BACHELOR OF CHEMICAL ENGINEERING (HONS)

LAB REPORT SUBMISSION FORM

EKC 2131 CHEMICAL ENGINEERING LAB III

NAME Nisha Fareena Khan ID 1102171011

EXPERIMENT NO. & TITLE PACKED BED DISTILLATION COLUMN
EXP 6
WEEK OF EXPERIMENT 2
DATE OF EXPERIMENT 5/11/2019
DATE OF SUBMISSION 12/11/2019

NAME OF GROUP MEMBERS ID

Nisha fareena Khan 1102171011
Mathaneshan Rajagopal 1103173003

MARKING SIGNATURES
DETAILS TOTAL MARKS
AWARDED
Attitude 5
Participation 5

Lab Report 40 CHEMICAL ENGINEERING LAB III

INCHARGE
Total 50
(DR. PADMESH/MS. MADIHAH MISKAN)

On-time submission Late submission

0
Table of Content

1. Abstract ………………………………………………………. 2
2. Objective ………………………………………………………. 3
3. Introduction …………………………………………………….. 3-7
4. Procedure …………………………………………………….8-10
5. Result and Discussion …………………………………………..11-13
6. Conclusion and Recommendation ………………………………14
7. References …………………………………………………..15
8. Appendices …………………………………………………..16-19

1
1.0.Abstract

Most of the processes in chemical industry are involved in purifying

components. As a consequence, a large part of the energy use in many industrial
sectors can be attributed to separation processes. Distillation is the dominant
separation technology in chemical industries despite its huge energy consumption.
Distillation consumes about 3% of the total energy consumed globally.The main
objectives of this experiment is to study the operation of packed bed distillation
column, and to operate the column under total reflux and desired reflux condition
using Fenske’s and Mc-Cabe Thiele’s methods. The number of stages obtained
from the total reflux is tend to be 4.3 and frm the 4:15 and 10:15 desired reflux
tends to be 8 and 16 stages respectively. Solving Rayleigh’s equation and calculate
the feed and bottom feed moles that tend out to be 47 moles and 11.61 moles
respectively. After the nuber of theoretical stages were find through Frenke’s
equation the HETP value was calculated to be 0.234m with the height of the column
be 0.90m. The refractive Index obtained for total reflux for top and bottom distillate
is 1.319 and 1.32 respectively. The ROL obtained in both the cases of desired reflux
are 0.56 and 0.74.

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2.0.Objective
The main objectives are:
1.1 To study the operation of a packed bed distillation column.
1.2 To verify the rayleigh equation.
1.3 To operate the column under total reflux condition and calculate the minimum
number of theoretical stages using fenske’s equation.
1.4 To operate the column under any desired reflux condition and calculate theoretical
number of stages using Mc-Cabe Thiele’s method.
1.5 To calculate the HETP for known packed height.

3.0.Introduction
1. Principles:

Distillation is by far the most common process used in petroleum and chemical
industries for separation of liquid mixtures by the difference of their relative volatility
or boiling points. Distillation is preferred over other separation processes due to its
advantages like less time consumption, better efficiency and ability to treat greater
volumes of mixture. The basic requirement of separation of two components by
distillation is that the composition of vapour is different from the composition of liquid
with which it is in equilibrium with the boiling point of the liquid. If relative volatility
is very close to 1, they have similar vapour pressures and hence, it will be difficult to
separate the two components by distillation. Distillation is a unit operation capable of
producing pure substance from liquid mixtures (Geankoplis, 1993, p643).

Continuous process distillation is used widely for large industries whereas, batch
distillation is preferred by small industries where it is economical for small scale
separation processes. Some sectors in a pharmaceutical industries, high value added
chemicals and bio-chemical industries prefer batch operation as it is highly useful in
separation of mixture that become viscous upon concentration (Geankoplis, 1993,
p644).

Packed columns are used for distillation operation when the separation is easy and
the column diameter is relatively not too large. Packed column are generally less
expensive then plate columns are have low pressure drop. Packed columns can be

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designed by the same method used for adsorption column where it depends on the
overall transfer coefficient and the height of transfer units. The height of the column is
usually based on the number of theoretical plates and the height equivalent to a
theoretical plate (HETP) (McCabe_W.L._Smith_J.C._Harriott_P, 1993, p576).
For the calculation of height equivalent to theoretical plate (HETP):

Several examples of metal, plastic, and ceramic type packing are shown in the
picture below.

Figure 2.1: Different types of packing.

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 The feed contains components of different volatilities, and enters the column almost
at the middle. The liquid flows in direction of gravity through the packing, and the
vapour flows upward through the column. Differences in concentration cause the less-
volatile components to change from the vapour phase to the liquid phase. The packing
increases the time of contact, which raises the separation efficiency. The exiting vapour
contains the more volatile components, while the liquid product stream reads low in
volatile components (Bravo, Jose L. and James K. Fair, 1990, p19-29).

Figure 2.2: Distillation column with packed bed.

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 Batch distillation with only a single still does not give a good separation unless the
relative volatility is very high. To obtain product with a narrow composition range, a
rectifying batch still is used that consist of a reboiler, a rectifying column, a condenser,
some means of splitting of a portion of condensed vapor or distillate as reflux and the
receiver. The operation of a batch still and column can be analyzed using the same
operating line equation as for the rectifying section of the continuous distillation:

Since the slope of the operating line is R / (R+1), the slope increases as the reflux
increases, until when reflux is infinite. Under total reflux slope is 1. The operating line
then coincides with the diagonal. The number of plate is minimum at total reflux.
Minimum number of plates required can be calculated from the terminal concentration
of xB and xD based on the relative volatility of the components α, which is defined in
terms of equilibrium concentrations:
Minimum number of theoretical plates required:

The above equation is known as fenske’s eqn. The final ratio does not change much
over the range of temperature encountered in a typical column, so the relative volatility
is taken as constant.

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 2. Applications:
 Distillation columns are widely used in refining oil from crude oil.
 Distillation plants supply water to areas that have scarcity of water by
purification.
 Liquor, wine and beer are produced by means of distillation.
 Cosmetic product, pharmaceutical product, and chemical products if on a small
scale are produced using packed bed distillation.
 Packed beds are also used in certain variants of the distillation and absorption
processes referred to as strippers and scrubbers.

3. Advantages and Disadvantages:

Advantages Disadvantages
1. Cost efficient distillation column 1. Packing can break during
as the diameter is less the 0.6m. installation or due to thermal
2. The packed beds are able to expansion.
handle corrosive material as the 2. For high liquid flow rates it is not
packing are made of inert cost efficient.
material. 3. During low flow rate liquid
3. Lower pressure drop therefore contact efficiency is reduced.
preventing column flooding. 4. Not efficient in handling solid or
4. Good for thermally sensitive other source of fouling.
liquids.

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4.0.Procedure

Opening Procedure

1. A standard curve of x vs R.I at methanol water ratio from 0 – 1 was prepared.

2. The volume of water and methanol was noted down.
3. All the valve V1-V16 were kept in closed position.
4. Switches on the panel were at OFF position.
5. Water was filled in the cold water tank.
6. The reboiler was filled with methanol-water solution, valve V1 and air vent
valve V2 were opened.
7. After on valve V1 and V2 were closed.
8. Electric supply was connected to set up.
9. The process temperature was set at 95°C.
10. The heater and cooling water pump were started.
11. The cold water flow rate valve V3 was adjusted to a moderate value.
12. Cyclic timer for total reflux was set.
13. Waiting time was 25-30 minute for the system to achieve steady state.
14. The samples were taken from the bottom & distillate stream.
15. Samples were cooled down to room temperature in order to measure the
refractive indices.
16. Refractive indices of samples at different temperatures were measured.
17. The temperature and refractive indices were noted.
18. The cyclic timer was adjusted to a desired reflux ration and for 3-5 min.
19. The samples from both distillate and bottom product were taken out.
20. Samples were cooled down to room temperature and refractive indices were
measured.
21. Refractive indices of samples at different temperatures were measured.
22. The refractive indices were measured.
23. The experiment for different set point temperatures and reflux ratios was
repeated.
Closing Procedure:
1. When the experiment was over water supply was shut down.
2. The pump, heater, and main power supply were Switch OFF.
3. The column, reflux drum and receiving tank were drained.

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Figure 4.1 shows the block diagram of packed bed distillation column. The set-up
consists of a column, which is packed with glass rings. An electric heater or reboiler is
installed at the bottom of the column. A tank is provided to collect the bottom product.
Shell and tube type condenser is provided to condensate the vapour. A tank with pump
and rotameter is provided for circulation of cooling water. Reflux drum is provided to
collect the condensate. Receiving tank is for collecting the distillate. Drain valves are
provided for drainage purposes.

Figure 4.1: Block diagram of packed bed distillation column.

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Formulas:

Rayleigh’s Equation

It is used to find the Feed composition or composition of the bottom distillate. For batch
distillation process where a fixed quantity of feed is charged to the distillation column
and separation of volatile products is done by supplying heat through the still or
reboiler. As the boiling point of liquid is reached a portion of liquid starts to vaporize
to the top of the column and directed to the condenser, the vapor leaving the column is
always in equilibrium with the liquid in the bottom of the column, thus a material
balance equation is produced by Rayleigh called Rayleigh Equation which provides
standard equilibrium data (Neutrium, 2016, Distillation).

Fenske’s Equation

The Fenske equation in continuous fractional distillation is an equation used for

calculating the minimum number of theoretical plates required for the separation of a
binary feed stream by a fractionation column that is being operated at total reflux (i.e.,
which means that no overhead product distillate is being withdrawn from the column).

Mc-Cabe Thiele’s method

To calculate the slope of the feed line.

Fraction of liquid in the feed.

y = ( q/ q − 1 ) x – (xF /(q – 1)) To calculate the q-line.

ROL=xd/R+1 Rectifying operating line(y-intercept).

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 5. Result and Discussion

The McCabe-Thiele method uses the equilibrium curve diagram to determine the
number of theoretical stages require to achieve a desired degree of separation. The main
information required are the feed conditions, distillate, feed composition, and the
bottom composition and reflux ratio (Neutrium, 2016, Distillation). If a column is
designed to follow the MaCabe- Thiele’s method for separation of a binary mixture
where the feed has concentration of xf, the bottom distillate has a concentration of xw,
and the top distillate has a composition of xd. The method involves plotting the diagram
into 3 sections the rectifying section operating line (ROL), the feed line and the
stripping section line (SOL). The number of theoretical stages can be determine from
the number of triangles that can be drawn between the operating lines.

In this experiment one sample was collected to determine the total reflux of the
solution, whereas two samples were to indicate the desired reflux of the solution
provided that was methanol- water. The set temperature was 95⁰C, and the total reflux
the value of R (Reflux Ratio) is 1. The values of xf, xd, and xw were obtained from the
calibration chart using the mole fraction of methanol and the value of R.I obtained by
the composition of methanol- water as shown in the table 1 in appendix. Where the
values of xd=0.87 xf=0.23 and xw=0.02. These values are obtained from the graph 5.1
where the refractive Index were used to determine the composition of the feed, top and
bottom reflux. The following refractive Index used are shown in the table 2 appendix.
From the graph 5.1 the values are calibrated and used further in the experiment.

Furthermore the equilibrium data of methanol-water separation is shown in table

5.2. From this data the Boiling point was required to be determined. The graph 5.3
shows the equilibrium data constructed.

Tthe 100 96.4 93.5 91.2 89.3 87.7 84.4 81.7 78.0 75.3 73.1 71.2 69.3 67.5 66.0 65.0 64.5

Xthe 0 0.02 0.04 0.06 0.08 0.1 0.15 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0.95 1.0

Ythe 0 0.134 0.23 0.304 0.365 0.418 0.517 0.579 0.665 0.729 0.779 0.825 0.87 0.915 0.958 0.979 1.0

Table 5.2: T-x-y date for ethanol water system.

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 As we know that the composition is equal to the feed composition i.e xf the
temperature is equal to the bubble temperature of the feed tBP. From the graph 5.3 the
corresponding boiling temperature shown that corresponds to xf=0.23 is 80.5⁰C.
Therefore the bubble point of the feed tBP=80.5⁰C.Feed temperature selected as it is
entering at room temperature = 25⁰C.Average temperature tBP =52.75⁰C. Acurve is
drawn from the vapour liquid data. Whereby the value of xb, xf and xd are plotted on
the diagonal of the curve. As for total reflux the value of q such as the fraction of liquid
in the feed is 1 therefore the graph. The number of theoretical stages are calculated by
counting the rectangle constructed with in the graph 5.4 as shown.

For the desired reflux the graph 5.5 where L:D ratio is 4:15 where the value of
R is to be 0.267. After getting the value of q from the latent heat of the solution the
value of q calculated id to be 1.108. In order to give a clear description of the figure 5.5
the following steps were used to calculate the theoretical number of stages.

1. Points 𝑥 , 𝑥𝐷 and 𝑥𝐹 were marked on the diagonal of the equilibrium curve

shown above.
2. From 𝑥 , the q line was drawn till it cut the equilibrium curve.
3. Points 𝑥𝐷 were joined and extended till the y-axis.
4. The intercept on y-axis = 0.617 = xD/Rm+1 , where Rm = minimum reflux
ratio.
5. On putting value of 𝑥𝐷 , we get, Rm = 0.617
6. For industrial apparatus of distillation column, R = 1.2 Rm = 0.264
7. Intercept of rectifying section operating line (ROL) on y-axis = xD/R+1 = 0.74
8. The above intercept was marked on the y-axis and joined with point XD which
gave the ROL. The point where it cut the q line was marked.
9. The points B and XB were joined to get the stripping section operating line
(SOL). These steps were constructed according to the McCabe Thiele method.

We can get ideal number of stages = 8 as shown in the graph 5.5. For the graph 5.6
the desired reflux ratio used is 10:15, where R is 0.667 and Rm is 0.556 the ROL value
is 0.56. The number of ideal stages obtained from the 10:15 graph is 16. The value of
xd,xf and xw are 0.94, 0.23 and 0.01 respectively. As from the Franske’s equation the
number of stages calculated theoretically is 3.83 which is significantly close to the no
of stages obtained from the total reflux graph 5.4. The HETP calculated for the N 3.83

12
was to be 0.234 with the height given to be 0.90 m. The minimum number of stages
obtained from Fenske equation for practical and experimental calculations are 3.8 under
total reflux. This implies that our equipment is working fine.

The deviations in the curve or the calibration chart is due to error in measurement
and error in equipment therefore the readings consist of instrumental and graphical
error. The number of stages obtained from total reflux is 4.3 and from desired reflux is
8 and 16. The total reflux after removing the reboiler and the condenser is 2. That is
near to the theoretical value from Frenke’s equation.

Refractive Index Refractive Index Xd Xw

Top Bottom
1.319 1.32 0.87 0.02
1.317 1.32 0.94 0.02
1.317 1.315 0.94 0.01
Table 5.6: Refractive Index with composition

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 6. Conclusion and Recommendation

As per the observations the current setup can be made as an 8 tray column by
replacing the reboiler, which would further act as an ideal tray. This in turn would
increase the degree of separation and reduce the operating time. As for the desired
reflux ratio due to error in observation the 4:15 and 10:15 reflux ratio gave us 8 and 16
stages/trays to complete distillation respectively.

Further calculations taking into account the diameter, height and other parameters
of the distillation column which will give us more insight to the column internals and
hence the problem are being done. The minimum number of stages obtained from
Fenske’s equation for practical and experimental calculations are 3.8 under total reflux.
This implies that our equipment is working fine. The molar composition of the feed and
the bottom reflux is obtained by Rayleigh’s equation.

As per recommendations, the molar composition or the mass value of the feed
should be informed further with the handling of the temperatures with time. The water
should be clear from any impurities to ensure no wastage of power and heat. The
measurement in refractive index should have minimum error.

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7. References
1. Bravo, Jose L. and James K. Fair, 1990, "Distillation Columns." Chemical
Engineering Progress: p19-29. [online].[Accessed 10th November,2019].
Available from World Wide Web:

http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/Distillat
ionColumns/DistillationColumns.html.

2. Geankoplis, 1993, “Transport Process and Unit Operation” (Edition 3rd).

University of Minnesota: Simple Distillation methods, p.643-644.
3. McCabe_W.L._Smith_J.C._Harriott_P, 1993, “Unit Operation of Chemical
Engineering” (5th Edition). McGraw-Hill, Inc.: Distillation. P576-577.
4. Neutrium, 2016, “Unit Operations and Distillations”. [online].[Accessed 10th
November,2019]. Available from World Wide Web:
https://neutrium.net/unit-operations/distillation/mccabe-thiele-plot/

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 8. Appendix

Data

Relative volatility α 3.32

Molecular weight of methanol MM 32 g/mole
Molecular weight of Water MW 18 g/mole
Enthalpy of feed HF 0 kJ/kmole
Packed height Z 0.90 m

N Volume Volu Mass of Mass Moles Mole Mole Refrecti

o of me of Methan of of s of fraction ve Index
Methan Water ol Wate Methan Wate of
ol (ml) (0.79*V r ol r Methan
(ml) ) (1*V (mol) (mol) ol
(g) ) X
(g)
1 0 10 7.9 0 0.247 0 1 1.3185
2 1 9 7.11 1 0.222 0.056 0.799 1.3215
3 2 8 6.32 2 0.198 0.111 0.641 1.323
4 3 7 5.53 3 0.173 0.167 0.509 1.3255
5 4 6 4.74 4 0.148 0.222 0.400 1.326
6 5 5 3.95 5 0.123 0.278 0.307 1.326
7 6 4 3.16 6 0.099 0.333 0.229 1.3278
8 7 3 2.37 7 0.074 0.389 0.160 1.3255
9 8 2 1.58 8 0.049 0.444 0.099 1.3245
10 9 1 0.79 9 0.025 0.500 0.048 1.321
11 10 0 0 10 0 0.556 0 1.315

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 Table 1: Observation table for calibration Chart.

Time Top Reflux Bottom reflux

Total Reflux 1.319 1.32
4:15 1.317 1.32
10:15 1.317 1.315
Table 2: Refractive Index of distillates.

Refractive Index Refractive Index Xd Xw

Top Bottom
1.319 1.32 0.87 0.02
1.317 1.32 0.94 0.02
1.317 1.315 0.94 0.01
Table 3: Refractive Index with composition.

McCabe-Thiele method:

80.5+25
Average temperature tBP = = 52.75⁰C.
2

Calculation of q value: q = λF + CPF(tBP − tF ) λF

Where, tBP – Bubble point of feed

tavg – Average temperature

λF – Latent heat of methanol-water feed mixture at tBP

CPF – Heat capacity of methanol-water feed mixture at tavg

From Perry’s handbook,

Latent heat of water at 80.5°C (tBP), λW = 4.16 x 104 J/mol

Latent heat of methanol at 77°C, λM = 3.43 x 104 J/mol

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Therefore,

λF = (xF*λM) + ((1-xF)*λW) = ((0.23)*(3.43 x 104 )) + ((0.77)*(4.16 x 104 )) =

39990.00 J/mol

Heat capacity of water at 53.5°C (tavg), CPW = 75.34 J/mol-K

Heat capacity of methanol at 53.5°C, CPM = 87.46 J/mol-K

Therefore, CPF = (xF*CPM) + ((1-xF)*CPW) = ((0.23)*(87.46)) + ((0.77)*(75.34)) =

78.1276 J/mol-K

After putting values, we get, q = 1.108

Equation of q line:

y = ( q/ q − 1 ) x – (xF /(q – 1))

After putting values of xF and q, we get:

y = 10.25x – 2.12

ROL=xd/R+1 =0.74

Rm=xD/Rm+1=0.617

R=L/D=0.267

Rayleigh’s Method

For the composition of total reflux values:

𝑿
𝟑𝟐 = 𝟎. 𝟐𝟑
𝑿 (𝟏 − 𝑿)
𝟑𝟐 + 𝟏𝟖

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Therefore,

X=0.35

(1-X) = 0.65

As the compositions of the feed.

So F = 0.047 Kmol = 47.04mol.

Putting values into Rayleigh’s equation to find B which is the outlet moles of the
bottom product.

47.04(1−0.23)
3.32ln[ ]
𝐵(1−0.01)

B = 11.61 mol

D = F-B

D = 47.04 – 11.61 = 35.39 mol.

Fenske’s Equation

For the composition of total reflux values:

Nm =(log [ 0.87(1-0.02)/0.02(1-0.87)]/log3.32)-1

Nm = 3.83 no of stages.

Height equivalent to theoretical plate (HETP).

0.90
HETP = 3.83 = 0.234m.

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