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This schematic illustrates what happens in a distillation column. A liquid mixture is fed into the
distillation column. On entering the column, the heated feed is partially vaporized and rises up
the column. However, as it rises, it cools by contacting the descending cooler liquid and partially
condenses so that, while part of vapor continues to flow upward, the condensed portion is
enriched in the less volatile component(s) and flows downward. As the vapor continues to flow
upward, it undergoes partial condensation a number of times and each time becomes richer in the
more volatile component(s).
Unit Operations Lab 4
March 11, 2010
Group 3
Shrikant Shah
Brandon Farr
Alex Georg
Michael Ogiefo
Mohammed Khatib
Ghassan Alkhateeb
Unit Operations ChE-382 Group No. 3
p. 1
Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
Spring 2010
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Binary Distillation
1.
Table of Contents
WP&C.....................................................................................................................................2
1.
Introduction............................................................................................................................3
2.
Theory......................................................................................................................................5
3.
Apparatus..............................................................................................................................13
4.
5.
Procedure..............................................................................................................................19
8.
Error Analysis.......................................................................................................................21
9.
References.............................................................................................................................22
1. WP&C
What is the purpose of this experiment?
The purpose of this experiment is separate a mixture of a 5% wt methanol-water solution in a binary distillation
column. About 0.1-2 GPM of methanol-water mixture will be introduced into the round bottom flask of the column.
The column will operate at temperatures ranging from 0-100oC. The column will be run and allowed to reach steady
state before samples from the six stages will be obtained and tested with a Refractometer to eventually obtain the
methanol concentration in each stage.
What are the hazards associated with the experiment?
1. Methanol is relatively toxic fluid. It can cause eye, skin and respiratory tract irritation when carelessly
exposed to lab personnel.
2. The electrical wires for the thermocouples are carelessly exposed. If lab personnel were to accidentally touch
them while conducting experiment, they run the risk of an electric shock.
3. The persistent use of fluids like water and methanol could lead to fluid spillage. If lab personnel were to walk
over an affected area, they run the risk of injuries due to a fall.
How will the experiment be conducted in a safe manner?
1. Lab personnel should wear gloves, goggles, slip resistant shoes, and a facemask when conducting experiment
especially when handling the methanol.
2. Paper towels or task wipers should be in close proximity to clean up any fluid spills that may occur during
experiment.
3. The Distillation column should not be heated until the mixture has reached the Reboiler section of unit.
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Signatures:
Shrikant Shah
Brandon Farr
Alex Georg
Michael Ogiefo
Mohammed Khatib
Ghassan Alkhateeb
1. Introduction
Distillation is a physical separation process that uses the differences in volatility between
compounds in a liquid mixture. Binary distillation separates two liquid components from one
another. All fluids possess some degree of volatility that is a measure of their tendency to
vaporize. A higher volatile compound such as methanol will vaporize more quickly when
compared to water under the same atmospheric conditions. Boiling the two components would
also make the difference even more apparent, as the less volatile water would boil at a higher
temperature than the methanol. More importantly, even when two components are mixed
together, the unique physical properties of the individual component still causes the more volatile
component to vaporize faster. This is what ultimately makes distillation possible.
A single step of distillation uses these principles of volatility to achieve a separation of
compounds at equilibrium. At the boiling point of a mixture, the more volatile component exists
as a greater fraction in the vapor than it will in the liquid. In a methanol-water mixture,
distillation would yield a greater mole fraction of methanol in the vapor than in the liquid.
Unit Operations ChE-382 Group No. 3
p. 3
Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
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Binary Distillation
Condensing the vapor and adding more distillation steps or stages in series is the basis for
continuous distillation. When a continuous system is arranged vertically, the system is defined
as a distillation column. In such a column, falling liquids vaporize at lower stages and rising
vapors condense at higher ones. A heat source at the bottom of the column enables this action,
creating a decreasing temperature gradient up the column. With more distillation steps greater
purity can be achieved in top and bottom of the column.
Distillation columns are widely used for separations in industry, most notably in
petroleum, natural gas, and chemical processing, as well as any other large-scale liquid
production. In processing petroleum, different hydrocarbons can be separated according to their
volatility. Medicinal herbs can be distilled from plant matter in the pharmaceutical industry.
Methanol is distilled for high alcohol content products such as whiskey.
In this experiment, we will distill a mixture of methanol and water in a column distiller.
The apparatus has six trays that will act as the stages of the continuous distillation. Collection of
the condensate at each of these stages will allow an analysis of the composition at each plate.
The temperature will also be recorded at each stage. Ultimately, decreasing temperatures and
increasing compositions of methanol will be observed up the column. Finally, vapor-liquid
equilibrium data will allow a comparison between experimental results and theoretical trends.
2. Theory
Distillation is the separation, by vaporization, of different components in a mixture
because of the different volatilities that they possess at a given boiling point of the mixture.
When a mixture reaches a specific temperature and pressure a certain amount of the mixture
moves into the vapor phase until the vapor reaches the mixtures vapor pressure. This point is
known as the vapor-liquid equilibrium. Volatility is a measure of a pure components vapor
Unit Operations ChE-382 Group No. 3
p. 4
Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
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Binary Distillation
pressure at a set pressure and temperature in a specific mixture. It is incorrectly assumed that the
components of a mixture will separate based on their boiling points when pure. Rather, the
boiling point of a mixture is based on the total vapor pressure of a mixture, which is a sum of the
vapor pressures of each individual component in the mixture. This is known as Daltons law.
sat
P = (v pa + v pb )
(1)
Where,
sat
v pa
v pb
This means that a component will not boil off cleanly meaning it is impossible through
distillation to obtain a pure substance. The vapor created above a mixture is also a mixture of
components. The composition of the vapor is based on the volatility of each of the substances.
Raoults law helps us to determine what the volatility, or K value of a substance. This in turn
allows us to find the mole fraction of a component in the vapor phase.
y a=
v pa x a
(2)
psat
Where:
ya
v pa
xa
Psat
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Not all mixtures obey Raoults law. Some components that have high solubility with each
other form azeotrope. An azeotrope is a mixture that has either a higher or lower boiling point
than the boiling point of any of the pure components. This means that when a mixture reaches an
azeotrope, such as ethanol and water at 95.6 % water, it behaves as a pure substance.
The simplest of all distillation techniques is called flash distillation. Flash distillation occurs
when a mixture at a specific temperature and pressure is allowed to drop in pressure. This
changes the vapor-liquid equilibrium of the mixture and creates a vapor rich in the most volatile
component(s). This is also the crudest form of distillation and does not allow for refinement of
the distillates.
A more complicated form of distillation is batch distillation. Batch distillation uses both a
boiler and a condenser, but only allows one separation, or cut, to be taken from the mixture.
Figure 1: A schematic of a typical continuous distillation tower. A is the kettle that holds the
liquid mixture, B is the Reboiler that adds heat to the mixture, C is the distillation column that
holds the trays or packing, D is the condenser that turns the distillate to a liquid product.
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Continuous distillation is the most complicated and most common form. It has a boiler,
condenser and multiple trays or packing which allows the vapor to condense as it moves up the
column and cools. The trays or packing allows for a better separation of the components in the
mixture which in the end gives purer products. It also adds a lot of complexity to the system.
Figure 2: A typical tray in a distillation column. A is the tray itself, B are the holes in the tray
that allow the vapor to pass through the tray, C and D are the tubes that allow liquid to pass from
one tray to another. As the vapor moves up the column it gets progressively cooler which allows
some of the mixture to condense and further concentrates the vapor with the lightest
component(s).
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Figure 3: This shows a simple McCabe-Thiele diagram. The number of steps corresponds to the
number of trays needed for a given mixture.
Determining the size of the tower and the number of trays needed was historically a very
difficult process involving many calculations. The McCabe-Thiele method greatly simplified that
process. The method uses a graphical representation of the material balance equations as
operating lines on a graph of the liquid composition (x-axis) and the vapor composition (y-axis).
The bottom line in Figure 3 is the x-y line. This starts at the origin and ends where x and y both
equal 1.This line would represent a distillation column that operated at total reflux and total boilup, meaning that all of the vapor and all of the liquid is recycled back into the system. The next
line added is the vapor liquid equilibrium line for a binary system which is found
experimentally. By moving step-wise between the two lines we can find the number of
theoretical plates needed for a specific separation of a binary mixture and the liquid and vapor
composition at any point in the distillation column. These stage lines can be seen in Figure 3.
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Figure 4: McCabe-Thiele diagram with operating lines and feed line added.
In practice, we want to draw a purified product out of the column in the form of either a
distillate (top of the column) or the bottoms product (bottom of the column) or both. This
requires a column that operates at a partial reflux and/or a partial boil-up ratio. This means that
we cannot use the x-y line for such a column. In Figure 4 we see the addition of a line for reflux
ratio (slope L/V) and a line for the boil-up (slope L/V). The boil-up lines slope increases as we
increase the amount of bottoms product that we remove from the system. Subsequently, as we
remove more distillate as product we decrease the slope of the top operating line, which is the
line for the reflux ratio. By changing the amount of liquid re-boiled, which is liquid returned to
the column as a vapor, or by changing the amount of vapor refluxed, returned to the column as a
liquid, we change the number of theoretical plates necessary for a given separation. The q
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(quality) line in Figure 4 is the feed line which is the composition of the stream entering the
distillation column. We can see from the diagram in Figure 4 that where that line intersects with
the two operating lines is the feed stage, or the tray at where the incoming stream enters.
The quality q is defined as:
q=
H h f
LL
F
Hh
(3)
Where:
ZF
q
( q1
) x + 1q
(4)
Where:
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( )
(5)
Where:
The McCabe-Thiele method is widely used for binary mixtures. When dealing with multicomponent mixtures addition assumptions and calculations are necessary. There are a number of
issues that need to be watched when sizing a continuous distillation column properly. They are:
Foaming- foaming occurs when the gas passing upward causing the liquid to bubble
excessively. While this normally depends on the properties of the liquid, it can also be caused by
improper tray designs.
Entrainment- Occurs when the vapor velocity is too high due to a column having too
small of a diameter. This causes liquid to be held up at the trays and does not allow proper
circulation of the liquid.
Weeping- Occurs when the vapor velocity is too low. When the velocity drops too low,
liquid starts to fall, or weep, through the holes in the plates. This does not allow enough liquid to
get to the re-boiler which means that the entire column needs to be shut down and re-started.
Flooding- This occurs when liquid entrainment become too severe. This causes a large
pressure drop in the column and contaminates the distillate.
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3. Apparatus
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22
24
T8
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Figure 5 represents the Binary Distillation apparatus without any of the support beams. The column is
constructed of a round bottom flask (7) which holds a methanol- water solution. This solution is distilled by
applying electrical energy to the heating jacket (24) which heats up the solution causing the volatile liquids and
gases to rise. Total reflux occurs in the system by feeding cooling water (10) into a cooling coil (16) at the top
of the column. Thermocouples (T1-T9) measure the temperatures at various points in the system and output
them onto an electrical temperature monitor (21). Liquid and gaseous samples are taken at ever one of the 6
stages via sample ports (L1-L6 &G1-G6) and tested with a Refractometer to calculate the density and
eventually the composition of the samples.
Table 1: Binary Distillation Apparatus Summary (For Figure 5)
Component No.
Apparatus Component
Manufacturer
Description
Notes/Safety
1
MCD
Funnel
Na
Nalgene
Nalgene
Swagelok
Na
Nalgene
Na
10
11
Cold Chicago
Faucets
12
Marsh Instrument
Company
13
Cold Chicago
Faucets
14
Schutte &
Koerting Co.
15
Temperature Gauge
Moeller
16
Cooling Coil
Na
17
Temperature Gauge
Weksler
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18
Cold Chicago
Faucets
19
Heat Controller
Na
20
Powerstat
21
Monogram
22
Thermocouples
Omega
23
Square D Safety
Switch
24
Na
Component No.
Celsius.
Allows cooling water to exit system
and drain.
Used to turn on heaters individually
including heating jacket.
Conducts electricity and passes it into
the heating jacket
Displays temperature taken at the
different thermocouples.
Measure temperature at different
stages in distillation column.
Reading outputs on Digital
temperature display
Controls the electricity passing into
the electric heating jacket turning it
either on or off.
Heats the bottom of the distillation
column electrically.
T1
Omega
T2
Stage 1 Thermocouple
Omega
T3
Stage 2 Thermocouple
Omega
T4
Stage 3 Thermocouple
Omega
T5
Stage 4 Thermocouple
Omega
T6
Stage 5 Thermocouple
Omega
T7
Stage 6 Thermocouple
Omega
T8
Omega
T9
Omega
Component
No.
G1
Notes/Safety
Make sure probe is secure and
tube is filled with white oil.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Pay close attention to
temperature so column does not
overheat.
Na
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G2
Na
G3
Na
G4
Na
G5
Na
G6
Na
L1
Na
L2
Na
L3
Na
L4
Na
L5
Na
L6
Na
Tap Water
Lake Michigan
White Oil
Chevron Superla 5
Used in preparation of
Methanol-water solution.
Used inside the
temperature probe tube
within the round bottom
flask.
Methanol
Aldrich Chemical
Company
Ice
Micropipette
Na
Notes/Safety
Clean up any spillage
immediately.
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Test Tubes
Refractometer
Graduated Cylinder
Nalgene
Task wipers
Kimberly Clark
Professional
breakage immediately if it
occurs.
Clean up any glass
breakage immediately if it
occurs.
Use caution when
handling. Calibrate before
operation.
Clean up any spillage
immediately.
Clean any mess or spillage
promptly.
5. Procedure
Distillation Column Operation:
1. Make a 5 mol% methanol solution by mixing it with water in the 13 gallon feed tank (4)
using graduated cylinders for measurement.
Note: make sure not to over fill the round bottom flask (7). It only needs to be filled
halfway or until the thermocouple (T1) is in contact with the mixture.
2. Pour the methanol-water mixture into the feed container and turn ON the three-way valve
in order to fill up the round bottom flask.
3. Open the cooling water supply valves (11 & 13) to supply cooling water to the distillation
column.
4. Start up the distillation column by turning on the power supply switches (22) to supply
heat to the distillation column.
5. Record the temperature of each of the thermocouples (T1-T9) located throughout the
column by analyzing the digital temperature monitor (21). Also record the readings of
the inlet cooling water temperature gauge (12), the outlet cooling water temperature
gauge (17), the inlet cooling water pressure gauge (15), and the cooling water rotameter
(14).
6. Make sure to collect the samples at each stage via the sample ports (G1-G6 &L1L6) of the distillation column and record the index of refraction by using the
Refractometer.
7. After the distillation process is done, make sure to turn OFF the heater power supply,
and the cooling water supply.
Operating the Bausch & Lomb Abbe-3L Refractometer:
1 Make mixtures from 10% Methanol with water to 100% Methanol in small test tubes
Unit Operations ChE-382 Group No. 3
p. 17
Shah, Farr, Georg, Ogiefo, Khatib, Alkhateeb
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using a pipette.
2 Turn ON the Refractometer and the water heating system.
3 Open the prism assembly and remove the tissue.
4 Use a capillary tube to apply your liquid sample to the prism and close the prism
assembly.
NOTE: Be careful not to let the glass pipette tip touch the prism since this may scratch the
prism glass.
5
6
Adjust the toric lens, so the light shines on the prism and look through the eyepiece.
Analyze the index of refraction of the sample:
a When the index of refraction of your sample is close enough, then you will see
lighter region on the top and darker region on the bottom.
b If you cannot distinguish between these two regions then adjust the compensator
scale dial of the machine and the toric lens until the dark and light region is
completely separated.
Note: it is an iteration process between adjusting the light and the focus wheel located on the
front of the Refractometer.
c Once the clear distinguishable line between dark and light region is seen then
press the momentary contact switch located on the left hand side of the machine
until you see the scale. Then read off the index of refraction by looking at the
top scale and the refined bottom scale.
7 After you have noted down the index of refraction, record the temperature by
reading the temperature scale.
8 Make sure to clean the prism after testing each sample with a solvent and dabbing it with
tissue.
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8. Error Analysis
Component
Nalgene
0.5mL
Electronic Balance
0.01g
Temperature Gauges
Weksler
&
Moeller
1 oF
Monogram
0.1 oC
0.0001
Refractometer
Description
Listed above are components of the binary distillation lab whose specific uncertainties would
directly affect our recoded data. If these uncertainties were to occur, they would affect our
overall results by adding specific uncertainties to them.
9. References
1. Wankat, Phillip C.; Separation Process Engineering, second edition, Prentice Hall,
2007
2. R. Bird, W. Stewart, E. Lightfoot. Transport Phenomena. Wiley, 2006
3. Towler, G. and Sinnott, R., Chemical Engineering Design: Principles. BH, 2008
4. W. McCabe, J. Smith, and P. Harriot, Unit Operations of Chemical Engineering. 7th
ed. McGraw-Hill, 2005.
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9. Bennett C.O., Myers J.E., Momentum, Heat, and Mass transfer. 3 rd edition New York.
McGraw-Hill, 1982.
10. Wikipedia: http://en.wikipedia.org/wiki/Distillation
11. Website: http://lorien.ncl.ac.uk/ming/distil/distil0.htm
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