UNIVERSITI TUNKU ABDUL RAHMAN (UTAR)

FACULTY OF ENGINEERING AND GREEN TECHNOLOGY (FEGT)

UGPA3071 PETROCHEMICAL LABORATORY
LAB REPORT: DISTILLATION USING TRAY COLUMN WITH REFLUX
Lecturer: Dr Yeoh
Group Members:
Name
1
2
3
4
5

Soo Hoo Weng Hong

Liew Chun Yih
Siow Kuai Qing
Moor Jie Wei
Yu Gen Qian

1. Objectives

ID
13AGB03516
13AGB05776
13AGB02711
14AGB05536
13AGB05459

Course
PE
PE
PE
PE
PE

Year/Sem
Y3/S1
Y3/S1
Y3/S1
Y3/S1
Y3/S1

a. To operate a distillation column with constant reflux ratio.

b. To carry out mass balance calculations on the distillation column.
c. To compare the performance for packed and tray column for distillation process.
2. Introduction
Distillation is a main unit operation in many chemical industries and process industry. It
is used for the separation of components in a liquid mixture of volatile constituents, and can be
carried out in a continuous or batch system. Distillation can be used to separate binary or multicomponent mixtures by using the concept of application and removal of heat to exploit
differences in relative volatility. The heat causes higher volatility components to be vaporized,
leaving less volatile components as liquids. Mixtures with high relative volatilities are easier to
separate, but separations of close-boiling and azeotropic feeds are difficult, hence special
distillation techniques can be apply to separate these mixtures (Naik, n.d.). Distillation will
produce product of desired quality rich in concentration of one component of the original
solution.
Various types of distillation columns designed to perform specific types of separations. In
batch operation, the feed to the column is introduced in batch-wise which the column is charged
with a 'batch' and then the distillation process is carried out. After the desired task is achieved, a
next batch of feed is introduced.
Continuous columns process a continuous feed stream. There are two types, which are
tray column and packed column. Tray column is where trays are used to hold up the liquid to
provide better contact between vapour and liquid, hence better separation while for packed
column is 'packings' are used to enhance contact between vapour and liquid (Naik, n.d.).
This experiment is designed to study the distillation of a binary mixture of ethanol and
water in a packed distillation column.
2.1 Theory

Figure 2.1 shows the vapour-liquid equilibrium curve (x-y diagram) and the operating line for the
distillation process under general reflux.
The

general

equation

of

the

operating

line

can

be

expressed

as:

where R is the reflux ratio and xd is the mole fraction of the liquid distillate collected at the top.

As the reflux ratio is increased, the gradient of the operating line for the rectification section
moves towards a maximum value of 1. Physically, what this means is that more and more liquid
that is rich in the more volatile components are being recycled back into the column.
If the distillation is carried out in a plate column, it is possible to calculate the number of
theoretical plates that are required for the distillation. This makes it possible to define a height of
the packed column which effects separation of a mixture equivalent to a theoretical plate. The
height so calculated is known as the Height Equivalent to a Theoretical Plate (HETP). If the
column is to be packed then the height of packing can be estimated from:
H = N x HETP
Where H = packing height

2.2 Equipment: Description and Assembly

The distillation column is made of borosilicate 3.3 glass with PTFE gaskets and stainless steel.
Please refer to the process flow diagram in Figure 2 and the description of labeling in Table 1.
1

Reboiler (B1) a 10 L horizontal reboiler equipped with two 1,5 kW cartridge heaters
(W1a & W1b). The reboiler is supplied with liquid level switch LS-01, a temperature
probe TIC-201. The reboiler also comes with a charge port for feeding, a drain valve is
fitted at the bottom of the reboiler.

Sieve Tray Column (K1) a DN 50 borosilicate column with 10 sieve trays and equipped
10 temperature probes, which are TI-101 until TI-110. A temperature probe TT-112 is
available for distillate temperature measurement. A differential pressure sensor is also
provided to measure the pressure drop across the sieve tray column. Column height:
approx. 1m.

Top condenser- a high efficiency condenser with 0.5

m2 exchange area and cooling

water connections.
4

2
Product cooler having 0.035 m exchange area and cooling water connections.

Product Tank (B3 & B4) a 5 L graduated tank with venting connection and valves.

Feed Tank (B2) a 30L cylindrical tank with discharge and venting.

Table 1: Description of Tags in Figure 1

Tag
TT 101 to TT110
TT 111
TT 112
TIC 201
FI 102
KS 01

Description
Column temperature
Feed temperature
Top column temperature
Reboiler temperature
Entrainer flowrate
Timer
based
reflux

Units
C
C
C
C
ml/min
s

Range
0.0-100.0
0.0-100.0
0.0-100.0
0.0-100.0
0.0-150.0
0-9999

controller
Position 1 : total reflux
Position 2 : total distillate
Position 3 : timer controlled
DPT 301
W1a & 1b
LS 01

reflux
Differential pressure
Heater power
Reboiler level switch

mmH2O
W
-

3. Procedures
3.1 Operation with Constant Reflux Ratio (Postion 3 in KS 01)

0-400
0-3000
-

1. The reboiler B1, feed tank B2, product tank B3 and B4 was washed. The mixture of
ethanol and water was prepared. The percentage of alcohol was recorded.
2. The general start-up procedures was performed as described in the operating manual.
3. The refractive index calibration curve was performed for ethanol-water mixture with
various composition. The data was recorded in Table 2.
2. The reflux timer was set to x second for set 1 and y second for set 2.
3. When the distillate started to condense into the product tank B3, the feed pump P1 was
switched on. The pump stroke was set to obtain a flow rate of approximately 60 mLPM. Then the
reflux control (KS-01) was set to position 3.
4. Once the distillation column has reached stable condition, the top and bottom temperatures
were recorded.
5. The samples from the distillate and bottom product were collected.
6. The refractive index for all samples were measured and their compositions were determined.
The data was recorded in Table 3.
7. The steps 5 to 7 were repeated at regular intervals of 10 minutes until the bottom sample RI
values reached constant.
8. When samples were done collected, heater power was switched off.
9. The calibration curve for data collected was plotted.

4. Result
Table 2: Composition Table Based on Refractive Index

Purity of ethanol: 99%

Density of ethanol: 790.6 kg/
m3
Density of water:

1000 kg/

m3
Volume

of Volume

of Mole

fraction Wt%

Refractive

ethanol (mL)

water (mL)

ethanol

ethanol

index (RI)

10

0.000

0.000

1.3333

0.033

8.075

1.3393

0.072

16.480

1.3420

0.117

25.270

1.3460

0.171

34.470

1.3477

0.235

44.100

1.3501

0.316

54.200

1.3530

0.418

64.800

1.3556

0.552

75.940

1.3569

0.735

87.667

1.3588

10

1.000

100.000

1.3580

Graph 2: Calibration Curve for Refractive Index (RI) versus Ethanol Mole Fraction

Graph of refractive index (RI) against mole fraction of ethanol

1.37
1.36

1.36

f(x) = 0.05x^3 - 0.12x^2 + 0.09x + 1.34

R = 0.98

1.36
1.35
1.35
1.34
1.34
1.33
1.33
1.32

0.2

0.4

0.6

0.8

Table 3: Composition Table Based on Refractive Index for Distillate and Bottom Product
Heater power: 2kW
Reflux ratio: 3
% of ethanol in the feed stream: 0.072% (20vol %)
Time
Distillate
Bottom Product
Temp ( Refract.
Mole
Temp ( Refract.
(min)
index
Fraction
index
)
)
0
72.8
10
74.0
20
74.6
30
74.7
40
75.5
50
75.6
5. Discussion

1.3450
1.3459
1.3457
1.3471
1.3464
1.3464

0.1257
0.1404
0.1371
0.1612
0.1489
0.1489

89.1
89.6
89.7
89.8
89.4
89.8

1.3411
1.3410
1.3408
1.3404
1.3393
1.3398

Mole
Fraction
0.069
0.0676
0.065
0.0597
0.0457
0.052

1.2

Using McCabe-Thiele method to determine theoretical number of plates for each time
intervals from t= 0 mins until t = 50mins at every 10 minutes intervals. The graphs were shown
as below and using the presented values to calculate the height equivalent theoretical plates
(HETP)
T=0mins

Figure 6: McCabe-Thiele Diagram at time = 0minutes

XD = 0.1257
XB = 0.069
Number of stages calculated = 0.8 (Checalc.com, 2015)
Height equivalent theoretical plates,

HETP=

H
n plate

= 1/0.8m
=

T=10mins

1.25

Figure 6: McCabe-Thiele Diagram at time = 10minutes

XD = 0.1404
XB = 0.0676
Number of stages calculated = 1 (Checalc.com, 2015)

Height equivalent theoretical plates,

HETP=

H
n plate

= 1/1m
= 1m

T=20mins

Figure 6: McCabe-Thiele Diagram at time = 20 minutes

XD = 0.1371
XB = 0.065
Number of stages calculated = 1(Checalc.com, 2015)
Height equivalent theoretical plates,

HETP=

H
n plate

= 1/1 m
=1m

T=30 mins

Figure 6: McCabe-Thiele Diagram at time = 30 minutes

XD = 0.1621
XB = 0.0597
Number of stages calculated = 1.5(Checalc.com, 2015)
Height equivalent theoretical plates,

HETP=

H
n plate

= 1/1.5 m
= 0.667 m

T=40mins

Figure 6: McCabe-Thiele Diagram at time = 40 minutes

XD = 0.1489
XB = 0.0457
Number of stages calculated = 1.8 (Checalc.com, 2015)
Height equivalent theoretical plates,

HETP=

H
n plate

= 1/1.8 m
= 0.556 m

T=50mins

Figure 6: McCabe-Thiele Diagram at time = 50 minutes

XD = 0.1489
XB = 0.052
Number of stages calculated = 1.6(Checalc.com, 2015)
Height equivalent theoretical plates,

HETP=

H
n plate

= 1/1.6 m
= 0.625 m

Table 4: Mole fraction of water and ethanol at 50min

Distillate product
Xethanol
0.1489

Bottom product
Xethanol
0.052

Xwater
0.8511

In order to find total pressure of distillate and bottom product,

Raoults Law was apply:
P= x i P isat
Using Antoine Equation to calculate Psat :
I n Psat =A

B
t ( C ) +C

Where Water

Where Ethanol

A: 16.3872

A: 16.8958

B: 3885.79

B: 3795.17

C: 230.170

C: 230.918

For Distillate (Ethanol)

I n Psat Distillate Ethanol =16.8958

I n Psat Distillate Ethanol =4.2122

sat
Distillate Ethanol

=67.5030 kpa

3795.17
68.3+230.918

Xwater
0.948

For Distillate (Water)

I n Psat Distillate Water =16.3872

3885.79
68.3+230.170

I n Psat Distillate Water=3.3682

sat
DistillateWater

=29.025 kpa

For Bottom (Ethanol)

I n Psat Bottom Ethanol =16.8958

3795.17
88.4+ 230.918

I n Psat Bottom Ethanol =5.0511

sat
Bottom Ethanol

=149.9892kpa

For Bottom (Water)

InP

sat
BottomWater

=16.3872

3885.79
88.4+230.170

InP

sat
BottomWater

=4.1860

Psat Bottom Water=65.9963 kpa

Therefore total pressure for distillate was:

P= x Distillate Ethanol P

sat
Distillate Ethanol

+ x Distillate Water P

sat
Distillate Water

0.1489 67.5030 kpa+ 0.8511 29.025 kpa

P=

P=34.754 kpa

While the total pressure for bottom was:

P= x Bottom Ethanol P

sat
Bottom Ethanol

+ x Bottom Water P

0.052 149.9892 kpa+ 0.948 65.9963 kpa

P=

P=70.3639 kpa

sat
Bottom Water

To find gas mole fraction, y of Ethanol:

x Ethanol P sat Ethanol
y Ethanol =
P

For Distillate Ethanol:

x
P
y Distillate Ethanol = Distillate Ethanol
P
y Distillate Ethanol =

sat
Distillate Ethanol

0.1489 67.5030 kpa

34.754 kpa

y Distillate Ethanol =0.2892

For Bottom Ethanol

x Bottom P sat Bottom Ethanol
y Bottom Ethanol =
P
y Bottom Ethanol =

0.052 149.9892 kpa

70.3639 kpa

y Bottom Ethanol =0.1108

Relative volatility formula:
=

y Ethanol ( 1x Ethanol )
x Ethanol ( 1 y Ethanol )

Distillate
Distillate=

y Distillate Ethanol ( 1x Distillate Ethanol )

x Distillate Ethanol ( 1 y Distillate Ethanol )

 Distillate =

0.2892 ( 10.1489 )
0.1489 ( 10.2892 )

Distillate=2.3256
Bottom product
Bottom=

Bottom=

y Bottom Ethanol ( 1x Bottom Ethanol )

x Bottom Ethanol ( 1 y Bottom Ethanol )
0.1108 ( 10.052 )
0.052 ( 10.1108 )

Bottom=2.2716

Average Relative Volatility formula:

1

avg=( Distillate Bottom) 2

Therefore
1

avg=( 2.3256 2.2716 ) 2

avg=2.2984 (apply McCabeThiele Diagram)

To find Minimum number of stages, N, Fenske Equation was applied:

log
Minimum number of stages , N =

x Distillate ethanol
1x Bottom ethanol

1x Distillate ethanol
x Bottom ethanol

log avg

log
Minimum number of stages , N =

0.1489
10.052

( 10.1489
0.052 )
log2.2984

Minimum number of stages , N =1.852

Underwood equation was applied to calculate the minimum reflux ratio in a column.
Underwood equation was obtained from (Wolfram Demonstrations Project, 2015) as follow:

st

1 Equation:
Where Xi, F

NC

i=1

ij

ijiF =1q
denotes mole fraction of i in feed

denotes root of equation

ij

denotes volatility of component i relative to heaviest component

denotes feed quality

As saturated liquid was fed in the experiment, q=1

ww x wF ew x eF
+
=11
ww ew

, w denotes water

e denotes ethanol
1 0.928 2.2984 0.072
+
=0
1
2 .2984
0.928
1

=-

0.1655
2 .2984

-2.1329+ 0.928 = 0.1655 0.1655

1.0935 = 2.2984
=2.102

nd

2 Equation :

NC

i=1

ij

ijiD =Rmin+1

ww x wD ew x eD
+
=Rmin +1
ww ew

, w denotes water
e denotes ethanol

1 0.8511 2 .2984 0.1489

+
=Rmin +1
12.102 2 .29842.102
-0.7723 + 1.8262 = Rmin + 1
Minimum Reflux Ratio , Rmin =0.054

3. From this experiment, the top and bottom products that were collected from the distillates and
had their refractive indices tested and recorded for a total of 50 minutes with 10 minutes interval
and totaling up to 6 top products and 6 bottom products. While conducting the experiment, a
calibration curve of the refractive index against the mole fraction of ethanol is plotted. These
values were taken as the theoretical values for the experiment data. To measure the refractive
index differing ratios of volume of water and ethanol are tested to retrieve the refractive index

and to plot the calibration curve. These ratios range from 0:10 water to ethanol to 10:0, these
refractive indices are then recorded in a table to be used to plot the calibration curve. From the
calibration curve an equation is obtained, that is:
y = 0.0539x3 - 0.1217x2 + 0.0908x + 1.3354
Where the,
X = mol fraction of ethanol in the sample
Y = refractive index of the sample.
This equation is used to calculate the mole fraction of ethanol in the sample. These values are
calculated as 0.1257, 0.1404, 0.1371, 0.1612 and 0.1489 for the top product and 0.069, 0.0676,
0.065, 0.0597, 0.0457 and 0.052 respectively for the bottom products. From the results collected
it is shown that the top product has a higher concentration of ethanol compared to the bottom
product, this is due to ethanol being more volatile when compared to water and boils quicker and
collects at the condenser at the top of the distillation column.

For the theoretical amount of stages, the McCabe-Thiele method is used. By using the
mole fractions of both top and bottom products and their refractive indices. The differences in
the refractive indices of the top and bottom products affects the theoretical amount of plates that
are required for distillation. The larger the difference the lesser the amount of plates required and
vice versa. The mole fractions also relate to the amount of theoretical plates by inverting the way
refractive index works with the amount of theoretical plates, the higher the difference of mol
fraction in the products, the more plates required. In Question 1 in the above sections,
calculations were made to prove that the larger the amount of theoretical plates the HETP of the
column decreases. From McCabe-Thiele method, the average theoretical amount of plates
required from 6 sets of data were 1.3 and the minimum amount of stages calculated from the
Fenske Equation is 1.852.

While the experiment was conducted, the reflux ratio was maintained to a constant value
of 3. This is because it allows the calculation of the theoretical amount of stages. During the

experiment, the reflux timer for both set 1 and set 2 is adjusted to a 30seconds interval. Set 1 of
the reflux timer is used to manage the interval where liquid is allowed to re-enter the distillation
column and set 2 of the reflux timer is used to manage the feed that enters the reboiler. The
purpose is to ensure that there is enough product inside the column to ensure the production of a
top product and a bottom product. In order to determine the minimum reflux ratio, Underwoods
Equation is used and the value determined is 0.054 which is lower than the constant value that is
set.

In this experiment, there are unavoidable errors that will cause inaccuracies in the data
collected which will lead to the discrepancies in the data calculated, first off while collecting the
top product, some of the ethanol might have evaporated due to it being very volatile. This also
applies to the measuring of the refractive index while using the refractometer.

4. Bubble cap column is a bell shaped cap which covered the holes in each tray of distillation
tower. Each bubble cap assembly consists of a riser and a cap. The cap is mounted to create free
spaces for the raising vapor through the liquid on the tray. The raising vapor is directed
downward by the cap and then discharging through the slot in the cap and finally releases to the
liquid. The caps creates the continuous contact between rising vapors and liquid. This ensure the
maximum contact of both phases and also increase the effectiveness of mass transfer between
vapor and liquid (Werner, n.d.).
Packed column is the pack tower that filled up with layers of devices called packing
(Wakao & Kaguei, 1983). There are many types of packing. The purpose of packing is to
distribute the liquid so it flows over a large amount of surface area and exposed more liquid to
vapor. This eventually increase the total contact area between two phases and also increase the
mass transfer from the vapor to the liquid (Naik, n.d.).
There are few considerations needs to be taken when comparing the performances of bubble cap
and packed column (SM, n.d.).

Operating range

Bubble cap column can be used to handle a wider range of liquid and vapor flow rates but
packed column is not suitable for very low liquid flow rates. Thus, bubble cap column
can be used in high turndown condition.

Pressure drop
Packing has the advantage of a lower pressure drop across the column compared
to bubble cap column which is beneficial while operating under vacuum.

Maintenance
Bubble caps is having difficulty in cleaning as they are most susceptible to plugging and
packed column is easier to clean.

Liquid hold-up
Packed column has the lower liquid hold-up compared to bubble cap column. This is an
important issue when hazardous liquid is used and must be kept as small as possible for
safety purposes.

Cost
Packed column is cheaper than bubble cap column due to its simple design.

In conclusion, packed column is the cheapest and are satisfactory for most applications but
bubble cap column is better for specific applications.
6. Conclusion
Tray distillation column is suitable for separation of water-ethanol mixture as it requires
small number of stages to obtain high concentration of volatile component and low minimum
reflux ratio. Tray distillation column will be cost effective as it requires less stages in the column.

7. References
1.

S.

Naik.

n.d.. DISTILLATION

COLUMNS.

[ONLINE]

Available

at:

http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationColumns/Distill
ationColumns.html. [Accessed 13 July 2016].

2. Wakao, N. & Kaguei, S.. 1983. Heat and mass transfer in packed beds. Netherlands: Harwood
Academic (Medical, Reference and Social Sc.) [Accessed 13 July 2016]

3.
SM.
n.d.. Plant
operations:
Trays
types.
Available
http://www.separationprocesses.com/Operations/POT_Chp02a.htm [Accessed 13 July 2016]

at:

4. Werner Slken. n.d.. Distillation column: Column Internals, bubble cap trays, valve trays,
sieve

trays,

structured

packing.

Available

at:

http://www.wermac.org/equipment/distillation_part2.html [Accessed 13 July 2016]

5. Checalc.com. (2015). Binary Distillation McCabe Thiele Diagram. [online] Available at:
http://checalc.com/calc/binary.html [Accessed 14 Jul. 2016].