Heterogeneous Extractive Batch Distillation of Chloroform - Methanol – Water : Feasibility and Experiments

A novel heterogeneous extractive distillation process is considered for separating the azeotropic mixture chloroform – methanol in a batch rectifying column, including for the first time an experimental validation of the process. Heterogeneous heavy entrainer water is selected inducing an unstable ternary heteroazeotrope and a saddle binary heteroazeotrope with chloroform (ternary diagram class 2.1-2b). Unlike to well-known heterogeneous azeotropic distillation process and thanks to continuous water feeding at the column top, the saddle binary heteroazeotrope chloroform – water is obtained at the column top, condensed and further split into the liquid – liquid decanter where the chloroform-rich phase is drawn as distillate. First, feasibility analysis is carried out by using a simplified differential model in the extractive section for determining the proper range of the entrainer flowrate and the reflux ratio. The operating conditions and reflux policy are validated by rigorous simulation with ProSim Batch Column® where technical features of a bench scale distillation column have been described. Six reproducible experiments are run in the bench scale column matching the simulated operating conditions with two sequentially increasing reflux ratio values. Simulation and experiments agree well. With an average molar purity higher than 99%, more than 85% of recovery yield was obtained for chloroform and methanol

REGSOLexpert: Entrainer Selection Tool for waste solvent recovery by batch distillation processes

A general procedure to systematize the search of several alternatives enabling the separation of non-ideal binary mixtures such as pressure-swing distillation, azeotropic and extractive distillation is presented. The use of heterogeneous entrainers is specially highlighted

Optimisation of heterogeneous batch extractive distillation

This paper considers the optimisation of batch extractive distillation, using heterogeneous entrainers for the first time. The objective function includes the maximum of overall profit and the optimisation variables are the entrainer flowrate and the reflux ratio that is an optimal combination of both decanted phases. Simulation and optimization is performed within MATLAB, by using a genetic algorithm coupled to a short-cut model of the distillation column. The performance of the optimisation scheme is illustrated through the separation of chloroform – methanol mixture with water considering either a constant or a piecewise constant policy for both optimization variables

Heterogeneous batch distillation processes for waste solvent recovery in pharmaceutical industry

A summary about our experiences in the introduction of heterogeneous entrainers in azeotropic and extractive batch distillation is presented in this work. Essential advantages of the application of heterogeneous entrainers are showed by rigorous simulation and experimental verification in a bench batch distillation column for separating several azeotropic mixtures such as acetonitrile – water, n hexane – ethyl acetate and chloroform – methanol, commonly found in pharmaceutical industry

Practical residue curve map analysis applied to solvent recovery in non-ideal binary mixtures by batch distillation processes

Batch distillation inherent advantages has initiated recent search for process feasibility rules enabling the separation of azeotropic or difficult zeotropic binary mixtures thanks to the addition of an entrainer. A systematic procedure enabling to find suitable process and eventually suitable entrainer for the separation of zeotropic or azeotropic binary mixture is described. It brings together into practical use batch distillation process feasibility rules, chemical affinity insight and thermodynamic data analysis available in the literature. The procedure has been implemented in a wizard computer tool and is illustrated on the separation of the water – acetonitrile binary homoazeotrope. Through this tool, all possible 224 feasibility rules and 326 batch distillation sequence processes are checked systematically for each entrainer

On the Riemannian structure of the residue curves maps

In this paper, we revise the structure of the residue curve maps (RCM) theory of simple evaporation from the point of view of Differential Geometry. RCM are broadly used for the qualitative analysis of distillation of multicomponent mixtures within the thermodynamic equilibrium model. Nevertheless, some of their basic properties are still a matter of discussion. For instance, this concerns the connection between RCM and the associated boiling temperature surface and the topological characterization of the distillation boundaries. In this paper we put in evidence the Riemannian metric hidden behind the thermodynamic equilibrium condition written in the form of the van der Waals–Storonkin equation, and we show that the differential equations of residue curves have formal gradient structure. We discuss the first non-trivial consequences ofthis factfor the RCM theory ofternary mixtures

Improved Design and Efficiency of the Extractive Distillation Process for Acetone–Methanol with Water

We show how thermodynamic insight can be used to improve the design of a homogeneous extractive distillation process, and we define an extractive efficiency indicator to compare the optimality of different designs. The case study is related to the separation of the acetone–methanol minimum boiling azeotrope with water. The process flow sheet includes both the extractive distillation column and the entrainer regeneration column. Insight from analysis of the ternary residue curve map and isovolatility curves shows that a lower pressure reduces the minimal amount of entrainer needed and increases the relative volatility of acetone–methanol in the extractive column. A 0.6 atm pressure is selected to enable the use of cheap cooling water in the condenser. We optimize the entrainer flow rate, adjusting both column reflux ratios and feed locations, by minimizing the total energy consumption per product unit. The total annualized cost (TAC) is calculated for all processes. Double-digit savings in energy consumption and in TAC are achieved compared to literature values. We then propose a novel efficiency indicator that describes the ability per tray of extractive section to discriminate the desired product between the top and the bottom of the extractive section. Shifting the feed trays’ locations improves the efficiency of the separation, even when less entrainer is used

Reducing process cost and CO2 emissions for extractive distillation by double-effect heat integration and mechanical heat pump

Double-effect heat integration and mechanical heat pump technique are investigated for the extractive distillation process of the acetone–methanol minimum boiling azeotropic mixture with entrainer water and compared from the economical view by the total annual cost (TAC) and environmental aspect by CO2 emissions. Firstly, A novel optimal partial heat integration (OPHI) process is proposed and optimized through the minimization of a newly defined objective function called OF2 that describes the energy consumption used per product unit flow rate and allows comparison with the literature direct partial and full heat integration processes. We find that the minimum TAC is not achieved by the full heat integration process as intuition, but by the new OPHI process. Secondly, the vapour recompression (VRC) and bottom flash (BF) mechanical heat pump processes are evaluated with respect to energy and CO2 emissions. We proposed a new partial VRC and a new partial BF process in order to reduce the high initial capital cost of compressors. Overall the results show that compared to the conventional extractive distillation process the proposed OPHI process gives a 32.2% reduction in energy cost and a 24.4% saving in TAC while the full BF process has the best performance in environmental aspect (CO2 emissions reduce by 7.3 times)

Isopropyl alcohol recovery by heteroazeotropic batch distillation

Solvent recovery is becoming a major issue in the pharmaceutical and specialty chemical industries. Solvent recovery by conventional batch distillation is limited by the frequent presence of azeotropes in the used solvent mixtures. Most distillation processes for the separation of azeotropic or difficult zeotropic mixtures involve the addition of an entrainer (homogeneous and heterogeneous azeotropic distillation or extractive distillation). In this study the recovery of IPA (isopropyl alcohol) from an industrial waste stream (IPA/water mixture) was studied by conventional batch distillation and heteroazeotropic batch distillation, using cyclohexane as entrainer. First the ternary IPA/water/cyclohexane azeotrope (boiling temperature of 64.1 °C), then the binary IPA/cyclohexane azeotrope (boiling temperature of 69.3°C) and finally pure IPA was distilled. 99.96 mass% IPA could be obtained by heteroazeotropic distillation, using cyclohexane as entrainer. By using this procedure the IPA recovery is 97.6%, which is high compared to the conventional distillation techniques. The binary azeotrope could be reused in a subsequent heteroazeotropic batch distillation

Low pressure design for reducing energy cost of extractive distillation for separating Diisopropyl ether and Isopropyl alcohol

We show how reducing pressure can improve the design of a 1.0-1a mixture homogeneous extractive distillation process and we use extractive efficiency indicators to compare the optimality of different designs. The case study concerns the separation of the diisopropyl ether (DIPE)–isopropyl alcohol (IPA) minimum boiling azeotrope with heavy entrainer 2-methoxyethanol. We first explain that the unexpected energy cost OF decrease following an increase of the distillate outputs is due to the interrelation of the two distillate flow rates and purities and the entrainer recycling through mass balance when considering both the extractive distillation column and the entrainer regeneration column. Then, we find that for the studied case a lower pressure reduces the usage of entrainer and increases the relative volatility of DIPE–IPA for the same entrainer content in the extractive column. A 0.4 atm operating pressure is selected to enable the use of cheap cooling water in the condenser. We run an optimization of the entrainer flow rate, both columns reflux ratios, distillates and feed locations by minimizing the total energy consumption per product unit. Double digit savings in energy consumption are achieved while TAC is reduced significantly. An extractive efficiency indicator that describes the ability of the extractive section to discriminate the desired product between the top and the bottom of the extractive section of the extractive section is calculated for comparing and explaining the benefit of lowering pressure on the basis of thermodynamic insight