Startup of a reactive distillation process with a decanter

The startup of a reactive distillation process for the production of propyl acetate including a decanter is studied. A simulation model is presented which describes the whole startup from a cold and empty state and takes into account the liquid phase split in the decanter. The simulation model is successfully validated with own dynamic experimental data. Different startup strategies are developed and analysed in simulation studies showing the high influence of the initial charging of decanter and reboiler on the startup time

Production zone method : a new non-ideal shortcut method for distillation column Design

Graphical shortcut methods are useful tools for the design of distillation columns. The proposed nonideal shortcut method includes a graphical representation and is based on the concept of operation leaves. This new method uses a production segment rather than a completely specified product, which eliminates any sensitivity to the composition of the minor product. Concerning phase equilibria, no restrictive assumptions are made. The study aimed (1) to determine whether a specified separation respects the mass balance and thermodynamic feasibility and (2) to find the minimum reflux ratio for a preliminary design of the column. Designs obtained with this new method for ideal, non-ideal, and azeotropic mixtures give purity and recovery rates close to the specifications, which might be impossible to obtain with a conventional ideal shortcut like the well-known Fenske–Underwood–Gilliland shortcut method. The distillation boundaries of azeotropic mixtures are taken into account thanks to a non-ideal thermodynamic model applied to the calculation, which is not the case with a conventional ideal shortcut. The paper examines the following mixtures: an ideal mixture of ethanol, n-propanol, and n-butanol; a non-ideal mixture of acetone, water, and acetic acid; and an azeotropic mixture of acetone, isopropanol, and water

Dynamics of reactive distillation for the production of ethyl acetate: experiments at a pilot plant and modelling

In order to understand the complex behaviour of the reactive distillation process and to be able to provide an accurate design of a reactive column, detailed analyses on both continuous and transient regime become necessary. The objective is the definition of a reliable simulation model, based on experimental data obtained from a real pilot-scale plant device for the heterogeneously catalysed esterification of acetic acid and ethanol to form ethyl acetate and water. The choice of the parameters for the continuous equilibrium model was discussed and the simulation results provided good agreement with experimental data, revealing an interesting sensitivity of the catalyst activity to the feed composition. Once column configuration and operational parameters were validated, dynamic experiments were realized so as to interpret the sensitivity of different disturbances. Feed flow rates, reflux ratio and heat duty were perturbed and the consequent open loop transient responses were identified. The assessment of hydrodynamic parameters and the validation of the transient data allow the definition of a reliable dynamic model that represents tendencies and behaviours of the process well. The resulting model is to be applied into a more complex controllability methodolog

Experiments and dynamic modeling of a reactive distillationcolumn for the production of ethyl acetate by consideringthe heterogeneous catalyst pilot complexities

Great effort has been applied to model and simulate the dynamic behavior of the reactive distillation as a successfulprocess intensification example. However, very little experimental work has been carried out in transient conditions.The work presents a series of experiments for the production of ethyl acetate from esterification of acetic acid andethanol in a reactive distillation pilot column. The steady-state approach performed experiments with both excessof alcohol and stoichiometric feed configuration. Predicted and measured results show good agreement and reveala strong dependency of the structured packing catalyst activity on the pilot geometry and its operating conditions.The transient process behavior of the heterogeneously catalyzed system was deeply investigated and continuousand dynamic data were collected for an equilibrium model validation, after different perturbations on parameters.The experimental validation is shown to be essential to provide realistic hydrodynamic parameters, to understandthe sensitive parameters such as heat losses and to adapt values for the catalyst holdup as a function of the system

Analyse de faisabilité, conception et simulation de la distillation réactive liquide-liquide-vapeur. Application et validation expérimentale sur la production de l'acétate de n-propyle

A design methodology of reactive distillation process applied to vapor-liquid-liquid mixtures is presented in this study. Only a few work has been dedicated to such systems whereas they constitute a large application area of reactive distillation; therefore it represents a gap to fill in.Reliable and consistant computation of chemical and phase equilibria is required beforehand any feasibility assessment, design or simulation. The two most general ways to find such an equilibrium is to minimize the free Gibbs energy or to solve a specific set of equations; a single set of equations being able to describe all physical states of the system is defined instead of these two traditional approaches, avoiding numerical problems while keeping implementation and resolution simplicity.A reactive residue curve map (rRCM) tool taking into account chemical and phase equilibria has been developed and checked for C1-C5 acetate esterifications. Finally a feasible design on the high purity n-propyl acetate production, based on the rRCM analysis and publications, has been performed confirmed by steady-state simulation runs; the simulation tool was validated by thermodynamic, kinetic and pilot plant experiments. These experiments are presented detailed in the paper.Ces travaux de thèse apportent une contribution à la problématique de la conception de procédés de distillation réactive pour les systèmes liquide-liquide-vapeur réactifs. Ce type de systèmes, bien que présentant un vaste nombre d'applications potentielles, reste très peu étudié et le champ d'investigation s'y rapportant demeure encore très large.La base préalable à tout outil d'analyse de faisabilité, de conception ou de simulation d'un tel procédé requiert la détermination rapide et consistante des équilibres chimiques et entre phases. Une alternative aux approches classiques - minimisation de l'énergie libre de Gibbs et approches orientées équations - consistant à écrire un unique jeu d'équations capable de représenter toutes les combinaisons de phases possibles est proposée.Un outil de génération et de tracé de réseaux de courbes de résidu réactif (rRCM) prenant rigoureusement en compte les équilibres liquide-liquide-vapeur réactifs (LLV) a été développé et testé sur des réactions d'estérifications en C1-C5. Une configuration faisable de production d'acétate de n-popyle par distillation réactive, bâtie sur la base d'un réseau rRCM et de travaux sur les procédés de production d'acétates, a été développée à l'aide de simulations continues~;~afin de s'assurer la qualité de cette conception, l'outil de simulation s'appuie sur des données thermodynamiques, cinétiques et pilotes expérimentales

Analyse de faisabilité, conception et simulation de la distillation réactive liquide-liquide-vapeur (application et validation expérimentale sur la production de l'acétate de N-Propyle)

Ces travaux de thèse apportent une contribution à la problématique de la conception de procédés de distillation réactive pour les systèmes liquide-liquide-vapeur réactifs. Ce type de systèmes, bien que présentant un vaste nombre d'applications potentielles, reste très peu étudié et le champ d'investigation s'y rapportant demeure encore très large. La base préalable à tout outil d'analyse de faisabilité, de conception ou de simulation d'un tel procédé requiert la détermination rapide et consistante des équilibres chimiques et entre phases. Une alternative aux approches classiques - minimisation de l'énergie libre de Gibbs et approches orientées équations - consistant à écrire un unique jeu d'équations capable de représenter toutes les combinaisons de phases possibles est proposée. Un outil de génération et de tracé de réseaux de courbes de résidu réactif (rRCM) prenant rigoureusement en compte les équilibres liquide-liquide-vapeur réactifs (LLV) a été développé et testé sur des réactions d'estérifications en C1-C5. Une configuration faisable de production d'acétate de n-propyle par distillation réactive, bâtie sur la base d'un réseau rRCM et de travaux sur les procédés de production d'acétates, a été développée à l'aide de simulations continues ; afin de s'assurer la qualité de cette conception, l'outil de simulation s'appuie sur des données thermodynamiques, cinétiques et pilotes expérimentalesA design methodology of reactive distillation process applied to vapor-liquid-liquid mixtures is presented in this study. Only a few work has been dedicated to such systems whereas they constitute a large application area of reactive distillation ; therefore it represents a gap to fill in.Reliable and consistant computation of chemical and phase equilibria is required beforehand any feasibility assessment, design or simulation. The two most general ways to find such an equilibrium is to minimize the free Gibbs energy or to solve a specific set of equations ; a single set of equations being able to describe all physical states of the system is defined instead of these two traditional approaches, avoiding numerical problems while keeping implementation and resolution simplicity. A reactive residue curve map (rRCM) tool taking into account chemical and phase equilibria has been developed and checked for C1-C5 acetate esterifications. Finally a feasible design on the high purity n-propyl acetate production, based on the rRCM analysis and publications, has been performed confirmed by steady-state simulation runs ; the simulation tool was validated by thermodynamic, kinetic and pilot plant experiments. These experiments are presented detailed in the paper.TOULOUSE-ENSIACET (315552325) / SudocSudocFranceF