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Department of Chemical Engineering

Unit Operations Laboratory

Batch Distillation Overview

Distillation is commonly used in separating and purifying liquids in industry. Its operation is
based on differences in boiling points between the components being separated. The lighter
components move up the column and the heavier components fall down. When the relative
volatility between the components being separated is high, distillation tends to be cheaper than
other separation methods.

In this project, ethanol and isopropanol are separated using a twelve-plate distillation column. A
batch will be prepared in the steam-heated reboiler prior to the start of the lab period. The
column will be started up under total reflux conditions, and then distillate product will be drawn
off. By operating the column under different conditions, its performance can be characterized.
Control of the column throughout experimentation will be achieved using a computerized control
system. Sample compositions will be determined using Gas Chromatography as outlined on the
Batch Distillation Theory web page.

This web page provides an overview of the following topics as they relate to the Batch
Distillation project:

Purpose
Concepts to Review
Study Questions
Prediction of Planned Runs
Useful Apparatus Data
Possible Objectives

In addition, you should download and review the handout provided by your faculty advisor.

Modified: 4/24/2007 Kevin M. Sapp page 1/6


Original Document: Jullie Lawson © 2007
Department of Chemical Engineering
Unit Operations Laboratory

Purpose

• To study the performance of a binary distillation column operated in batch mode.


• To study the operating parameters (such as distillate composition and Murphree
efficiency as a function of time), modeling, and control issues involved in batch
distillation.
• To develop an understanding of how reflux rate/reflux ratio affects the efficiency of the
column and the composition of distillate and bottoms products as a function of time.

Concepts to Review

In order to satisfactorily complete this laboratory exercise, it is important to have a thorough


understanding of the following concepts:

• Batch distillation
• Reflux rate, reflux ratio, boil up rate
• Overhead or distillate product, bottoms product
• Vapor-liquid equilibrium (VLE)
• Relative volatility
• Murphree efficiency, point efficiency, Fenske efficiency
• Degrees of sub-cooling
• McCabe-Thiele Method
• Ponchon-Savart Method
• Short-cut distillation methods
• Rigorous plate to plate calculating procedures
• Euler’s method for solving differential equations
• Material and energy balance closure

Study Questions

1. What are the independent variables for this experiment? (i.e. Given the distillation
column in the laboratory and its associated control configurations, what variables can you
directly manipulate?)
2. How can you tell when steady state is achieved?
3. How long does it take to reach steady state under total reflux conditions?
4. How do different non-infinite reflux ratios affect the column performance?
5. How do the results from the McCabe-Thiele, Ponchon-Savarit, shortcut, and rigorous
calculation methods compare? Should they differ?

Modified: 4/24/2007 Kevin M. Sapp page 2/6


Original Document: Jullie Lawson © 2007
Department of Chemical Engineering
Unit Operations Laboratory

6. If the theoretical and actual number of stages is known for a given operating condition,
what is the overall column efficiency,?
7. How does Murphree tray efficiency vary along the length of the column? Relate this
efficiency to the overall column efficiency.
8. How does the reflux rate, reflux ratio, boil-up rate, and steam flow rate affect the
Murphree efficiency, overhead product composition, and bottoms product composition?
9. Is the Fenske equation applicable for this system? (Hint: Is relative volatility constant?)

Prediction of Planned Runs

The project planning process should include determination of a set of operating conditions to be
analyzed.

It is strongly recommended that the first lab period be used to accomplish the following tasks, at
a minimum:

o Run the column at total reflux.


o Determine the time required to reach steady state.
o Take samples from the reboiler and distillate product.
o Learn how to set-up for drawing off distillate product, even if you do not perform this
task the first week.
o From total reflux operation, obtain the overall column efficiency using the top and
bottoms samples.

Note that it is easy to choose conditions that are outside of the performance limits of the
apparatus, are impossible to perform during the allotted laboratory time (e.g. it takes more than
four hours to reach steady-state), are insensitive to the different initial conditions, or for which
no meaningful parameter values can be determined.

You should carefully study the limitations of the existing experimental apparatus as a part of the
planning process rather than finding out in the subsequent laboratory runs that the experimental
values obtained are useless.

Useful Apparatus Data

• The batch distillation system includes a 12-plate column (bubble cap trays), a steam-
heated reboiler, a water-cooled condenser, and a distillate product tank.
• The column can be divided into two sections:

Modified: 4/24/2007 Kevin M. Sapp page 3/6


Original Document: Jullie Lawson © 2007
Department of Chemical Engineering
Unit Operations Laboratory

o The Stripping Section: located on the first floor, consists of the reboiler and
sample tap, reboiler mixing pump, steam, water, and air (for operation of
pneumatic water control valves) supplies
o The Enriching Section: located on the second floor, consists of the condenser,
standpipe where the liquid is held up after being condensed, distillate and reflux
lines, sample tap on the reflux line, air (for operation of pneumatic control valves)
and water supplies
• Other specifications for the column are as follows:
o Distance between plates 12’’
o weir height 1’’
o hold-up on plates 2 lb/plate
o hold-up in condenser 4.5 lb.
• A diagram of the distillation column is shown below. This is the computer control screen
from which the column is operated.

Modified: 4/24/2007 Kevin M. Sapp page 4/6


Original Document: Jullie Lawson © 2007
Department of Chemical Engineering
Unit Operations Laboratory

• The starting reboiler composition will be approximately 50% ethanol, 50% isopropanol,
up to 4% methanol, and less than 1% other components including methyl isobutyl ketone,
ethyl acetate, and naphtha solvent (refer to MSDS for Ethanol) available on the Batch
Distillation Safety web-page).
• Liquid will not begin accumulating in the standpipe until the reboiler temperature reaches
approximately 176°F. IF THE TEMPERATURE EXCEEDS 180°F seek assistance.
• It is recommended that samples be taken every 10 to 15 minutes during operation.
• Some recommended values for independent variables:
o Steam flow: 100 to 300 lb/h
o Distillate flow: no flow or at least 30 lb/h
o Water flow: valve 100% open unless control of the reflux temperature is desired

Modified: 4/24/2007 Kevin M. Sapp page 5/6


Original Document: Jullie Lawson © 2007
Department of Chemical Engineering
Unit Operations Laboratory

o Reflux ratio: R=3,4 provide good starting points; use theoretical calculations to
determine other reflux ratios for operation.
• There is no computer read-out for the distillate tank level or the water flow rate—be sure
to check the tank sight-glass and water rotameter every 15 minutes.
• If a valve malfunctions, use its corresponding manual bypass and notify the lab
supervisor.
• If you have any question about where a line goes, trace it!
• Do not always trust the computer monitor indications! Whenever possible, measure
variables another way to verify values.

Possible Objectives

Several tasks that have been the basis of previous projects include:

• Study the effect of changing different flows such as steam, water (affects reflux
temperature), reflux, and distillate on product composition. (Note dependencies between
these flows when planning—for example, to achieve a high distillate flow rate, you will
need a certain minimum flow rate of steam).
• Study the effect of changing the reflux ratio on product composition.
• Determine how to operate the column in order to achieve constant distillate composition.
• Determine the time to reach a specified product composition (either instantaneous
composition or collective composition of all distillate drawn off)
• Determine any or all of the following as a function of time at various reflux rates or
reflux ratios:
• distillate product composition
• bottoms product composition
• stage by stage temperature profile
• stage by stage composition profile
• stage by stage flow profile
• heat transfer rate to the condenser
• heat transfer rate to the reboiler
• Murphree efficiency

Note that your project may cover more than one of these objectives or additional objectives of
your own design.

Modified: 4/24/2007 Kevin M. Sapp page 6/6


Original Document: Jullie Lawson © 2007