Professional Documents
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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
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
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.
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.
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
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
1.36
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
HETP=
H
n plate
= 1/0.8m
=
T=10mins
1.25
HETP=
H
n plate
= 1/1m
= 1m
T=20mins
HETP=
H
n plate
= 1/1 m
=1m
T=30 mins
HETP=
H
n plate
= 1/1.5 m
= 0.667 m
T=40mins
HETP=
H
n plate
= 1/1.8 m
= 0.556 m
T=50mins
HETP=
H
n plate
= 1/1.6 m
= 0.625 m
Distillate product
Xethanol
0.1489
Bottom product
Xethanol
0.052
Xwater
0.8511
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
sat
Distillate Ethanol
=67.5030 kpa
3795.17
68.3+230.918
Xwater
0.948
3885.79
68.3+230.170
sat
DistillateWater
=29.025 kpa
3795.17
88.4+ 230.918
sat
Bottom Ethanol
=149.9892kpa
sat
BottomWater
=16.3872
3885.79
88.4+230.170
InP
sat
BottomWater
=4.1860
P= x Distillate Ethanol P
sat
Distillate Ethanol
+ x Distillate Water P
sat
Distillate Water
P=34.754 kpa
P= x Bottom Ethanol P
sat
Bottom Ethanol
+ x Bottom Water P
P=70.3639 kpa
sat
Bottom Water
sat
Distillate Ethanol
y Ethanol ( 1x Ethanol )
x Ethanol ( 1 y Ethanol )
Distillate
Distillate=
Distillate =
0.2892 ( 10.1489 )
0.1489 ( 10.2892 )
Distillate=2.3256
Bottom product
Bottom=
Bottom=
Bottom=2.2716
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
st
1 Equation:
Where Xi, F
NC
i=1
ij
ijiF =1q
denotes mole fraction of i in feed
ij
, w denotes water
e denotes ethanol
1 0.928 2.2984 0.072
+
=0
1
2 .2984
0.928
1
=-
0.1655
2 .2984
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
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: