility knowledge, batch and continuous separation feasibility is studied under reflux ratio and entrainer flow-rate for a working example ternary system acetone-chloroform-benzene, which belonging to the 1.0-2 class case (a). Possible feasible regions are determined by finding the feasible points based on continuous methodology, they show minimum and maximum feed ratio as a function of the reflux, and a lower bound for the reflux ratio. Later on, simulations verified the feasibility of calculating results based on theoretical methodolog

From batch to continuous extractive distillation using thermodynamic insight: class 1.0-2 case B

A systematic feasibility analysis is presented for the separation azeotropic mixtures by batch and continuous extractive distillation. Based on batch feasibility knowledge, batch and continuous separation feasibility is studied under reflux ratio and entrainer flow-rate for the ternary system chloroform-vinyl acetate-butyl acetate, which belongs to the class 1.0-2 separating maximum boiling temperature azeotropes using a heavy entrainer. How information on feasibility of batch mode could be extended to the feasibility of continuous mode is then studied, possible feasible regions are determined by finding the feasible points based on continuous methodology, they show minimum and maximum feed ratio as a function of the reflux, and a lower bound for the reflux ratio. Results are validated by simulation

Extractive distillation: recent advances in operation strategies

Extractive distillation is one of the efficient techniques for separating azeotropic and low-relativevolatility mixtures in various chemical industries. This paper first provides an overview of thermodynamic insight covering residue curve map analysis, the application of univolatility and unidistribution curves, and thermodynamic feasibility study. The pinch-point analysis method combining bifurcation shortcut presents another branch of study, and several achievements have been realized by the identification of possible product cut under the following key parameters: reflux ratio, reboil ratio, and entrainer-feed flow rate ratio. Process operation policies and strategy concerning batch extractive distillation processes are summarized in four operation steps. Several configurations and technological alternatives can be used when extractive distillation processes take place in a continuous or batch column, depending on the strategy selected for the recycle streams and for the main azeotropic feeds

Extension of thermodynamic insights on batch extractive distillation to continuous operation

Nous étudions la faisabilité du procédé de distillation extractive continue pour séparer des mélanges azéotropiques A-B à température de bulle minimale ou maximale, avec un tiers corps E lourd ou léger. Les mélanges ternaires A-B-E appartiennent aux classes 1.0-1-a et 1.0-2 qui se subdivisent chacune en deux souscas selon la position de la courbe d'univolatilité. La colonne de distillation a trois sections, rectification, extractive, épuisement. Nous établissons les équations décrivant les profiles de composition liquide dans chaque section en fonction des paramètres opératoires: pureté et taux de récupération du distillat, taux de reflux ratio R et rapport des débits d'alimentation FE/F dans le cas d'un tiers corps lourd ; pureté et taux de récupération du produit de pied, taux de rebouillage S et rapport des débits d'alimentation FE/F dans le cas d'un tiers corps léger. Avec un tiers corps lourd alimenté comme liquide bouillant au dessus de l'étage d'alimentation du mélange A-B, nous identifions le distillat atteignable et les plages de valeurs faisables des paramètres R et FE/F à partir du critère général de faisabilité énoncé par Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2009, 48(7), 3544–3559). Pour la classe 1.0-1a, il existe des rapport FE/F et reflux ratio minimum. Le rapport FE/F est plus important pour le procédé continu que pour le procédé discontinu parce que la faisabilité du procédé continu nécessite que les profils d'épuisement et extractifs s'intersectent. Pour la classe 1.0-2, les deux constituants A et B sont des distillats potentiels, l'un sous réserve que le rapport FE/F reste inférieur à une valeur limite maximale. Le procédé continu exhibe également une valeur minimale de FE/F à un taux de reflux ratio donné, contrairement au procédé discontinu. Avec un tiers corps léger alimenté comme vapeur saturante sous l'étage d'alimentation du mélange A-B, nous identifions le produit de pied atteignable et les plages de valeurs faisables des paramètres S et FE/F à partir du critère général de faisabilité énoncé par Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2012, 51, 4643–4660). Comparé au cas des tiers corps lourds, le produit principal est obtenu en pied. Autrement, les comportements des classes 1.0-1a et 1.0-2 sont analogues entre les tiers corps léger et lourd. Avec un tiers corps léger, le procédé continu ajoute la contrainte que les profils de rectification et extractifs s'intersectent. La contrainte d'intersection des profils d'épuisement et extractif est partagée par les deux modes opératoires continu et discontinu. Ce travail valide la méthodologie proposée pour évaluer la faisabilité du procédé de distillation extractive continue et permet de comparer les tiers entre eux en termes de taux de reflux ratio minimum et de rapport de débit d'alimentation minimal. ABSTRACT : We study the continuous extractive distillation of minimum and maximum boiling azeotropic mixtures A-B with a heavy or a light entrainer E, intending to assess its feasibility based on thermodynamic insights. The ternary mixtures belong to the common 1.0-1a and 1.0-2 class ternary diagrams, each with two sub-cases depending on the univolatility line location. The column has three sections, rectifying, extractive and stripping. Differential equations are derived for each section composition, depending on operating parameters: distillate product purity and recovery, reflux ratio R and entrainer – feed flow rate ratio FE/F for the heavy case; bottom product purity and recovery, reboil ratio and entrainer – feed flow rate ratio for the light entrainer case. For the case with a heavy entrainer fed as a boiling liquid above the main feed, the feasible product and operating parameters R and FE/F ranges are assessed under infinite reflux ratio conditions by using the general feasibility criterion enounced by Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2009, 48(7), 3544–3559). For the 1.0-1a class, there exists a minimum entrainer - feed flow rate ratio to recover the product, and also a minimum reflux ratio. The minimum entrainer - feed flow rate ratio is higher for the continuous process than for the batch because of the additional requirement in continuous mode that the stripping profile intersects with the extractive profile. For the 1.0-2 class both A and B can be distillated. For one of them there exists a maximum entrainer - feed flow rate ratio. The continuous process also has a minimum entrainer - feed flow rate ratio limit for a given feasible reflux ratio. For the case with a light entrainer fed as saturated vapor below the main feed, the feasible product and operating parameters S and FE/F ranges are assessed under infinite reflux ratio conditions by using the general feasibility criterion enounced by Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2012, 51, 4643–4660), Compared to the heavy entrainer case, the main product is removed from the column bottom. Similar results are obtained for the 1.0-1a and 1.0-2 class mixtures whether the entrainer is light or heavy. With a light entrainer, the batch insight about the process feasibility holds for the stripping and extractive sections. Now, an additional constraint in continuous mode comes from the necessary intersection between the rectifying and the extractive sections. This work validates the proposed methodology for assessing the feasibility of continuous extractive distillation processes and enables to compare entrainers in terms of minimum reflux ratio and minimum entrainer feed flow rate ratio

Conception des procédés de distillation extractive continue basée sur des critères de faisabilité thermodynamique de la distillation extractive discontinue

Nous étudions la faisabilité du procédé de distillation extractive continue pour séparer des mélanges azéotropiques A-B à température de bulle minimale ou maximale, avec un tiers corps E lourd ou léger. Les mélanges ternaires A-B-E appartiennent aux classes 1.0-1-a et 1.0-2 qui se subdivisent chacune en deux souscas selon la position de la courbe d'univolatilité. La colonne de distillation a trois sections, rectification, extractive, épuisement. Nous établissons les équations décrivant les profiles de composition liquide dans chaque section en fonction des paramètres opératoires: pureté et taux de récupération du distillat, taux de reflux ratio R et rapport des débits d'alimentation FE/F dans le cas d'un tiers corps lourd ; pureté et taux de récupération du produit de pied, taux de rebouillage S et rapport des débits d'alimentation FE/F dans le cas d'un tiers corps léger. Avec un tiers corps lourd alimenté comme liquide bouillant au dessus de l'étage d'alimentation du mélange A-B, nous identifions le distillat atteignable et les plages de valeurs faisables des paramètres R et FE/F à partir du critère général de faisabilité énoncé par Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2009, 48(7), 3544 3559). Pour la classe 1.0-1a, il existe des rapport FE/F et reflux ratio minimum. Le rapport FE/F est plus important pour le procédé continu que pour le procédé discontinu parce que la faisabilité du procédé continu nécessite que les profils d'épuisement et extractifs s'intersectent. Pour la classe 1.0-2, les deux constituants A et B sont des distillats potentiels, l'un sous réserve que le rapport FE/F reste inférieur à une valeur limite maximale. Le procédé continu exhibe également une valeur minimale de FE/F à un taux de reflux ratio donné, contrairement au procédé discontinu. Avec un tiers corps léger alimenté comme vapeur saturante sous l'étage d'alimentation du mélange A-B, nous identifions le produit de pied atteignable et les plages de valeurs faisables des paramètres S et FE/F à partir du critère général de faisabilité énoncé par Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2012, 51, 4643 4660). Comparé au cas des tiers corps lourds, le produit principal est obtenu en pied. Autrement, les comportements des classes 1.0-1a et 1.0-2 sont analogues entre les tiers corps léger et lourd. Avec un tiers corps léger, le procédé continu ajoute la contrainte que les profils de rectification et extractifs s'intersectent. La contrainte d'intersection des profils d'épuisement et extractif est partagée par les deux modes opératoires continu et discontinu. Ce travail valide la méthodologie proposée pour évaluer la faisabilité du procédé de distillation extractive continue et permet de comparer les tiers entre eux en termes de taux de reflux ratio minimum et de rapport de débit d'alimentation minimalWe study the continuous extractive distillation of minimum and maximum boiling azeotropic mixtures A-B with a heavy or a light entrainer E, intending to assess its feasibility based on thermodynamic insights. The ternary mixtures belong to the common 1.0-1a and 1.0-2 class ternary diagrams, each with two sub-cases depending on the univolatility line location. The column has three sections, rectifying, extractive and stripping. Differential equations are derived for each section composition, depending on operating parameters: distillate product purity and recovery, reflux ratio R and entrainer feed flow rate ratio FE/F for the heavy case; bottom product purity and recovery, reboil ratio and entrainer feed flow rate ratio for the light entrainer case. For the case with a heavy entrainer fed as a boiling liquid above the main feed, the feasible product and operating parameters R and FE/F ranges are assessed under infinite reflux ratio conditions by using the general feasibility criterion enounced by Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2009, 48(7), 3544 3559). For the 1.0-1a class, there exists a minimum entrainer - feed flow rate ratio to recover the product, and also a minimum reflux ratio. The minimum entrainer - feed flow rate ratio is higher for the continuous process than for the batch because of the additional requirement in continuous mode that the stripping profile intersects with the extractive profile. For the 1.0-2 class both A and B can be distillated. For one of them there exists a maximum entrainer - feed flow rate ratio. The continuous process also has a minimum entrainer - feed flow rate ratio limit for a given feasible reflux ratio. For the case with a light entrainer fed as saturated vapor below the main feed, the feasible product and operating parameters S and FE/F ranges are assessed under infinite reflux ratio conditions by using the general feasibility criterion enounced by Rodriguez-Donis et al. (Ind. Eng. Chem. Res, 2012, 51, 4643 4660), Compared to the heavy entrainer case, the main product is removed from the column bottom. Similar results are obtained for the 1.0-1a and 1.0-2 class mixtures whether the entrainer is light or heavy. With a light entrainer, the batch insight about the process feasibility holds for the stripping and extractive sections. Now, an additional constraint in continuous mode comes from the necessary intersection between the rectifying and the extractive sections. This work validates the proposed methodology for assessing the feasibility of continuous extractive distillation processes and enables to compare entrainers in terms of minimum reflux ratio and minimum entrainer feed flow rate ratioTOULOUSE-INP (315552154) / SudocSudocFranceF

Extension of thermodynamic insights on batch extractive distillation to continuous operation. 2. Azeotropic mixtures with a light entrainer.

We have studied the continuous extractive distillation of minimum- and maximum-boiling azeotropic mixtures with a light entrainer. The ternary mixtures belong to class 1.0-2 and 1.0-1a diagrams, each with two subcases depending on the location of the univolatility line. The feasible product and feasible ranges of the operating parameters reboil ratio (S) and entrainer/feed flow rate ratio for the continuous process (FE/F) were assessed. Equations were derived for the composition profiles of the stripping, extractive, and rectifying sections in terms of S and FE/F. Class 1.0-1a processes enable the recovery of only one product because of the location of the univolatility line above a minimum value of the entrainer/feed flow rate ratio for both batch and continuous processes. Given a target purity, a minimum reboil ratio S also exists; its value is higher for the continuous process than for the batch process, for the continuous process where stricter feasible conditions arise because the composition profile of the rectifying section must intersect that of the extractive section. Class 1.0-2 mixtures allow either A or B to be obtained as a product, depending on the feed location on the composition triangle. Then, the univolatility line location sets limiting values for either the maximum or minimum of the feed ratio FE/F

Conceptual Design of Non-ideal Mixtures Separation with Light Entrainers

A method is proposed to study the separation of minimum-, maximum-boiling azeotropic, and low volatility mixtures with a light entrainer, to investigate feasible regions of the key operating parameters reboil ratio (S) and entrainer - feed flowrate ratio (FE/F) for continuous processes. The thermodynamic topological predictions are carried out for 1.0–2, 1.0–1a, and 0.0–1 Serafimov’s class diagrams. It relies upon the knowledge of residue curve maps, along with the univolatility line, and it enables the prediction of possible products at the bottom of the column and limiting values of FE/F. The profiles of the stripping, extractive, and rectifying sections are calculated by equations considering S and FE/F, and they bring information about the location of singular points and possible composition profile separatrices that could impair process feasibility. Providing specified product composition and recovery, the approximate calculations are compared with rigorous simulations of extractive distillation processes. Separating non-ideal mixtures using a light entrainer provides more opportunities for the case when it is not easy to find an appropriate heavy or intermediate entraine