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Done By:
ID No:
Experiment Date: Submission
Date:
Lab. Supervisor: Prof. Tareq Al-Bahri Lab.
Instructor:
Lab Report Grading
List of Figures
Figure 1: Schematic diagram of Distillation Column............................................................................6
Figure 2: Flow diagram of combined bubble-cap and packed distillation column.................................7
Figure 3: X –Y Diagram Total Reflux Bubble Cape Colum................................................................10
Figure 4: X –Y Diagram Partial Reflux Bubble Cape Column............................................................11
Figure 5: X –Y Diagram Total Reflux Packed Column.......................................................................12
Figure 6: X –Y Diagram Partial Reflux Packed Column.....................................................................13
Figure 7: Vol% Ethanol in water vs refractive index...........................................................................17
Figure 8: T-xy Diagram for ethanol water system...............................................................................17
List of Tables
Table 1: Efficiency calculation for bubble column at total reflux........................................................11
Table 2: Q re-boiler calculation for bubble column at total reflux.......................................................11
Table 3: Qcondesor calculation for bubble column at total reflux.......................................................11
Table 4: Qloss calculation for bubble column at total reflux...............................................................11
Table 5: Efficiency calculation for bubble column at Partial reflux.....................................................12
Table 6: Q re-boiler calculation for bubble column at Partial reflux....................................................12
Table 7: Qcondesor calculation for bubble column at Partial reflux....................................................12
Table 8: Qloss calculation for bubble column at Partial reflux............................................................12
Table 9: Efficiency calculation for packed column at total reflux.......................................................13
Table 10: Q re-boiler calculation for packed column at total reflux....................................................13
Table 11: Qcondesor calculation for packed column at total reflux.....................................................13
Table 12: Qloss calculation for packed column at total reflux.............................................................13
Table 13: Efficiency calculation for packed column at Partial reflux..................................................14
Table 14: Q re-boiler calculation for packed column at Partial reflux.................................................14
Table 15: Qcondesor calculation for packed column at Partial reflux..................................................14
Table 16: Qloss calculation for packed column at Partial reflux..........................................................14
Table 17: Data Sheet Bubble Tray Column.........................................................................................17
Table 18 : Data Sheet Packed Column.................................................................................................17
Table 19: volume % vs Refractive Index Table...................................................................................18
Table 20: Equilibrium data for ethanol water mixture.........................................................................18
Nomenclature:
NTS Number of theoretical stages
NA Actual number of stages
Eo Overall efficiency of the column
HETS Height equivalent to a theoretical stage
Introduction:
Distillation is a major commercial process used in the chemical and petroleum industries. It
is a physical separation process used to separate the liquid into different products based on
the difference in volatility (difference in boiling point). There are many types of distillation
columns, some of them are: Bubble-cap, packed bed, ballast trays and perorated (Sieve)
plates. This experiment examines two types of distillation columns Bubble-cap and Packed.
A bubble cap tray has some holes that a riser is fitted in each hole. And the riser is covered
by a cap. The vapor inside will be flowing up through the tower and contacts the liquid by
passing through bubble caps. Then the vapor is turned downward to bubble into the liquid
surrounding. Bubble cap trays cannot weep, this is because of their design. And they cost
more than valve trays and sieve trays. Bubble cap was mounted in a rectifying column that
concentrates the alcohol. Packed columns are commonly found in absorption, distillation,
stripping, heat exchangers and other operations, like removal of dust, mist and odors and for
other purposes. The distillation column contains one feed stream and two product streams.
The feed which is liquid introduced continuously at the midpoint (feed tray) into the column.
The product stream exiting the top is the overhead product (distillate). And the other product
stream leaving is called the bottom. The column has two sections. The top section is referred
to as the rectifying section (enriching). The bottom section is known as the stripping section.
Theoretical Background:
Using the McCabe-Thiele diagram, the number of theoretical stages (NTS) can be extracted
using the graphical data. They can also be numerically determined by solving the mass
balance for each stage composition with consideration of two sections including stripping and
enriching sections. After extraction of values of number of theoretical stages, the overall
efficiency can be calculated using:
NTS
Eo = ∗100 (1)
NA
The height equivalent to a theoretical stage (HETS) and height of transfer unit can be used for
analyzing the columns in packed column distillation. If packing height (Z) is known, then
value of height equivalent to theoretical stage can be found using:
Z
HETS= (2)
NTS
The other approach uses differential mass balance, and it is given as:
Gdy=K OG α ( y ¿− y ) dz (3)
2 2
v v
G dy dy
Z= ∫ =G ,∫ ¿ (4)
K OG α v
1
¿
y −y v
y −y
1
Where Z is the height of the packing and G is a mass transfer parameter. The integral
maybe evaluated graphically or numerically. Graphically, by calculating the area under the
plot y vs. (y∗ −y) −1, where y is the mole fraction at this stage and y∗ is the “equilibrium”
mole fraction at this stage.
Energy balance will be applied using the following equations:
𝑄𝑟𝑒𝑏𝑜𝑖𝑙𝑒𝑟= 𝑀 [λ𝑧+𝐶𝑝 (𝑇𝑠−𝑇𝐹)] (5)
TF= TI.4
𝑇𝑠 @ (𝑃𝑠 = 𝑃𝐼.4+1.0132)
𝑀𝑠= Steam flow rate, which was obtained from the volumetric flowrate of steam
𝑄 𝑐𝑜𝑛𝑑𝑒𝑛𝑠𝑒𝑟= 𝑀𝑐𝐶𝑝 (𝑇𝑜𝑢𝑡− 𝑇𝑖) (6)
𝑇𝑜𝑢𝑡 = TI.6 (out from the condenser)
𝑇𝑖𝑛 = TI.5 (into the condenser)
𝐶𝑝 @𝑇𝑎𝑣𝑔= [𝑇𝑜𝑢𝑡−𝑇𝑖𝑛 2]
𝑀𝑐 = Cooling water flow rate, which was obtained from the volumetric flowrate of the
cooling water
Objective:
Examine bubble cap and packed bed distillation columns under total and finite reflux.
Determine and compare separation efficiencies of bubble cap and pack bed columns.
Procedure: Start-up (Atmospheric operation)
1. The concentration of feed in the re-boiler vessel was ensured that it is correct and the
liquid level was ensured that it is at the vessel equator. (25L of a solution).
a. Valve check list was completed.
b. A bubble cap column was set-up (by closing V13 and V12).
2. Column was set to total reflux condition.
a. Cooling water circuit was start-up.
b. FCV.2 was opened slowly, to prevent a pressure surge to cooling system.
c. Water pressure was not allow to exceed 2.7 bar maximum as indicated by PI.2.
3. Heating circuit was started up.
a. PCV.4 was slowly open to avoid sudden steam surge condensate to re-boiler.
b. V.11 was not closed until steady flow of steam issued from condensate drain.
c. The steam-trap drain hoes was ensured that it was at safely position.
4. The re-boiler temperature was set to approximately 90 C.
a. The return line of product distillate to the re-boiler vessel was kept open.
Sampling and readings:
1. Equilibrium was allowed to be established and the values of temperatures, flowrates.
2. A sample was collected from the distillate by opening the sample valve; then the
refractive index of the sample taken was determined.
3. The reflux control valve, RCV.1 was adjusted to obtain the desired reflux ratio, which
is the ratio of rotameter scale readings.
4. The value of temperature indicators, flow meters and reflux indicators were recorded.
5. A sample from distillate was collected, then its R.I was determined.
a. V2 was closed, and timing was started.
b. Timing was stopped when the distillate approach the top graduation.
c. V2 was opened
Set-up for the packed column:
1. Cooling water ensured that passing through a packed-column overhead condenser.
a. The reflux flow valve was set to the packed column.
b. V13 was opened and V12 was closed.
2. The steps in the sampling and reading section were repeated
Results:
Bubble Cape Column Total Reflux Calculations
Table 1: Efficiency calculation for bubble column at total reflux
Tout Mc Ts Tavg Cp Qc
(K) (K) (K) (KJ/Kg.K) (KJ/s)
(kg /s )
285.4 0.141 280 282.7 4.19296 3.192
0.8
0.6
Y
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
X
Tout Mc Ts Tavg Cp Qc
(K) (K) (K) (KJ/Kg.K) (KJ/s)
(kg /s )
286.2 0.141 280 283.1 4.1954 3.6807
1.2
0.8
0.6
Y
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
X
Tout Mc Ts Tavg Cp Qc
(K) (K) (K) (KJ/Kg.K) (KJ/s)
(kg /s )
286.8 0.141 280 283.4 4.1953 4.0366
1.2
0.8
0.6
Y
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
X
Tout Mc Ts Tavg Cp Qc
(K) (K) (K) (KJ/Kg.K) (KJ/s)
(kg /s )
287.2 0.141 280 283.6 4.1951 4.274
Table 16: Qloss calculation for packed column at Partial reflux
1.2
0.8
0.6
Y
0.4
0.2
0
0 0.2 0.4 0.6 0.8 1 1.2
X
Weeping: At some point the normal fluid rate of flow is less as compare to liquid in
purification train column
Loading: this is condition when liquid flow rate is lower than the vapor flowrate in
functional purification train in between down comer and space.
Flooding: is phenomena when liquid flow rate is too low as compare to vapor flow
rate cause not to flow liquid down side from tray/bed in column.
Comments
There should be correct keep up flow rates of liquid and vapor in given operating
parameters of operating purification train column to avoid cause of flooding and
weeping problems during time of process operation.
Process equipment may habitually upkeep and examination to improve performance
of apparatus through performing experimentations
References:
[1] J. M. Coulson, J. F. Rihardson, J. R. Backhurst, and J. H. Harker. Particle Technology
and Separation Processes, volume 2 of Chemical Engineering. Pergamon, Oxford, 4th
edition, 1991.
[2] C. J. Geankoplis. Transport Processes and Unit Operations. McGraw Hill, New York,
3rd edition, 1993.
[3] W. L.McCabe, J. C. Smith, and P. Harriott. Unit Operations of Chemical Engineering.
McGraw-Hill, 5th edition, 1993.
[4] P. C. Wankat. Equilibrium Staged Separations. Elsevier, New York, 1988.
[5] http://www.srsengineering.com/our-products/distillation-columns/how-columns-
work/#:~:text=The%20distillation%20column%20is%20made,via%20holes%20in
%20the%20plat
Appendices:
A.1 Data Sheet:
Table 17: Data Sheet Bubble Tray Column
Bubble Tray Column Total Partial
Reflux Reflux
Time (min) 5 10 15 5 10 15
TI.1 (oC) 78.0 78.0 78.0 78.0 78.0 79.0
o
TI.1A ( C) 79.6 79.6 79.6 79.8 79.8 80.0
o
TI.1B ( C) 80.1 80.1 80.1 80.1 80.1 80.0
TI.2 (oC) 80.2 80.2 80.2 80.8 81.0 81.0
o
TI.2A ( C) 80.2 80.2 80.2 81.0 81.0 81.0
o
TI.2B ( C) 79.9 79.9 79.9 80.5 80.5 80.5
o
TI.2C ( C) 80.0 80.0 80.0 85.0 84.5 84.5
o
TI.2D ( C) 79.5 79.5 79.5 84.4 84.6 84.6
o
TI.2E ( C) 81.2 81.2 81.2 87.2 87.2 87.2
o
TI.2F ( C) 81.0 81.0 81.0 87.0 86.8 87.0
TI.3 (oC) 87.0 87.0 87.0 89.0 89.0 89.0
o
TI.4 ( C) 94.0 94.0 94.0 94.0 94.0 94.0
Water PI.2 (bar) 0.9 0.9 0.9 0.9 0.9 0.9
Water FI.2 (L/min) 8.5 8.5 8.5 8.5 8.5 8.5
o
CW In TI.5 ( C) 7.0 7.0 7.0 7.0 7.0 7.0
o
CW Out TI.6 ( C) 12.4 12.4 12.4 13.2 13.2 13.2
Steam PI.4 (bar) 0.65 0.65 0.65 0.65 0.65 0.65
Reflux Ratio (RA/RB) 2.4
Refractive Index (R.I.) 1.363 1.3632
0.6 100 0 0
0.598.1 0.0079 0.0851
0.4
95.2 0.0202 0.1659
91.8 0.0417 0.3036
0.387.3 0.0891 0.4273
0.2 84 0.1436 0.4929
0.183.2 0.2069 0.5347
82 0.2813 0.5685
0
7581 80 0.369985 0.6013
90 95 100 105
80.1 0.4773 0.6438
79.1 0.6102 Temperature
0.7028
78.3 0.7788 0.8022
78.2 0.8598 x 0.864
y
78.1 0.9038 0.9015
78.2 0.9504 0.9456
78.3 1 1
A.2 Sample Calculations
From Table 3
Mass of ethanol=7.23*0.789=5.7044 g
Mass of water=92.77*1=92.77 g
As R.I = 1.363
From table 3
70 % by volume ethanol
30 % by volume water
Mass of ethanol=70*0.789=55.23 g
Mass of water=30*1=30 g
Nactual= 8
E0= 30.025%
As R.I =1.3632
From Table 3
Wt% R.I
70 1.3630
80 1.3638
(1.3630-1.3632)/(1.3638-1.3632)=(70-x)/(80-x )
Mass of water=27.5*1=27.5 g
As R.I =1.3634
From Table 3
(1.3634-1.3630)/(1.3638-1.3630)=(x-70)/(80-70)
75 % by volume ethanol
25 % by volume water
Mass of ethanol=75*0.789=59.175 g
Mass of water=25*1=25 g
NTS= 2.712
E0= (HETS/Z)*100
E0= (0.553/1.5)*100
E0 = 36.87%
As R.I =1.3636
From Table 3
(1.3636-1.3630)/(1.3638-1.3630)=(x-70)/(80-70)
Mass of ethanol=77.5*0.789=61.147 g
Mass of water=22.5*1=22.5 g
NTS = 3.13
E0= (HETS/Z)*100
E0= (0.4792/1.5)*100
E0 = 31.94%
Ms=90*0.58966*10^-6=0.00053069 kg/min
Ms=0.000008844 kg/min
Qcondensor= McCp(Tout-Tin)
Tout= 12.4
Tin= 7
Cp at Tavg (Tout+Tin)/2
Qcondensor= 3.192kJ/sec
Ms=90*0.58966*10^-6=0.00053069 kg/min
Ms=0.000008844 kg/min
Qcondensor= McCp(Tout-Tin)
Qcondensor= McCp(Tout-Tin)
Tout= 13.2
Tin= 7
Cp at Tavg (Tout+Tin)/2
= 0.1415 kg/s
Ms=90*0.58966*10^-6=0.00053069 kg/min
Ms=0.000008844 kg/min
Qcondensor= McCp(Tout-Tin)
Tout= 13.8
Tin= 7
Cp at Tavg (Tout+Tin)/2
= 0.1415 kg/s
Ms=90*0.58966*10^-6=0.00053069 kg/min
Ms=0.000008844 kg/min
Qcondensor= McCp(Tout-Tin)
Tout= 14.2
Tin= 7
Cp at Tavg (Tout+Tin)/2
= 0.1415 kg/s