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Improvement of Batch Distillation Separation of Azeotropic Mixtures Distillation Is the Most Widespread Method for Separating Liquid Mixtures

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Improvement of Batch Distillation Separation of Azeotropic Mixtures Distillation Is the Most Widespread Method for Separating Liquid Mixtures %NVUEDELOBTENTIONDU %0$503"5%&-6/*7&34*5² %&506-064& $ÏLIVRÏPAR Institut National Polytechnique de Toulouse (INP Toulouse) $ISCIPLINEOUSPÏCIALITÏ Génie des procédés et de l'environnement 0RÏSENTÏEETSOUTENUEPAR Laszlo Hegely LE vendredi 15 novembre 2013 4ITRE Improvement of Batch Distillation Separation of Azeotropic Mixtures %COLEDOCTORALE Mécanique, Energétique, Génie civil et Procédés (MEGeP) 5NITÏDERECHERCHE Laboratoire de Génie Chimique, UMR 5503 $IRECTEURS DE4HÒSE Prof. Peter LANG, DSc Vincent GERBAUD, HDR 2APPORTEURS Prof. Jean-Michel RENEAUME Prof. Edit SZEKELY MEMBRES DUJURY: Prof. Michel MEYER Prof. Istvan FARKAS Prof. Peter LANG, DSc Vincent GERBAUD, HDR Prof. Jean-Michel RENEAUME Prof. Edit SZEKELY ii PhD thesis under common supervision presented for obtaining THE TITLE OF PHD OF THE INSTITUT NATIONAL POLITECHNIQUE DE TOULOUSE Doctoral school: Mécanique, Energétique, Génie civil, & Procédés Specialty: Process engineering and THE TITLE OF PHD OF THE BUDAPEST UNIVERSITY OF TECHNOLOGY AND ECONOMICS Doctoral school: Pattantyús-Ábrahám Géza Mechanical Sciences by László HÉGELY chemical engineer IMPROVEMENT OF BATCH DISTILLATION SEPARATION OF AZEOTROPIC MIXTURES Supervisors: Péter LÁNG DSc, Budapest University of Technology and Economics Vincent GERBAUD HDR, Institut National Polytechnique de Toulouse 2013 iii iv Acknowledgement This PhD thesis is the result of my research work performed under common supervision at the Department of Building Services and Process Engineering of the Budapest University of Technology and Economics and at the Laboratoire de Génie Chimique of Institut National Politechnique de Toulouse. First of all, I would like to thank my supervisors Prof. Péter Láng and Prof. Vincent Gerbaud for receiving me as a PhD student in Hungary and in France, respectively. They were always ready to help me, to discuss and correct my works, even though they are both very busy. I am also indebted to Prof. Jean-Michel Reneaume of and Prof. Edit Székely, the reviewers of this thesis for their careful reading and their constructive suggestions. I also thank Prof. István Farkas, Prof. Michel Meyer and Ivonne Rodríguez-Donis for accepting to be part of the jury. I also thank Gábor Modla and Ferenc Dénes, members of our research group in Budapest for their help and their ideas, and to Máté Erdős for his technical help with the figures of my thesis. I thank Márta Láng-Lázi for starting me in the world of research and teaching me Maple. I also thank Ivonne Rodríguez-Donis for her interest in my work and for our discussions. I would like to thank the French Embassy in Hungary for their scholarship, which made my studies in France possible. It is impossible to mention all the colleagues and friends in Toulouse, yet my special thanks go to Sofí and Marco for all their amity and support. Finally, I would like to say many thanks to my parents who always supported me and to my friends in Hungary who were patient with me. v Doctorat de l‟Université de Toulouse Délivré par l‟Institut National Polytechnique de Toulouse (INP Toulouse) et l‟Université des Sciences Techniques et Économiques de Budapest (BME), Hongrie École doctorale MEGeP Spécialité Génie des procédés et de l‟Environnement Le 15 novembre 2015 László HÉGELY Amélioration de la séparation distillation discontinue des mélanges azéotropiques La distillation est le procédé de séparation le plus répandu dans l‟industrie chimique. Pour la séparation des mélanges azéotropiques, une méthode spéciale de distillation doit être appliquée. Le but de mon travail était d‟améliorer la séparation des mélanges azéotropiques par distillation discontinue (DD). Un nouvel algorithme a été présenté pour la détermination de la séquence des produits de DD pour des mélanges multicomposants azéotropiques. Contrairement aux méthodes publiées précédemment, cet algorithme n‟a pas besoin des paramètres d‟équilibre. Configurations non-conventionnelles de DD ont été étudiées par simulation rigoureuse avec un accent sur l‟opération fermée. Nombreux modes d‟opération fermés étaient proposés, lesquelles diffèrent en l‟opération de réservoir supérieur. Les effets du recyclage des fractions sur un procédé de séparation existant de 6 lots d‟un mélange déchet azéotropique ont été étudiés. Les études ont été étendues pour un procédé de distillation extractive discontinue (DED). Un volume minimal de pré-fraction doit être incinéré. Le cas optimal de DED a donné un profit plus grand que celui de DD. DED a été étudié pour la séparation des deux mélanges azéotropiques. La séparation a été infaisable ou le rendement a été bas par DD, mais DED et le procédé hybride ont donné des rendements élevés. Une nouvelle politique de DED a été aussi proposée. Un modèle généralisé de la distillation hétéroazéotropique discontinue avec une rétention variable de décanteur a été développé. Dans une analyse de faisabilité, toutes les politiques opérationnelles possibles ont été identifiées. Ce modèle a été étendu pour la distillation extractive hétérogène discontinue. Mots clés : distillation discontinue, azéotropes, séquence des produits, distillation extractive discontinue, opération fermée, distillation hétéroazéotropique discontinue Laboratoire de Génie Chimique, 4 allée Emile Monso, 31432 Toulouse cedex 4 Département d‟installation et génie des procédés, Műegyetem rkp. 3, H-1521, Budapest, Hongrie Improvement of Batch Distillation Separation of Azeotropic Mixtures Distillation is the most widespread method for separating liquid mixtures. The separation of azeotropic mixtures requires a special distillation method. My aim was to improve the batch distillation separation of azeotropic mixtures. A new algorithm was presented for the determination of product sequences of batch distillation of multicomponent azeotropic mixtures. Non-conventional configurations were studied by simulation with emphasis on closed operation. The effects of off-cut recycle on a six-batch separation process of a waste solvent mixture were also investigated. Batch extractive distillation was studied for the separation of two azeotropic mixtures. A new extractive policy was also proposed. A generalised model of batch heteroazeotropic distillation with variable decanter hold-up was developed. This model was extended for batch heterogeneous extractive distillation. Keywords : batch distillation, azeotropes, product sequences, batch extractive distillation, closed operation, batch heteroazeotropic distillation Laboratoire de Génie Chimique, 4 allée Emile Monso, 31432 Toulouse cedex 4 Department of Building Services and Process Engineering, H-1521 Budapest, Hungary Résumé en français La distillation est la méthode appliquée la plus fréquemment pour la séparation des mélanges liquides, qui est basée sur la différence des volatilités des composants. Comme la distillation se compose d„étapes consécutives de vaporisation et condensation partielle, son besoin en énergie est très élevé. Pour cette raison, la conception et opération optimale des procédés de distillation est un enjeu important tant de point de vue de l‟économie que d‟environnement. Si le mélange est fortement non-idéal, des azéotropes peuvent se produire. Au point azéotropique, les compositions de la phase vapeur et celle de liquide sont identiques, ce qui signifie qu‟un mélange azéotropique ne peut pas être séparé par un procédé de distillation conventionnelle. Si la volatilité relative est très basse, la séparation est faisable en théorie, mais le taux de reflux et nombre des plateaux élevés rendent la distillation conventionnelle non rentable. Pour la séparation des mélanges azéotropiques et à points d‟ébullition voisins, des méthodes de distillation spéciales doivent être appliquées. Ces méthodes exploitent la sensibilité à la pression éventuelle de la composition azéotropique (distillation avec changement de pression), ou l‟influence favorable d‟un agent de séparation (entraîneur). L‟effet de l‟entraîneur est différent selon la technique de séparation. Dans le cas de la distillation homoazéotropique, un comportement azéotropique provoqué par l‟entraîneur est exploité. Dans le cas de la distillation extractive, l‟entraîneur, alimenté continuellement à la colonne, change les volatilités relatives favorablement. Dans le cas de la distillation hétéroazéotropique, l‟entraîneur forme deux phases liquides avec un des composants originaux, et cette répartition liquide-liquide est exploitée par décantation pour séparer le mélange originel. Dans certain industries, par exemple l‟industrie pharmaceutique, la récupération des solvants, l‟industrie chimique fine, la production d‟alcool et de teinture, la distillation est effectuée en mode discontinu. L‟avantage de distillation discontinue est que cela peut être appliqué pour la séparation des mélanges de quantité et composition variable. Dans les industries ci-dessus, des mélanges multicomposants azéotropiques sont fréquents. Dans le cas de la régénération des déchets mélanges des solvants, on cherche à récupérer un composant principal, ce qui est avantageux tant de point de vue de l‟économie (une quantité du mélange plus faible doit être incinérée) que de l‟environnement. L‟existence des azéotropes peut limiter le rendement, ou même rendre la séparation infaisable, à moins qu‟une méthode de distillation spéciale soit appliquée. La possibilité d‟économiser de l‟énergie et la réglementation environnementale plus sévère ont provoqué un intérêt accru à la recherche de la distillation discontinue dans les dernières dizaines d‟années, avec un accent
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