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43 views15 pagesCHE 514 (PROF SAKA ABDULKAREEM) PART B 29-Jan-2025 00-15-40
The document outlines the objectives and learning outcomes for a module on extractive and azeotropic distillation, focusing on the differences between the two methods and their applications in separating multi-component mixtures. It explains key concepts such as bubble and dew points, the design of distillation columns, and methods to determine minimum reflux ratios and theoretical trays. Additionally, it provides examples and calculations related to isothermal flash calculations and the determination of compositions in distillation processes.
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0% found this document useful (0 votes)
43 views15 pagesCHE 514 (PROF SAKA ABDULKAREEM) PART B 29-Jan-2025 00-15-40
The document outlines the objectives and learning outcomes for a module on extractive and azeotropic distillation, focusing on the differences between the two methods and their applications in separating multi-component mixtures. It explains key concepts such as bubble and dew points, the design of distillation columns, and methods to determine minimum reflux ratios and theoretical trays. Additionally, it provides examples and calculations related to isothermal flash calculations and the determination of compositions in distillation processes.
Uploaded by
Looking forwardCopyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
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/ 15
DEPARTMENT OF CHEMICAL ENGINEERING
SCHOOL OF INFRASTRUCTURE, PROCESS ENGINEERING AND
TECHNOLOGY
FEDERAL UNIVERSITY OF TECHNOLOGY, MINNA, NIGERIA
CHE 514 (Separation process Ill) SESSION: 2024/2025
LECTURE ONE: Extractive and Azootropic Distillation, Distillation of multi-
component mixture
Objectives
In this module, meaning and the difference between the Azeotropic and Extractive
distillation will be discussed, followed by the discussion on how to determine the
bubble and points of a mixture. The methods to solve multicomponent and
multistage distillation problems will also be discussed in this module.
Learning Outcomes
At the end of this module, the learners should be able to
1. Differentiate between the Azeotropic and Extractive distillation
2. Determine the dew points and bubble points at a given pressures of mixtures
of vapours and liquids respectively
3. Determine the minimum reflux ratio of multicomponent mixtures
4. Use the Lewis-Matheson method to determine the number of theoretical trays
Tequired to achieve a give separation
5. Determine the feed tray location for the separation of multicomponent
mixture
Introduction
Distillation is the process of purifying a liquid by a process of heating and cooling. In
azeotropic distillation, an azeotrope is formed prior to the separation of components
from a mixture. An azeotrope is a mixture of components having a constant boiling
point. In extractive distillation process, there is no need to form an azeotrope. In that
method, a third component is added to a binary mixture. This third component can
affect the volatility of existing components.
Azeotropic jon
An Azeotrope is a binary mixture of two or more liquids that boils at a constant
temperature at a given pressure and shows the same concentration and composition
in both the liquid and vapor phase. Azeotropic distillation is a separation technique
used to separate the components of a mixture by forming an azeotrope. Azeotropes
are component mixtures with a constant boiling point. This type of mixture cannot be
separated into components by simple distillation since all the components have the
same boiling point. When an azeotropic mixture is boiled, the proportion of
components in the liquid and its vapor phase is equal.
In azeotropic distillation method, a new component (known as the entrainer) is added
to the azeotropic mixture in order to form a new azeotrope that boils at a lower
1 temperature than the existing azeotrope. Then the system has two immiscible liquid
let us consider a mixture of ethanol
phases with different boiling points. For example, es
and water. It is known as abinary azeotrope because there are two miscible
components in the mixture. If benzene is added as the entrainer to this mixture, it
mixture. The mixture is now called
can affect the volatility of other components in the 8 x i
tertiary azeotrope since there are three components in the mixture. When this
mixture is distilled, it is known as azeotropic distillation.
lation
ion is a separation technique that includes the addition of a third
component to a binary mixture to permit the separation of the two components.
However, the third component does not vaporize during the distillation process; the
third component should be less volatile. Or else, it should have a higher boiling point.
If the binary mixture has two components with relatively similar boiling points, then
these components cannot be separated by simple distillation. This happens since
both components will be vaporized at nearly similar temperatures (poor resolution).
During the extractive distillation process, an azeotrope is not formed. The process
involves a solvent with a very low volatility as the solvent of the component mixture.
It is known as the separation solvent. During the distillation, the component with
highest volatility will be vaporized easily as the top product. The remainder is the
solvent and the other component (in the binary mixture). Since the solvent does not
form an azeotrope with the second component, it can also be separated easily with
an available method.
For example, extraction of toluene from paraffin can be done in extractive distillation
method. The mixture of toluene and iso-octane has nearly similar molecular weights.
Therefore, the separation of toluene out of this mixture is very difficult. But when
phenol is added to this mixture, the boiling point of iso-octane increases. This makes
it easy to separate toluene from this mixture.
Difference between Azeotropic and Extractive in
Trey Tome ecto LOL Led eae ts :
Extractive distillation is a
separation technique
that includes the
Azeotropic distillation is a separation technique - 4
used to separate the components of a mixture by ecomoncia bes:
forming an azeotrope. CV EaHeHNG a BaNy:
mixture to permit the
separation of the two
components.
ee eM Latte tly = ‘ ‘i
In azeotropic distillation technique, the formation In extractive distillation
of an azeotrope prior to the distillation is technique, a non-volatile component is added to
the mixture that can
affect the volatility of
components in the
mixture.
important.
eral
Extract
« distillation separates a componentinto .-rarates a component
the same chemical fone arnt of
substances.
Azeotropi
the vapor phase which has t!
composition as in the liquid phase.
Design of Distillation Column ‘
TThe following must be established to design a distillation column
‘1. Temperature, pressure, composition and flow rate of the feed
2. Pressure at which the distillation must be carried out. This is frequently
determined by the temperature of the cooling medium that will be used in the
condenser.
The feed should be introduced at the optimum feed tray location
4, Heat losses are assumed to be negligible
Ifthe items 1-4 are established, only three of the following can be specified
_ Total number of trays
. Reflux ratio
Ratio of vapor to bottom product produced in the reboiler (reboil rate)
Concentration of one component (maximum two) in one product
Split of a component between the distillate and the bottoms (maximum of two)
. Ratio of distillate to bottoms
PArwoNna
Multicomponent Flash
A flash is a single stage equilibrium distillation that is carried out in a simple vessel
that allows the vapour and liquid to separate ideally. It is normally assumed that the
vapour does not entrain and liquid droplets and that the liquid does not contain any
vapour pockets. Presented in Figure 1a is a liquid that is heated under pressure and
then allowed to flash adiabatically by lowering the pressure across the valve. While
Figure 1b shown a vapour feed that is partially condensed before it enters the flash
drum
Jsothermal Flash Calculation
The following is the Rachford-Rice procedure that can be used for isothermal flash
calculation s v)= =k, ) 20
solve fly" it
Where # = VIF and Ki= Ki te 2)
verw
2
os
Zz
** Tey, -))
2K,
& =e)
L=FF
8. Q=hV +hiL-heF
x
The procedure is as follows are
Specify the temperature and pressure of the fiquid and vapour or if possible
calculate one if the other is given
2. Obtain Ki's from a source
nd 1.0. A first assumption of 0.5 is
3. Assume a value of ¥ that is between 0 at
normally acceptable. This is called Wk and f (can thus be calculated
4. The next value of Y called Y*' can be calculated using the following
equations
where /o!)= Ete
yo") aw
is as close to zero.
yay
5. This procedure is repeated until the value of 4
Example one
The following stream is flashed isothermally at 3400 kPa (abs) and 38°C. Determine
the compositions and flow rates of the vapour and liquid streams
kmol/h ki Zi
He 909 80 0.435,
CHa 909 10 0.435
Benzene 227 0.01 0.109
Toluene 45 0.004 0.021
Total 2090 1.000
=0.5
sy)=y 2k)
We _ 0.4351 1-80) | 0.435(1- 10) 4 0:1094 (1-0.1) my 0.021(1 0.004)
Ke) os@0=1) 1+0.5(10-1) 1+0.5(0.1=1) 1+0.5(0.004 -1)
= - 1.3049
0 2(-ky
re De
2
0.435(-79)? , 0.435(-9)' , _0.109(0.99)° 0.021(0.996)'
Sv")- [l+0.5(79)? 1 +0.5(9))* i [1+0.5-0.99)/? 4 [1+0.5(0.996)]?
= 3.3215
®
yi ay Sy
yi) 205- £1:3049) _ 9 go
3.3215
yf)
ww
es
is as close to zero.
K Ri) fv") jy ye
1 71.3049 3.3215 0.5 0.8929
2 0.2053 10.5981 0.8929 0.8735
3 0.0261 8.0768 0.8735 0.8703
4 0.00265 7.7612 0.8703 0.870 0.00034
The equilibrium vapour flow rate:
v
== =087
aed V sy x F = 0.87% 2090 = 1818.3kmol/h
The equilibrium liquid flow rate:
L=F-V= 2090-18183 =271.7kmol/h
The liquid and vapour composition can be calculate using:
x= Tee) and yank,
x id
He 0.00624 0.49907
CHe 0.04926 0.4926
Benzene 0.786 0.00786
Toluene 0.1875 0.00063
Total 0.999 1.00016
Bubble and Dew Points
Pure liquids boil at a certain temperature at a given pressure. When a liquid that
contains a number of components boils at a given pressure this temperature is
referred to as the bubble point. The bubble point is the temperature where the liquid
starts to boil at any given pressure.
‘The bubble point is determined by the equation: Dita. xrki = 1
The dew point of a vapour that contains more than one component is that
temperature where the first droplet of liquid will form if the vapour is called at a given
pressure
The dew point is determined by the equation: tae
Example two
Determine the bubble point at 690 kPa (abs) of a liquid with the following
composition. Assume a first guess to be 160°F (71°C)
xi Ki
n-Ca 0.7992 7.0
is 0.104 051
nC5 0.0648 0.38
ne 0.0319 0.14 Yak = 0.7992 x 1.0 + 0.1041 x 0.5 + 0.0648 x 0.28 + 0.0319 x 0.14 = 0.8814
Try T = 170°F (76.7°C) (Ki= 1.13, 0.6, 0.5 and 0.18 respectively)
Dak = 0.7992 x 1.13 + 0.1041 x 0.6 + 0.0648 x 0.5 + 0.0319 x 0.18 = 1.0037
Key components
Lower boiling compounds are called light while the higher boiling ones are called
heavy
The light key is that component that is present in the bottoms in important amount. If
there are components lighter than the light key in the bottoms, it will only be in small
quantities. If all components are present in the bottoms in significant amounts then
the lowest boiling compound is the light key
The heavy key is that component that is present in the distillate in important
amounts. If there are components heavier than the heavy key in the distillate it will
only be in small amounts. If all components are present in the distillate in significant
amounts then the highest boiling component is the heavy key.
The relative volatility is always calculated relative to the heavy key as shown in the
equation
ki
gat
1” Kine
imum Reflux Ratio
This is the simplest reflux ratio that requires an infinite number of stages to separate
the key components. It will be recalled that for a binary system, the minimum reflux
ratio Rm is found by drawing a top operating line from (Xd, Xu) to the coordinate
where q -line intersects the equilibrium curve. This constitutes a so called pinch
which implies that a separation is impossible in this pinch zone. This also holds for
the separation of key components when a multicomponent mixture is distilled.
Underwood's Method for Rm
When the relative volatilities remain constant, the following relationship can be used
to determine Rm
akg, Aakp , det,
@,-9 a,-8 a8 nt 2
A yku , Fo%w , Gore
@,-8 a-9 a&-O ”
Xan, Xap, Xde ete are the mole fraction of components AB,
distillate. A is the light key and B the heavy key
mol of the feed to the molar
Where Xia, Xte, Xte,
Cetc inthe fed and
qis the ration of the heat required to vapourise 1
latent heat of vaporization of the feed.
aa, a, ac are the volatilities with the respect to the latest volatile component.
ot of first equation which lies between aa and as
tive volatility falling between those of
for two values of
Q is the ro e
¥ the light and
Note: if one component has a relat
heavy keys, it is necessary to solve
Example three
Amixed hydrocarbon stream must be distilled in a continuous distillation column.
The feed, distillate and bottoms products are shown in the following Table.
wood’s method; the @ values to try
Determine the minimum reflux ratio (use Unde!
are 1.022; 1.0235 and 1.025
Feed, kmol/h Distillate, kmol/h Bottoms, kmol/h
CHa 500
C2Ha 1500
‘C2He, LK 1000 995
CaHs, HK 100 96
CsaHs 50
n-CaHio 20
Use Underwood's method:
4%, 5X, cX,
kn , Gp , SOK 4.
G,-9 @-9 %-9
‘A B c
3x 0.316 1.0x 0.032 0.83 x 0.016 0.37 x 0.006 =0
+ + + =
0.37-8
10-0 0.83-0
8.7x0.158 3.3x 0.473 | 2.
+ +
3.3-0 23-0
8.7-8
1.3746 ES 1.5609 7% 0.7268 ip. 0.03 Pr 0.01328 5 0.00222 _ 0
10-6 0.83-0 0.37-8
87-9 33-0 23-0 @ Is found by trial and error
But 2, (O(a,
1,0(0(2.3
if 8= 1,025,
13746, 1.5609, 0.7268, 0.03 _,_0.01328_, 0.00222 __ g og
8.7-1.025 3.3-1.025 2.3-1.025 1.0-1.025 0.83-1.025 | 0.37-1.025
If@ = 1.0235
1.3746 4 1.5609 = 0.7268 a 0.03 Ss 0.01328 os 0.00222,
8.7-1.0235 331.0235 2.3-1.0235 1.0-1.0235 0.83-1.0235 0.37-1.0235
.00036
If@ = 1.022
1.3746 15609, 0.7268 , 003, 0.01328, 0.00222 ___ gogig
871.022 3.3-1.022 2.3-1.022 " 1.0-1.022 0.83-1.022 0.37-1.022
By trial and error @ = 1.0235
BX an * AyXap
@,-0 a,-8
= Rmt
0x 0.0013 _
1.0-1.0235.
8.7x 0.167
8.7-1.0235 3.
0.189 + 0.725 + 0.6 - 0.055 = Rm+1
Rm = 0.46 olburn's meth Minimum x Rati
Number of trays
Lewis -Matheson Method
This method assumes constant liquid/vapour ratios in the rectification and stripping
section. Operating lines are obtained by striking material balances over the
rectification and stripping section, For multicomponent mixtures operating lines must
be constructed for each component.
Thus for the rectification section
in Diy 7 3
Svea t 2Xai = pte tae ”
Equation 1 gives the composition of the vapour rising to a tray in the rectification
zone in terms of the composition of the liquid leaving the tray.
The operating line for the stripping sectio
Equation 2.
n is given by relationship presented in
Yt = Xess ~ ye Xa @)
Equation 2 gives the composition of the vapour rising to a tray in the stripping zones
in terms of the composition of the liquid leaving the tray. Equiliorium relationships are
also required with equations 1 and 2 in order to carry out these calculations.
Let the mixture consist of A, B, C and D and let the mole fractions in the liquid phase
be denoted by xa, xa, xc and xo and in the vapour ya, ys, ye and yo
Then
Yatyet yoyo =1 @)
Divide through by ye
ne @)
Ya = Kaxa and ye = Kexp (8)
Thus %4 = 74% = a, at ©)
Substitute Equation 6 into Equation 4
10 xB 24 app eee
+ ca x,t DB x5 8
ms
ap 2A + O08 5g
ao
atypXat Coo%e + acaxc + Apa%0 = yg
Thus: Z(aas*A) = 5
From equations 9a and 9b
ax.
Ya = Ona 8 oy = Hoanoee)
cox anes
ote and Yo = Fagard
Yo = Sanaa)
It can be shown in a similar manner that:
Example four
The vapour from the top tray of a distil
the table below. The column operates
composition of the two top trays (Take a
”
(8)
(9a)
(9b)
(10)
(11)
lation column has the composition shown in
with a reflux ratio of 4.5. Calculate the liquid
basis of D=100 kmol/hr)
le kmol% a ‘|
n-Butane (Cs) 4 41.2
n-Pentane (Cs) 15 15.9
T-Hexane (Cs) 50 62
m-Heptanes (C7) 28 247
T-Octane (Cs) 3 4.0
Example five
A mixture consisting of 0.4 mol fraction ethylene, 0.1 ethane and 0.5 propane is feed
at its bubble point to a distillation column that is operated with a reflux ration of 2.
1 ne and 0.03
The top product contains 0.833 mol fraction ethylene, 0,137 ether
The relative
propane. Determine the number of theoretical above the ser ee rie
volatilities can be assumed to remain constant at 4.5 ethylene,
for propane.
TUTORIAL QUESTIONS
4. The top composition and relative volatility of the components of a distillation
column are as follows:
Components. Mole fraction Relative |
4 0.945 1.0
2 0.005 2.04
3 0.200 0.70
The reflux ratio is 2 and a total condenser is used. Determine the composition of the
vapour on the third plate from the top.
2. It is required that a continuous distillation column separates 2 mixture of
hexane, heptane and octane. The feed rate of the mixture to the column is
400kmol/h. To achieve this, the distillation column has to separate the feed
into a distillate and bottom product as shown in Table 1.
Table 1: Compositions of mixture in the feed and the products.
Component | Feed (kmol/h) ] Distillate BotiomsW | Relative
D (kmol/h) (kmoth) volatility
Hexane 40 40 a7
Heptane 35 34 53
Octane 25 a +a
2.4 Use Underwood's method to estimate the minimum reflux ratio (Values of 8 lie
between as and aa i.e.ag <@
