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 ID Course Year/Sem
1. Soo Hoo Weng Hong 13AGB03516 PE Y3/S1
2. Liew Chun Yih 13AGB05776 PE Y3/S1
3. Siow Kuai Qing 13AGB02711 PE Y3/S1
4. Moor Jie Wei 14AGB05536 PE Y3/S1
5. Yu Gen Qian 13AGB05459 PE Y3/S1
1. Objectives

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 multi-
component 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.
2. 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.
3. Top condenser- a high efficiency condenser with 0.5 m 2exchange area and cooling water
connections.
4. Product cooler –having 0.035m 2exchange area and cooling water connections.
5. Product Tank (B3 & B4) – a 5 L graduated tank with venting connection and valves.
6. Feed Tank (B2) – a 30L cylindrical tank with discharge and venting.
Table 1: Description of Tags in Figure 1
Tag Description Units Range
TT 101 to TT110 Column temperature ̊C 0.0-100.0
TT 111 Feed temperature ̊C 0.0-100.0
TT 112 Top column temperature ̊C 0.0-100.0
TIC 201 Reboiler temperature ̊C 0.0-100.0
FI 102 Entrainer flowrate ml/min 0.0-150.0
KS 01 Timer based reflux s 0-9999
controller
Position 1 : total reflux
Position 2 : total distillate
Position 3 : timer controlled
reflux
DPT 301 Differential pressure mmH2O 0-400
W1a & 1b Heater power W 0-3000
LS 01 Reboiler level switch - -

3. Procedures

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

 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)
0 10 0.000 0.000 1.3333
1 9 0.033 8.075 1.3393
2 8 0.072 16.480 1.3420
3 7 0.117 25.270 1.3460
4 6 0.171 34.470 1.3477
5 5 0.235 44.100 1.3501
6 4 0.316 54.200 1.3530
7 3 0.418 64.800 1.3556
8 2 0.552 75.940 1.3569
9 1 0.735 87.667 1.3588
10 0 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) = 0.05 x³ − 0.12 x² + 0.09 x + 1.34
1.36 R² = 0.98

1.35

1.35

1.34

1.34

1.33

1.33

1.32
0 0.2 0.4 0.6 0.8 1 1.2

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. Mole
(min)
℃) index Fraction ℃) index Fraction
0 72.8 1.3450 0.1257 89.1 1.3411 0.069
10 74.0 1.3459 0.1404 89.6 1.3410 0.0676
20 74.6 1.3457 0.1371 89.7 1.3408 0.065
30 74.7 1.3471 0.1612 89.8 1.3404 0.0597
40 75.5 1.3464 0.1489 89.4 1.3393 0.0457
50 75.6 1.3464 0.1489 89.8 1.3398 0.052
5. Discussion

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)
H
Height equivalent theoretical plates, HETP=
n plate

= 1/0.8m
= 1.25 m

T=10mins
Figure 6: McCabe-Thiele Diagram at time = 10minutes
XD = 0.1404
XB = 0.0676
Number of stages calculated = 1 (Checalc.com, 2015)

H
Height equivalent theoretical plates, HETP=
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)
H
Height equivalent theoretical plates, HETP=
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)
H
Height equivalent theoretical plates, HETP=
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)
H
Height equivalent theoretical plates, HETP=
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)
H
Height equivalent theoretical plates, HETP=
n plate

= 1/1.6 m
= 0.625 m

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

 Distillate product Bottom product
Xethanol Xwater Xethanol Xwater
0.1489 0.8511 0.052 0.948

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

Raoult’s Law was apply:

P=∑ xi Pisat

Using Antoine Equation to calculate Psat :

B
I n P sat =A−
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)

3795.17
I n P sat Distillate Ethanol =16.8958−
68.3+ 230.918

I n P sat Distillate Ethanol =4.2122

Psat Distillate Ethanol =67.5030 kpa

For Distillate (Water)

 3885.79
I n P sat Distillate Water=16.3872−
68.3+230.170

I n P sat Distillate Water=3.3682

Psat Distillate Water =29.025 kpa

For Bottom (Ethanol)

3795.17
I n P sat Bottom Ethanol =16.8958−
88.4 +230.918

I n P sat Bottom Ethanol =5.0511

Psat Bottom Ethanol =149.9892 kpa

For Bottom (Water)

3885.79
I n P sat BottomWater =16.3872−
88.4+230.170

I n P sat BottomWater =4.1860

Psat BottomWater =65.9963 kpa

Therefore total pressure for distillate was:

P=∑ x Distillate Ethanol P sat Distillate Ethanol + x DistillateWater Psat Distillate Water

P=∑ 0.1489× 67.5030 kpa+¿ 0.8511 × 29.025 kpa¿

P=34.754 kpa

While the total pressure for bottom was:

P=∑ x Bottom Ethanol P sat Bottom Ethanol + x BottomWater Psat BottomWater

P=∑ 0.052× 149.9892kpa+ ¿ 0.948× 65.9963 kpa ¿

P=70.3639 kpa
To find gas mole fraction, y of Ethanol:

x Ethanol Psat Ethanol

y Ethanol =
P

For Distillate Ethanol:

x Distillate Ethanol P sat Distillate Ethanol

y Distillate Ethanol =
P

0.1489× 67.5030 kpa

y Distillate Ethanol =
34.754 kpa

y Distillate Ethanol =0.2892

For Bottom Ethanol

x Bottom Psat Bottom Ethanol

y Bottom Ethanol =
P

0.052 ×149.9892 kpa

y Bottom Ethanol =
70.3639 kpa

y Bottom Ethanol =0.1108

Relative volatility formula:

y Ethanol ( 1−x Ethanol )

α=
x Ethanol ( 1− y Ethanol )

Distillate

y Distillate Ethanol ( 1−x Distillate Ethanol )

α Distillate =
x Distillate Ethanol ( 1− y Distillate Ethanol )

0.2892 ( 1−0.1489 )
α Distillate =
0.1489 ( 1−0.2892)

α Distillate =2.3256
Bottom product

y Bottom Ethanol ( 1−x Bottom Ethanol )

α Bottom=
x Bottom Ethanol ( 1− y Bottom Ethanol )

0.1108 ( 1−0.052 )
α Bottom=
0.052 (1−0.1108 )

α Bottom=2.2716

Average Relative Volatility formula:

1
α avg=( α Distillate × α Bottom ) 2

Therefore

1
2
α avg=( 2.3256 × 2.2716 )

α avg=2.2984 (apply∈McCabe−Thiele Diagram)

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

x Distillate ethanol 1−x Bottom ethanol

Minimum number of stages , N =

log
( 1−x Distillate ethanol
×
x Bottom ethanol )
log α avg

0.1489 1−0.052
Minimum number of stages , N =
log ( 1−0.1489 ×
0.052 )
log 2.2984
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:

NC
α x
1st Equation: ∑ α ij−θiF =1−q
i=1 ij

Where Xi, F  denotes mole fraction of i in feed

θ denotes root of equation

α ij denotes volatility of component i relative to heaviest component

q denotes feed quality

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

α ww x wF α ew x eF
+ =1−1 , w denotes water
α ww −θ α ew−θ

e denotes ethanol

1× 0.928 2 .2984 ×0.072

+ =0
1−θ 2 .2984−θ

0.928 0.1655
=-
1−θ 2.2984−θ

-2.1329+ 0.928 θ =0.1655– 0.1655 θ

1.0935 θ = 2.2984

θ=2.102

NC
α x
nd
2 Equation : ∑ α ij −θiD =Rmin+ 1
i=1 ij
α ww x wD α ew x eD
+ =Rmin +1 , w denotes water
α ww−θ α ew −θ

e denotes ethanol

1× 0.8511 2 .2984 ×0.1489

+ =R min +1
1−2.102 2.2984−2.102

-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 at:

http://www.separationprocesses.com/Operations/POT_Chp02a.htm [Accessed 13 July 2016]

4. Werner Sölken. 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].