4th Opp Final Report
4th Opp Final Report
4th Opp Final Report
1
Declaration of originality
2
Acknowledgements
During practical day I received help from technicians since they explained practical
procedure and how should the practical carried, also from my group mate since we
where cooperating together in order to perform the practical
3
EXECUTIVE SUMMARY
4
TABLE OF CONTENT
Declaration of originality…………………………………..2
Acknowledgements…………………………………………3
Executive summary……………………………………..4
1.Introduction ……………………………………………….7
1.1 Back ground …………………………………………………7 .
1.2 main objective…………………………………………………7
1.3 Specific objective……………………………………………..7
1.4 Scope………………………………………………………….7
2 Literature review ……………………………………………..8
2.1 Types of distillation column ………………………………..8
2.2 type of column internals……………………………………...8
2.3 Basic operations and terminology…………………………..9
2.5 Vapor pressure and boiling…………………………………12
2.6 Relative volatility……………………………………………..12
2.7 Vapor liquid equilibria………………………………………12
3 Distillation column design…………………………………10
3.1 Mccabe-thiele method……………………………………..10
4 factors affecting distillation column and operation…..12
5 Methodology………………………………………………….14
5.1 Description of equipment…………………………………...14
5.2 consumables required………………………………………14
5.3 Addition equipment…………………………………………..14
5.4 Utilities………………………………………………………..14
5.5 Experiment procedure………………………………………14
6 Results…………………………………………………………16
6.1.1 Table observation sheet…………………………………16
6.1.2 Table of density……………………………………………16
5
6.1.3 Table of heat of vaporization……………………………..16
6.1.4 Table of heat capacity……………………………………..16
6.1.5 Table of equilibrium data……………………………………16
6.2 Calculation……………………………………………………18
6.2.1 Feed preparation…………………………………………..18
7 Discussion…………………………………………………….29
7.1 Conclusion……………………………………………………29
7.2 Recommendation…………………………………..……….29
8 References
9 Glossary ………………………………………………………30
6
Introduction
Back ground
The preparation of batch distillation practical will be prepared on the 16 march
2022at vaal university of technology laboratory. It is a continuous separation in which
a mixture is continually fed into the process (without interruption) and separated
fractions are continuously extracted as output streams. At least two output fractions
should be produced during the process. At least one volatile distillate fraction, which
has boiled and been separately captured as a vapor condensed to a liquid, and
almost always a bottom or residuum fraction, which is the least volatile residue that
has not been separately captured as a vapor condensed to a liquid, are included in
these fractions. The two main advantages of a continuous distillation process are
efficiency and quantity. When batch distillation is utilized, the batch size is
determined by the still pot size. This is not a limitation of continuous process only the
amount of upstream feed storage limits the process capacity.
1.3 Scope
The preparation of batch distillation practical will be prepared on the 4 march 2022 at
vaal university of technology laboratory, The practical while mainly focuses on
separating mixture which inside contain vapor and liquid composition , with this
process going to separate more volatile component from less volatile component
using distillation column which consist of bottom and top operating sections, The
classification or calculation number of stage won’t be covered during the practical.
During practical day I received help from technicians since they explained practical
procedure and how should the practical carried , also from my group mate since we
where coopering together in order to perform the practical.
7
LITERATURE REVIEW
Distillation is a separation process components in a mixture by making use of the
fact that some components vaporize more than others, when vapours are produced
from a mixture, they contain the components of the original mixture, but in
proportions which are determined by the relative volatility of these components. The
vapour is richer in some components, those that are more volatile and so a
separation occurs
2.1 Types of distillation column
Batch and continuous distillation
-Batch column
In batch operation, the feed to the column is introduced batch-wise. That is, the
column is charged with a 'batch' and then the distillation process is carried out. When
the desired task is achieved, a next batch of feed is introduced.
Continuous Columns
In contrast, continuous columns process a continuous feed stream. No interruptions
occur unless there is a problem with the column or surrounding process units. They
are capable of handling high throughputs and are the most common of the two
types. We shall concentrate only on this class of columns.
Continuous distillation
Can be further classified according to the
The nature of the feed that they are processing
Binary column Feed- mixture only contains two component
Multi component feed -contains more than two components
The number of product streams they have
Multi product column – column has more than two product streams.
Where the extra feed exits when it is used to with separation
Extractive distillation- where the extra feed appears in the bottom product stream.
Zeotropic distillation- where the extra feed appears at the top product stream.
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Packed column-'Packings' are utilized instead of trays to improve contact between
the vapours and the liquid.
Main components of distillation columns
A vertical shell- where the separation of liquid components carried out
Column internals- such as trays / plates and packing which are used to enhance
components separations
A reboiler- to provide the necessary vaporisation for the distillation process
A condenser- to cool and condense the vapour leaving the top of the column
Reflux –to hold the condensed vapour from the top of the column so that liquid
(reflux) can be recycled back to the column
Below diagram represents the schematic of a type of distillation unit with a single
feed and two product streams, together with the condenser and reboiler constitute a
distillation column.
9
The heating source in refineries could be the output streams of other columns. At the
bottom of the column, the vapour generated in the reboiler is reintroduced into the
unit. The bottoms product, or simply bottoms, is the liquid that is taken from the
reboiler.
The vapour rises the column and is cooled by a condenser as it reaches the top of
the unit. The condensed liquid is collected in a reflux drum, which serves as a
holding vessel. The reflux is the process of returning some of this liquid to the top of
the column. The distillate, or top product, is the condensed liquid that is taken from
the system.
As a result, there are internal vapour and liquid fluxes within the column, as well as
external feeds and product streams flowing into and out of it.
Trays and plates
The terms "trays" and "plates" are interchangeable in this context. Trays come in a
variety of shapes and sizes, but the most popular are:
Bubble cap trays
A riser or chimney is put over each hole in a bubble cap tray, and a cap covers the
riser. Cap with bubbles the cap is installed with enough space between the riser and
the cap to allow vapour to pass through. The vapour rises via the chimney and is
guided downward by the cap, eventually discharging through the cap's slots and
bubbling into the liquid on the tray.
Valve trays
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Perforations in valve trays are covered by liftable caps. Vapour flows elevate the
caps, forming a flow space for vapour to pass through. The lifting cap allows the
vapour to flow horizontally into the liquid, allowing for better mixing than sieve trays.
Sieve trays
Sieve trays are nothing more than metal plates with holes drilled into them. Through
the liquid on the plate, vapour rises straight up. Design factors include the hole
arrangement, quantity, aand size.
Sieve and valve trays have largely replaced bubble cap trays in many applications
due to their efficiency, wide operating range, ease of maintenance, and low cost.
Diagram below shows the path way of vapour and liquid flow across a tray and
across a column
Each tray includes two 'downcomers,' one on each side. Gravity causes liquid to fall
through the downcomers from one tray to the next. gif of activtra (2090 bytes) The
flow through each plate is depicted in the right-hand diagram.
A weir on the tray guarantees that there is always some liquid (holdup) on the tray
and is designed such that the holdup is at a desirable height, such as covering the
bubble caps.
Vapour flows up the column and is forced to pass through the liquid via the
perforations on each tray because it is lighter. The active tray area refers to the area
on each tray that allows vapour to travel through.
2.4 Destillation principle
The differences in boiling points of the distinct components are used to separate
components from a liquid combination by distillation. Additionally, the boiling point
properties of the liquid mixture will vary based on the amounts of the components
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present. As a result, the vapour pressure properties of liquid mixes affect distillation
processes.
α A.B = ( )( )
Y A YB
/
XA XB
When the relative volatility of two components is very close to one, it indicates that
their vapour pressure properties are highly comparable. This means that their boiling
temperatures are quite similar, making distillation a challenging process to separate
the two components.
2.7 Vapour liquid equilibria
Binary mixing VLE data is frequently presented as a plot, as illustrated in the figure
below. At intense pressure, the VLE plot expresses the bubble-point and dew-point
of a compound. The equilibrium line is a curving line that depicts the compositions of
gas and liquid in equilibrium at a given pressure.
12
This particular VLE plot depicts a binary combination with a reasonably easy to
separate uniform vapour-liquid equilibrium. On the other hand, the next two VLE
plots below indicate non-ideal systems that will be more challenging to separate. The
shapes of the curves can tell us something, and this will be described later.
Azeotropic methods yield the most fascinating VLE curves. An azeotrope is a liquid
mixture that yields the same composition when vaporized. Two alternative azeotropic
systems are shown in the VLE plots below, one with a minimum boiling point and the
other with a maximum boiling point. The equilibrium curves intersect the diagonal
lines in both graphs, indicating azeotropic sites where azeotropes exist. To put it
another way, azeotropic systems produce VLE plots with equilibrium curves that
cross diagonals.
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3 Destillation column design
VLE data is used to build distillation columns for the mixes to be separated. The
number of stages, and hence the number of trays, necessary for the separation will
be determined by the mixture's vapour-liquid equilibrium characteristics (as
represented by the form of the equilibrium curve). Using the McCabe-Thiele
approach to construct a binary column exemplifies this point.
3.1 Mccabe-thiele method
The McCabe-Thiele method is graphical, and it use the VLE plot to compute the
theoretical number of stages required to effect binary mixture separation. It is based
on the assumption of constant molar overflow, which means that:
Heat effects (heats of solution, heat losses to and from column, etc.) are insignificant
because the molar heats of vaporisation of the components are essentially the same.
1 mole of liquid is vaporized for every mole of vapour condensed.
The design technique is straightforward. Operating lines are drawn initially, using the
VLE diagram of the binary mixture as a guide.
The mass balance relationships between the liquid and vapour phases in the column
are defined by operating lines.
The bottom (stripping) section of the column has one operational line, while the top
(rectification or enrichment) section has two.
The constant molar overflow assumption also ensures that the operational lines are
in good shape.
Rectifying section operating line
The rectification section's operating line is as follows. On the VLE diagram, the
required top product composition is first found, and a vertical line is dr awn until it
14
intersects the diagonal line that divides the VLE plot in half. From this instersection
point, a line with the slope R/(R+1) is drawn, as shown in the image below.
R is the reflux ratio, which is defined as the ratio of reflux flow (L) to distillate flow
(D). It is a measure of how much of the material traveling to the top of the column is
returned to the column as reflux.
TOP OPERATING LINE
Y n=
( ) (
Ln
Vn
X+
D
X
Vn D )
BOTTOM OPERATING LINE(stripping section)
Constructed from the following diagram below
Where Ln isa liquid that goes down∧v n vapour that goes up
Y n= ( ) (
Lw
Vw
X+
B
X
Vw B )
REFLUX RETIO
L
R=
D
FEED operating line
15
q xf
Y n= x−
1−q q−1
16
5 Methadology
5.1 Description of equipment
-A mash packing column, bottom boiler with electrical heater, condenser, and feed
pump make up the continuous distillation plant.
-After an electrical heater has preheated the binary mixture in the tank, it is fed via a
column feed pump.
-The solution is heated with the bottom resistor once the boiler has been full.
- Once the solution reaches boiling point and the column is stable, the distillate can
be taken and fed while keeping the reflux ratio constant.
5.2 Consumables required
- Methanol
- Distilled water
5.3 Additional equipment
- One liter measuring cylinder
- Weighing balance
- Glass beakers
5.4 Utilities
- Power supply: three phases, P=3.5
- Tap water for cooling
- Compressed air
5.5 Experiment procedure
A 15 L Methanol/ water mixture is to be synthesized and the mixture is to contain
methanol at a concentration of 30% (w/w).
Start up
all switches was to 0 and the emergency pushbutton was checked wether is not
pressed .the plant was connected to the electrical mains , valves V2, V3, V4, V5, V7,
V8, V9, V10, V11, V12, V14, V21, V23 was shut off and V26 and valves V1, V15,
V16, V17, V18, V19, V22 and V27 was opened ,Valve V6 was permanently opened
to avoid overpressure in the feeding line . valve V25 was partially opened and the
boiler was filled with the mixture to be distilled until the electrical resistor J2 is
completely plunged also tank D1 was filled with the mixture to be distilled .the switch
was turned from AUT TO AUDO the E.L.C.B switch was connected and the start
button 5 was pushed and the switch of resistor J2 was set to 1. the electrical resistor
was powered using the output 4-20 mA of the 2nd loop of the controller no.2,
proportional to 0-2500 W (select the 2nd loop with pushbutton Loop and then the
indication Out with pushbutton, finally increase its value with pushbutton to 100%).
the plant was connected to the tap water using the rubber hose and the solution
was waited to boil and the mixture was taken to the boiling point and then the
17
heating power was decreased to 60% ( the 2nd loop was selected its value with
pushbutton Loop and then the indication Out with pushbutton, finally its value was
with decrease with pushbutton to 60%). and the tap water was opened . the column
was let to total reflux for about 5 minutes (until the temperature TI6 was stable) and
the switch of the pump G1 was turned to position 1. ,Feed, e.g. 5L/h (about 40%),
using the output of the 4th loop of controller no. 1 (select the 4th G1) loop with
pushbutton Loop and then the indication Out with pushbutton , finally its value was
increase or decrease with pushbutton to e.g. 40%) and Wait until the container of
the preheating resistor J1 was filled and S the 1st loop was selected (TIC1) of
controller no.1 , loop with pushbutton Loop was selected and then the indication Out
with pushbutton, finally its value was increase or decrease i with pushbutton to e.g.
50% and heater J1 was switched on . valve V4 was opened and The preheating
temperature was less than the boiling point of the mixture .To select the reflux ratio,
turn the switch was turned to position 1 . the Start and Stop times was
selected(sec) on the timers, to give the desired reflux ratio , valve V13 was partially
opened and Run the column was runned for 20 minutes while the flow rate of
cooling water was measured.
Shut down
The “Reflux” switch was set to 0 and the switch of resistor was set J1 to 0 ,the
switch of pump G1 was to 0 and Close valve V1 was closed Set the switch of the
heating resistor J2 to 0 .Close valve V13 was closed. tank D2 , D3 and D4 was
drained and the tap water was closed the E.L.C.B was disconnected and the plant
was switched from the power supply.
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RESULTS
6 Findings
Calculations
19
1/compositionmeth composition H O
AV density= + 2
ρmeth ρH O 2
1/1−compositionH O compositionH O
801.11= 2
+ 2
777.98 991.09
Bottoms
Consider water
mole of Water
¿ 327 K ρWater =
V olume of Water
C1
ρwater =
C 2¿ ¿ ¿
5.459
ρwater =
0.30542¿¿ ¿
=988 kg /m 3
C1
ρmethanol = ¿¿
C2 ¿
2.288
¿ ¿¿
0.2685 ¿
3
ρ methanol =757 kg/ m
1
ρavarage = ;
compositionmeth composition H O
+ 2
ρ meth ρH O 2
1
944.341=
1−composition H O composition H O
2
+ 2
757 988
20
m ole total ( 72.1+65.9+56.6+55.3 ) ×10−3
ρ avarage = =
V olume total ( 90+83+71+70 ) ×10−3
¿ 795.67 kg /m3
T 1 +T 2+T 3 +T 4 +T 5+T 6
AVARAGE TEMPERATURE=
4
309.8+ 305.5+304+302.5
¿ =305.5 K
4
C1
ρmeth = ¿¿
C2 ¿
2.288
¿
0.2685¿¿ ¿
5.459
ρ water = ¿¿
0.30542 ¿
¿ 992.23 kg /m3
1
ρ avg = ;
composition meth compositionH 2O
+
ρmeth ρH O 2
1
795.86=
1−composition H O composition H O
2
+ 2
781.38 992.23
¿ 953 kg /m3
T 1 +T 2+T 3 +T 4 +T 5+T 6
AVARAGE TEMPERATURE=
4
21
327.4+317.5+316.7+316.7
¿
4
¿ 319.58 K
C1
ρmeth = ¿¿
C2 ¿
2.288
¿ ¿¿
0.2685 ¿
3
¿ 770 , 048 kg/m
5.459
DENSITY OF WATER= ¿¿
0.30542 ¿
3
¿ 988 kg /m
1 /1−composition H O composition H O
953.08= + 2 2
770.048 988
Mass balance
m ass (kg)total
D=
t ime (hr )
249.9× 10−3
¿
0.333
¿ 0.75 13 kg /hr
Overall balance
F=B+ D
22
O.5928
F=
0.18
¿ 3.29 01 kg/hr
B=F−D
B=3.29−0.75
B=2.54 13 kg/ hr
( R+1 ) x +( R+ 1 )
R xd
y n= n
2 0.91
¿ x n+
2+ 1 2+ 1
¿ 0.669 x n+ 0.30 2
Ln=R D
¿ 2 ×0.75=1.5 01kg / hr
¿ 2.261 kg/hr
Ln D
y n= x n +1+ x =0.669 x n+1 +0.30 2
Vn Vn d
λ water=5.2053 × 1007 ¿
¿ 37752478 J /kmol
¿ 43388799 J /kmol
23
C p=C 1+ ( C2 ×T ) + ( C 3 × T 2 ) +(C 4 × T 3 )+(C 5 ×T 4 )
CAPACITY OF WATER=2.7637 ×10 + (−2.0901 ×10 ×318.2 ) + ( 8.1250× 10 ×318.2 ) + (−1.4116 ×10 × 31
5 3 0 2 −2
Capacity of water
7 23 4 J oules
¿
kmol . K
84402 J
methanol capacity=
kmol . K
F F
mixture capacity=C water composition w +C methanol composition metnanol
68435.85 J oules
¿
kmol . K
≈1
( )
q xf
yq= x q−
q−1 q−1
1.07 0.3
¿ x −
1.07−1 q 1.07−1
¿ 15.29 0 xq −4 .2913
y m=¿
LM 2.54 12 ×0.12 11
¿ x m−
Vm 2.48
24
McCabe-Thiele graph
More volotile component fraction
From the graph we obtained 5 theoretical stages and feed is fed on plate number 4
J
¿ 5289
kg . K
J oules
¿ 278 2
kg . K
J oules
¿ 1973 .
kg . K
¿ 8743 . W
25
Energy condenser =ṁC P ( T 8−T 7 )
T 7=290.4 K ∧T 8 =291.8 K
T 7 +T 8
T =T avarage = =291 k
2
water capacity =2.7637 ×105 + (−2.0901 ×103 ×291.1 ) + ( 8.1250× 100 ×291.12 ) + (−1.4116 ×10−2 × 291.13 )+ ¿
5197 J
¿
kg . K
mass water
mass flow=ṁ=
t ime
0.814
¿ =0.07 12 kg /s
11.61
¿ 411. 439 W
B
AVARAGE CAPACITY =C pmethanol compositionmeth +C capacity of water x Bw
4185.89+2552.59
¿
2
J oules
¿ 44 69
kg . K
¿ 921 . 4 W
26
7.1 Discussion
Runs 3, 4, and 5 achieved the greatest ethanol purity composition with a mole
fraction of 0.802. The third iteration calculated 5 theoretical trays, resulting in a tray
efficiency of 50%, which is a higher tray efficiency with the same purity. Due to the
azeotrope, which requires an endless number of stages to reach a 0.9 mole fraction
of ethanol, there is currently no way to achieve such purity. Runs three and four
utilized five theoretical trays, while runs three and four used four, implying that runs
four and five were superior at separation at a lower capital cost.
7.2 Conclusion
This experiment was performed to determine the energy balance, mass balance,
mole fraction, bottom composition and distillate composition the principle of mccabe-
thiele was used to determine the rectifying section, stripping section and feed line
equation in order to determine the number of stages and locate the feed stage point.
The experiment was successful since we had technicians in service of need also the
equipment or materials to carry the practical where available. The experiment helped
to separate the less volatile component from more volatile component, where’s the
less volatile component leaves at bottom and more volatile component leaves at
bottom.
7.2 RECOMMENDATIONS
27
recommendations is that someone should try to concentrate on altering the feed and
reflux inlets into the distillation column. Our investigation was hampered by the fact t
hwe were unable to finish enough runs to observe this behavior. In the future, the dis
tillation experiment should be run at different steam pressures than our values, and t
he distillation column and reboiler should perhaps be insulated.
28
References
Fair, James R.’’ Design Aspects for Reactive Distillation.’’ Chemical Engineering
October 1998:158-166
Shelley, Suzanne.’’ Winds of change out of thin air chemical Engineering June
1991:36-42
Perry, Robert H. and Don W, Green. Perry’s Engineers Handbook 7 th edit.new York
McGraw-hill, 1997:13-1-13-108
Eckles, Andrew J.’’ Difficult to process it’’ chemical Engineering septermber 1997:94-
100
29
GLOSSARY
Reflux- Is the ratio between the amount of reflux that goes back diwn the distillation
column and the amount of reflux that is collected in the receiver.
Condenser-Is a equipment that lower the temperature of the refrigrerant so it can be
converted into liquid form.
Reboiler- Equipment used to provide heat to the bottom of industrial distillation
columns.
Destillation column- Is an item used in the distillation of liquid mixture to separate
mixture into its components parts.
More volatile component- component with highest vapour.
Less volatile component-component with lowest vapour.
Volatility-
Stripping section- Section in which less volatile component in the mixture under
separation on it.
Rectifying section- Section where more volatile component is removed through
contacting rising vapour with the down flowing liquid.
Vapour- is a diffused matter such as smoke or fog.
Distillation plates- Is a stage in which two phases such as liquid and vapour phases
of a substance, establish an equilibrium with each other.
30