Experiments in Chemical Engineering

Binary Distillation

Experiment 1 BINARY DISTILLATION

INTRODUCTION
Distillation is one of the most important but also the most energy intensive separation process that chemical engineers should be concerned about. Thus, a good understanding of the theories and application of this unit operation is essential in order to minimize energy consumption. There are many types of distillation operations, depending on the process followed, the type of equipment and the number of volatile components present in the solution to be purified. In this laboratory exercise the one using the concept of a binary equilibrium relationship by operating a simple batch distillation set-up is investigated. The binary system applied is ethanol-water where students will investigate the validity of the Rayleighs equation.

OBJECTIVES
The experiment is composed of two parts with the following objectives: 1. To investigate the applicability of the Rayleighs Equation to describe differential distillation. 2. To determine the temperature and concentration profile in a differential distillation process.

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THEORY
Distillation is a unit operation commonly used for purifying liquids and separating a liquid mixture of miscible and volatile substances into individual components or, in some cases, into groups of components. A liquid can be classified as volatile when it is readily vaporized at a relatively low temperature. The boiling of the more volatile components of the mixture drives the distillation process. When the vapor is cooled, the more volatile material condenses in a greater proportion than the less volatile material. The components are separated based on their physical properties, specifically, relative volatilities. Relative volatility, a tool used to express the magnitude of the equilibrium distribution, is defined as

( (
where

) )

Relative volatility Vapor composition Liquid composition More volatile component Less volatile component

There are two types of distillation classified according to its mode of operation. These are continuous and the batch distillation. In a batch system, the column can handle different mixtures by simply changing its operating conditions. The main disadvantage to using this kind of system, however, is that the longer the components are exposed to high temperature, the better the chances that the components are broken down via thermal degradation. Along with this, the energy requirements are usually higher for a batch system. Conversely, continuous distillation, as the name implies, feed is continuously supplied and separated into two or more products over some period. On the other hand, batch distillation involves the processing of a batch of feed at a given time and split into products by selectively removing the more volatile fractions over time. A. Differential Distillation When a binary solution of volatile liquids is subjected to batch differential distillation, the concentration of the solution in the distillery still decreases in the more volatile component as the boiling point of the solution increases. The resulting vapor is allowed to condense through a condenser and collected together as the distillate product.

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Binary Distillation

The problem in this case is to relate the initial amount of feed together with its concentration and the amount of over-all distillate collected and its concentration. At any given time, the concentrations may be related by material balance. Referring to Figure 1, if W is the amount in the still at any time of concentration x, a more volatile component balance yields ( ( )( ) )
X

y dW

x W-dW

Figure 1: Distillation System Integrating, considering the initial feed as F and concentration xF,

This equation is referred to as Rayleighs Equation. The instantaneous liquid composition, x, and the corresponding vapor composition, y are assumed to be in equilibrium with one another. Vapor Liquid Equilibria (VLE) data may be determined from Vapor-PressureTemperature, Boiling Point Composition diagram or equilibrium data, or x-y diagram for the binary system.

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The Rayleigh Equation may be simplified to various forms such as: 1. If Henrys law applies, y = mx where m = H/P. The integrated equation yields

this equation, however, is applicable only for dilute solutions, where the partial pressure of the vapor is a linear function of composition. 2. If the relative volatility, may be assumed practically constant then, ( )

substituting this in the previous equation and integrating gives [ ]

or in terms of individual components, Subscript 1 refers to the initial amounts and subscript 2 refers to the final amounts found in the solution. The amount of distillate may be determined by material balance together with its composition. If the above assumptions could not be applied, the best way to evaluate the integral of Equation 2 is by graphical or numerical methods. The graphical method is shown in Figure 2. Graphically, plot versus x at different stages of the experiment to relate the amount distilled at any time with composition and temperature by getting the area under the curve and comparing this area and composition with the experimental data obtained. The validity of the simplified equation may also be compare with the experimental data.

Figure 2: Graphical Method

Experiments in Chemical Engineering

Binary Distillation

EQUIPMENT
A. Actual Equipment

Control System

Packed Column

Boiler

Still

Figure 3: Laboratory Distillation Column

B. Equipment Design The equipment contains a 4-inch bubble cap batch distillation column which may be operated under total or partial reflux conditions. Also used in this experiment is a distillation column packed with glass beads for total reflux operations. As for the determination of the refractive index, a refractometer was used.

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Binary Distillation

PROCEDURE
A. Preparation of a Calibration Curve 1. Prepare a 0, 10, 20, 30, 40, 50, 60, 70, 80, 90 (% v/v) ethanol solution. 2. Use the refractometer to determine the refractive indices of the different solutions. 3. Plot the refractive index versus ethanol concentration.

B. Batch or Differential Distillation Experiment 1. Setup the batch distillation apparatus. 2. Make 10% ethanol (25 mL pure ethanol and 225 mL water). 3. Heat the setup until the first drop of condensate is collected. Record the initial temperature reading and start the time. 4. For every 10 mL of condensate collected, record the corresponding time and temperature. 5. Using a refractometer, determine the refractive index of the samples collected. 6. Repeat steps 4 and 5 until you have at least six runs or until 60 to 70% of the solution is distilled.

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Binary Distillation

Binary Distillation
DATA SHEET
A. Calibration Data
Concentration of C2H5OH-H2O (% v/v) 0 10 20 30 40 50 Refractive Index 1.3325 1.336 1.315 1.354 1.3555 1.360 Concentration of C2H5OH-H2O (% v/v) 60 70 80 90 99 Refractive Index 1.3595 1.361 1.361 1.360 1.3595

B. Batch Distillation
Condensate Temperature (C) Refractive Index Bottom Sample Temperature (C) Refractive Index Middle Sample Temperature (C) Refractive Index

Volume (mL)

Time (minsec)

1 drop

st

10 20 30 40 50 60 70 80 90 100

45 88 88 89 90.5 92 94 95 96 98 98

0 1.361 1.3615 1.36155 1.362 1.3605 1.36 1.3585 1.354 1.348 1.339

45 75 78 83 85 87 89 91 93 94 95

0 1.34 1.339 1.3385 1.338 1.336 1.3355 1.334 1.3333 1.3333 1.3326

45 65 75 79 83 87 89 92 94.5 96.5 98

0 1.3615 1.361 1.3605 1.36 1.3585 1.358 1.355 1.35 1.345 1.3385

----108 218 330 449 614 749 937 1139 1358 1624

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GUIDE QUESTIONS
1. Plot the calibration curve as refractive index versus ethanol concentration. 2. Derive a correlation equation for refractive index as a function of concentration. Comment on the usefulness of this correlation. What is the range of concentration that generates the smallest and largest deviation? 3. Plot the F/W and the experimental ratio F/W versus the concentration of the residue. Describe the results. Is there good agreement between the experimental results with those obtained by Rayleighs equation? 4. Compare the experimental amount of total collected with the theoretical results using the graphical method of solution and using the average relative volatility during the entire differential distillation process. Tabulate and indicate the percent deviation.

ANALYSES AND CALCULATIONS

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APPENDIX

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