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Department of Chemical Engineering Unit Operations Laboratory

Continuous Distillation Theory


This handout provides important information on filtration theory and related issues: o o o o o o o o Continuous Distillation Theory Determination of Composition by Gas Chromatography Computer Simulation Degrees of Freedom/Sensitivity Material and Energy Balances Properties Statistical Analysis Important Remarks

Continuous Distillation Theory


The theory is well developed for the prediction of distillation column operations. This section provides an overview of some of the equations and theory associated with continuous distillation. For additional theory development, see Resources. In continuous mode, with feed and distillate and/or bottoms products, lighter components rise up the trays in the column as vapor and are finally liquefied in the condenser. This condensed liquid is either drawn off or reintroduced into the top of the column. Each tray of the column is assumed to be in vapor-liquid equilibrium. Geankoplis (1993) (see Resources) provides excellent diagrams illustrating the flows within a distillation column and the equilibrium on each tray. Several approaches can be taken:

Graphical Methods (McCabe-Thiele method and Ponchon-Savart method) Shortcut Methods (e.g. Fenske-Underwood-Gilliland method) Rigorous plate-to-plate calculations (using computer software)

The graphical and shortcut methods are specifically for steady state operations. While they do not apply directly to the unsteady operation of a distillation column, they can be useful in initially characterizing a column. For total reflux calculations, the Fenske equation (part of the FUG Shortcut Method) can be used to determine the number of plates required for a given separation. The rigorous plate-to-plate calculations can easily be performed with available computer aided engineering flowsheet simulation programs or special purpose distillation programs.

Modified: 4/19/2007 Original Document:

Kevin M. Sapp Jullie Lawson

page 1/4 2007

Department of Chemical Engineering Unit Operations Laboratory

Determination of Composition by Gas Chromatography o You will be injecting 0.1 micro-liter samples o At the beginning of each lab period, inject ethanol, isopropanol, and methanol standards. Note the retention time for each of these peaks. o Use the retention time for the standard peaks to identify peaks from your samples. o Use the relative peak areas of the components in your sample to determine the mole fractions of components in the sample.

Computer Simulation Using your knowledge and resources on Continuous Distillation Theory, develop a theoretical basis for predicting steady-state temperatures, pressures, flows, compositions, etc. for your experimental conditions. Use these results to plan your experimental runs then compare your actual results with those predicted. HYSYS is an excellent programming resource for computer simulation of distillation columns. A tutorial is available online at http://hysys.che.ufl.edu/unit_op_lab_examples/index.html Start-up Simulation o Several computer programs are available to perform the dynamic calculations, and return the tray-by-tray characteristics as a function of time. o The HYSYS Plant flowsheet simulation package can be run in dynamic mode for this purpose. o Ideally, you would like to determine the following as a function of time: distillate product composition bottoms product composition stage by stage composition profile stage by stage flow profile heat transfer rate to the condenser heat transfer rate to the reboiler o And determine the effect of Murphree efficiency on the above effect of feed plate location on the above time to reach steady state

Modified: 4/19/2007 Original Document:

Kevin M. Sapp Jullie Lawson

page 2/4 2007

Department of Chemical Engineering Unit Operations Laboratory

Steady State Simulation o Several computer programs are available to perform the dynamic calculations, and return the tray-by-tray characteristics as a function of time. o The HYSYS Plant flowsheet simulation package run in steady-state mode is recommended for this. o Ideally, you would like to determine steady-state values for: distillate product composition bottoms product composition stage by stage composition profile stage by stage flow profile heat transfer rate to the condenser heat transfer rate to the reboiler o And determine the: effect of Murphree efficiency on the above effect of feed plate location on the above Tray Efficiency Evaluation Determining the efficiency of the trays in the column is an iterative trial and error procedure. First the programs or simulation packages (e.g. in HYSYS Plant simulation) must be setup to simulate the operation of the column. Next, the user guesses the tray efficiencies and the computer performs a tray-by-tray calculation to determine the concentration of the distillate and bottoms products. If the values of the calculated distillate and bottoms concentrations equal to the values found experimentally, then the guessed efficiencies are assumed to be correct. Otherwise, another estimate of the efficiencies is made and the program should be executed again. This is repeated until the predicted product compositions are the same as those determined experimentally.

Degrees of Freedom/Sensitivity
The main independent variables available for study in the experiments include:

Flow rates (feed, distillate, bottoms) Steam flow rate Condenser water flow rate Feed position

Consider effects of changes of these variables on key distillation performance indicators. Note that there are limits to the control of these variables with the equipment available, and not all of these variables will affect performance in a measurable way.
Modified: 4/19/2007 Original Document: Kevin M. Sapp Jullie Lawson page 3/4 2007

Department of Chemical Engineering Unit Operations Laboratory

Material and Energy Balances


Use the experimentally determined compositions and flow rates to determine material balances. Also perform energy balances over the column, around the reboiler, and around the condenser, determining duties and heat transfer coefficients as needed. Resolve any data discrepancies and obtain closure on the material and energy balances.

Properties
Properties for ethanol and isopropanol are well known. Material and Safety Data Sheets for these major components, as well as methanol, methyl isobutyl ketone, and ethyl acetate, which are present in small amounts, are available for download on the Continuous Distillation Safety webpage. HYSYS DISTIL can be used to create vapor-liquid equilibrium curves for the binary system of ethanol and isopropanol, as well as the ternary system of methanol, ethanol, and isopropanol. Preparation of XY phase diagrams and HXY diagrams for the experimental conditions is strongly recommended. Note the importance of selecting an appropriate property estimation model.

Statistical Analysis
Apply appropriate statistical procedures to determine the apparent error in results.

Important Remarks
Whenever possible, measure variables several times and different ways to verify values.

Modified: 4/19/2007 Original Document:

Kevin M. Sapp Jullie Lawson

page 4/4 2007

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