1.

Abstract/summary

Regarding to the experiment objectives, which is to determine the pressure drop of the
distillation column for various boil-up rates in batch distillation, to observe the degree of
forming on trays for each power increment, to plot the curve relating pressure drop and boil-
up rate, to determine the refractive index for unknown concentration of
methylcyclohexane/toluene from the distillation column for each power increment. We do
this experiment using distillation column provided. To determine the pressure drop, we setup
different power which is 500W, 750W, 1000W, 1250W and 1500W. From the data collected,
we plot the graph of pressure drop versus boil-up rate. The graph shows that the pressure
drop is directly proportional to the boil-up rate. During experiment progress we observe that
there are three level of degree of forming which is gentle, flooding and forming. We collect
the data of refractive index for each power increment and put it in the observation table. To
determine the refractive index for unknown concentration, we mix the mixture of toluene and
methylcyclohexane in appropriate volume that we assume, and then we measure the
refractive index using refractometer. From the data, we plotted the graph of refractive index
versus percentage of toluene to find the percentage of toluene in the unknown concentration.

1
 2. Introduction

Distillation is defined as a process in which liquid or vapor mixture of two or more substances is
separated into its component fractions of desired purity, by the application and removal of heat.
Distillation is based on the fact that the vapor of a boiling mixture will be richer in the
components that have lower boiling points, therefore when this vapor is cooled and condensed,
the condensate will contain more volatile components. At the same time, the original mixture
will contain more of the less volatile material.
There are many types of distillation column, each designed to perform specific types of
separation, and each differs in terms of complexity;
I. Batch column: in batch operation, the feed to the column is introduced batch-
wise. That is, the column is charge with a `batch` and then the distillation process
is carried out. When the desired task is achieved, a next batch of feed is
introduced.
II. Continuous column: in contrast, continuous columns process a continuous feed
stream. No interruptions occur unless there is a problem with the column or
surrounding process unit. They are capable of handling high throughputs and are
the most common of the two types, trays column and packed column;
a. Binary column – feed contains only two components
b. Multi-component column – feed contains more than two components
c. Tray column(internal) – where trays of various design are used to hold up
the liquid to provide better contract between vapor and liquid
d. Packed column – where instead of trays `packings` are used to enhance
contact between vapor and liquid.

2
 Distillation columns are made up of several components, each of which is used either to
transfer heat energy or enhance material transfer. A typical distillation contains several major
components:
I. A vertical shell where the separation of fluid components is carried out
II. Column internals such as trays/plates or packings which are used to enhance
components separations
III. A reboiler to provide the necessary vaporization for the distillation process
IV. A condenser to cool and condensed the vapor leaving the top of the column
V. A reflux drums to hold the condensed vapor from the top of the column so
that liquid (reflux) can be recycle back to the column.
Operation and terminology; the liquid mixture that is to be processed is known as the
feed and this is introduced usually somewhere near the middle of the column to a tray known as
the feed tray. The feed tray divides the column into a top (enriching) section and bottom
(stripping) section. The feed flows down the column where it is collected at the bottom in the
reboiler. Heat is supplied to the reboiler to generate vapor. The source of heat input can be any
suitable fluid, although in most chemical plants this is normally stream. In vapor raised in the
reboiler is re-introduced into the unit at the bottom of the column. The liquid removed from the
reboiler is known as the bottom product.
The vapor moves up the column, and as it exits the top of the unit, it is cooled by a
condenser. The condensed liquid is stored in a holding vessel known as the reflux drum. Some of
this liquid is recycled back to the top of the column and this is called the reflux. The condensed
liquid that is removed from the system is known as the distillate or top product.
Thus, there are internal flows of vapor and liquid within the column as well as external flows of
feeds and product streams, into and out of the column.

3
4
 3. Aims/Objectives

The objectives of this experiment:

1. To determine the pressure drop of the distillation column for various boil-up rates in
batch distillation.
2. To observe the degree of forming on trays for each power increment
3. To plot the curve relating pressure drop and boil-up rate
4. To determine the refractive index for unknown concentration of
methylcyclohexane/toluene from the distillation column for each power increment.

5
 4. Theory

Distillation is a process of separating two or more miscible liquids by taking advantage of

the boiling point differences between the liquids. To understand how distillation works consider
the mixture of toluene and methylcyclohexane for this distillation experiment. Heat is added to
the mixture of toluene and methylcyclohexane and eventually the most volatile component (in
this case methylcyclohexane) begins to vaporize.
As the methylcyclohexane vaporizes it takes with it molecules of toluene. The
methylcyclohexane-toluene vapor mixture is then condensed and evaporated again, giving a
higher mole fraction of methylcyclohexane in the vapor phase and a higher mole fraction of
toluene in the liquid phase.
This process of condensation and evaporation continues in stages up the column until the
methylcyclohexane rich vapor component is condensed and collected as tops product and the
water rich liquid is collected as bottoms product. Figure below, illustrates the distillation column
used in the experiments.

6
 To understand distillation, first consider what happens upon heating a liquid. At any
temperature, some molecules of a liquid possess enough kinetic energy to escape into the vapor
phase (evaporation) and some of the molecules in the vapor phase return to the liquid
(condensation).
Equilibrium is set up, with molecules going back and forth between liquid and vapor. At
higher temperatures, more molecules possess enough kinetic energy to escape, which results in a
greater number of molecules being present in the vapor phase. If the liquid is placed into a closed
container with a pressure gauge attached, one can obtain a quantitative measure of the degree of
vaporization. This pressure is defined as the vapor pressure of the compound, and can be
measured at different temperatures.

7
 5. Apparatus

• Distillation column
• Methylcyclohexane 50mol%
• Toluene 50mol%
• Computer interface
• Automatic digital refactometer
• Distilled water
• Measuring cylinder
• Conical flask
• Stop watch

6. Procedure

8
a) Distillation column
1. Make sure all valves on the equipment are fully closed.
2. Open valve 10 (V10)
3. Fill the boiler with 10L of mixture consist of 50 mol% methyhcyclohexane and 50
mol% toluene which will be distilled. Make sure the filler cap was replaced.
4. Switch on the control panel power
5. Set the temperature selector switch to T9
6. Turn the power controller for the reboiler heating element fully anti-clockwise and
switch it on.
7. Adjust the power to 0.5kW; let it stabilized for 10 minutes.
8. Observe the degree of forming on the trays
9. Open valve 7 (V7) and valve 6 (V6) then record the pressure drop value using
manometer tube.
10. Open valve 3 (V3), collect 90ml of upper product volume (methylcyclohexane) and at
the same time record the time taken for volume to reach 90ml.
11. Repeat step 7 until 10 for 0.75kW, 1.0kW, 1.25kW and 1.5kW of power increment.

a) Finding refractive index using Refractometer

1. Take the refractive index value using automatic digital refractometer for each power
sample of product at each power increment.
2. Running the automatic digital refactometer:
i. Clean the surface using distilled water
ii. Switch on the power
iii. Press ZORE setting (SWL key)
iv. Press start key after placing the sample, record the refractive index value
v. Clean and switch off.

a) Non distillation mixing of methylcyclohexane and toluene

9
1. Assume 10ml of solution equal to 10 mol%
2. Let say sample A, mix 0 mol% methylcyclohexane with 100 mol% toluene using
conical flask.
3. Stir the solution carefully
4. Repeat step 2 until 3 for;
i. B (20 mol% methylcyclohexane, 80 mol% toluene)
ii. C (40 mol% methylcyclohexane, 60 mol% toluene)
iii. D (60 mol% methylcyclohexane, 40 mol% toluene)
iv. E (80 mol% methylcyclohexane, 20 mol% toluene)
v. F (100 mol% methylcyclohexane, 0 mol% toluene)
5. Record the refractive index value for all sample using automatic digital refractometer
6. Plot the pressure drop versus boil-up rate graph.
7. Determine the unknown concentration from refractive index versus percentage of
methylcyclohexane graph.

10
 7. Result

A. Using distillation column

Power (watt) Collection Boil-up rate Pressure drop Refractive index

time (s) (ml/s) (mm H2O)

500 85.2 1.056 68 1.43846

750 20.4 4.41 89 1.43911

1000 12.6 7.14 115 1.44028

1250 3.00 30 219 1.44708

1500 2.88 31.25 223 1.44785

Power (watt) Observation Concentration of unknown

(toluene mol %)

500 Gentle 21.4

750 Gentle 22.7

1000 Flooding 24.9

1250 Flooding 39.8

1500 Foaming 40.9

B. Without using distillation column (finding refractive index from mixing of solution)

Sample Mixture percentage (mol %) Refractive index

Methylcyclohexane Toluene

A 0 100 1.49685

B 20 80 1.48110

11
 C 40 60 1.46800

D 60 40 1.44726

E 80 20 1.43754

F 100 0 1.42310

Column temperature: 102 ºC

Process temperature: 104.9 ºC

Pressure drop versus boil-up rate graph

Refractive index versus percentage of toluene graph

12
 8. Discussion

Distillation is a commonly used method for purifying liquids and separating mixtures of liquids
into their individual components. Familiar examples include the distillation of crude
fermentation broths into alcoholic spirits such as gin and vodka, and the fractionation of crude oil
into useful products such as gasoline and heating oil. In the organic lab, distillation is used for
purifying solvents and liquid reaction products.
In this experiment we have to determine the pressure drop of the distillation column for
various boil-up rates in batch distillation, to observe the degree of forming on trays for each
power increment, to plot the curve relating pressure drop and boil-up rate, to determine the
refractive index for unknown concentration of methylcyclohexane/toluene from the distillation
column for each power increment.

After completing preparing and setup the equipment, we run the experiment. This
experiment can be divided into three stages. First is distillation at the distillation column, second
is finding refractive index using refractometer and third is non distillation mixing of
methylcyclohexane and toluene.

For distillation using the distillation column provided we need to determine the pressure
drop at each of power increment. Firstly we switch on the control panel and setup the power
value at 500 watt and wait for 10 minutes, this is done so that the solution of toluene and
methylcyclohexane stable, ready for the distillation process and the amount of product produce is
enough for the experiment. Although there is often slightly shift of power value at the control
panel, but we manage to get the constant value which we needed. This slight shift of power value
may affect the pressure drop and the condition in the distillation column.

After 10 minutes, we open the valve and start to estimate the pressure drop. At the same
time we also collect 90ml of upper product or in other name is distillate which is
methylcyclohexane and records the time taken to collect the sample. The sample was brought to
refractometer to measure its refractive index.

13
 To use refractometer, clean the lens of refractometer using distilled water and set the first
value by pressing the ZERO setting key, then after placing the sample start key was pressed. The
refractometer will indicate the refractive index for the sample automatically. We repeat the same
step for 750 watt, 1000 watt, 1250 watt and 1500 watt of each power increment.

For non distillation mixing of methylcyclohexane and toluene, we assume 10 ml solution

equal to 10 mol%, and then we setup 6 samples which have different amount of
methylcyclohexane and toluene but overall is 100ml. The samples were brought to the
refractometer to estimate its refractive index. All the data we tabulate in the table at the result
section.

In this experiment, methylcyclohexane become the upper product or distillate because it

has lower boiling point than toluene thus more volatile (boiling point for methylcyclohexane is at
101 °C meanwhile for toluene is at 110.6 °C).

We observe that there are 3 levels of vapor flow condition in the distillation column
during the distillation process which is firstly gentle, secondly flooding and third is foaming.
Gentle flow refers to the flow of vapor which in steady condition and no sudden abrupt rise
occurs. Flooding refers by excessive vapor flow, causing liquid to be entrained in the vapor up
the column. Forming refers to the expansion of liquid due to passage of vapor or gas. Although it
provides high interfacial liquid-vapor contact, excessive foaming often leads to liquid buildup on
trays.

We plotted the graph of pressure drop versus boil-up rate and graph of refractive index
versus percentage of toluene. From the graph it can be said that the pressure drop is directly
proportional to the boil-up rate. The second graph is used to find the percentage of toluene in a
unknown concentration.

During the experiment there are several precaution steps that need to be alert. Avoid
direct contact with distillation column because it is hot, use glove to hold the measuring cylinder
during taking the volume of methylcyclohexane, clean the refractometer surface using distilled
water before use that apparatus, after finish the experiment, collect back the sample of mixture
because it can be reused, use spectacles provided during collecting the sample and lastly the
solution is flammable, avoid it from the fire.

14
 Fractionating columns are widely used in the chemical process industries where large
quantities of liquids have to be distilled. Such industries are the petroleum
processing, petrochemical production, natural gas processing, coal
tar processing, brewing, liquefied separation, and hydrocarbon solvents production and similar
industries but it finds its widest application in petroleum refineries. In such refineries, the crude
oil feedstock is a very complex multicomponent mixture that must be separated and yields of
pure chemical compounds are not expected, only groups of compounds within a relatively small
range of boiling points, also called fractions and that is the origin of the name fractional
distillation or fractionation. It is often not worthwhile separating the components in these
fractions any further based on product requirements and economics.

9. Conclusion

15
1. At 500 watt the pressure drop in distillation column is 68 mmH2O, at 750 watt the
pressure drop is 89 mmH2O, at 1000 watt the pressure drop is 115 mmH2O, at 1250 the
pressure drop is 219 mmH2O and at 1500 the pressure drop is 223 mmH2O.
2. The degree of forming at 500 and 750 watt is gentle, at 1000 and 1250 watt the flooding
occurs and at 1500 watt the forming in the distillation column trays occurs.
3. According to the graph plotted, the pressure drop is potentially proportional to the boil-up
rate.
4. According to the graph plotted, concentration of toluene (mol%) at 500 watt is 21.4 mol
%, at 750 is 22.7 mol% at1000 watt is 24.9 mol%, at 1250 is 39.8 mol% and at 1500 is
40.9 mol%.

10. Recommendations

• Avoid direct contact with distillation column because it is hot

16
• Use glove to hold the measuring cylinder during taking the volume of methylcyclohexane
• Clean the refractometer surface using distilled water before use that apparatus.
• After finish the experiment, collect back the sample of mixture because it can be reused.
• Use spectacles provided during collecting the sample.
• The solution is flammable, avoid it from the fire.
• Make sure the eye is directly to the meniscus at the manometer ruler during taking the
pressure drop value.

11. References

• http://chem.engr.utc.edu/webres/435f/dist/DIST-96.HTML
• http://en.wikipedia.org/wiki/Distillation_column
• http://www.armfield.co.uk/pdf_files/uop3.pdf
• http://www.scribd.com/doc/12276923/Distillation
• Working Guide to Process Equipment, McGrawhill 2nd edition, Norman p.Lieberman,
Elizabeth t.Liberman.
• Unit Operation of Chemical Engineering, McGrawhill 7th edition, Warren L Mccabe,
Julian C.Smith, Peter Harriot.
• Process unit operation,CPE521 lecture notes (semester 3).

17
12. Appendices

18