Distillation Techniques in Chemical Engineering
Distillation Techniques in Chemical Engineering
College of Engineering
Lesson Outcome
Mass Transfer Unit Operation The objective of this chapter is to describe most of distillation in some
November 2023
At the end of this topic the students are:
Instructor: Ibsa Neme 1. Able to define distillation, working principles of distillation, classify
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Simple distillation is practiced for a Steam distillation is used for the purification
mixture in which the boiling point of the of mixtures, in which the components are
temperature/heat sensitive; for example, organic
components differ by at least 70°C.
compounds.
It is also followed for the mixtures In the instrument setup, steam is introduced
contaminated with nonvolatile particles by heating water, which allows the compounds
(solid or oil) and those that are nearly to boil at a lower temperature.
pure with less than 10 percent This way, the temperature sensitive
compounds are separated before
contamination.
decomposition.
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Then vapour is partially condensed to earn 4) Azeotropic distillation: where the extra feed appears at the top product stream.
5) Tray distillation column: where trays of various designs are used to hold up the
back the less volatile compounds to the
liquid to provide better contact between vapor and liquid, hence better separation.
column to separate as bottom product.
6) Packed distillation column: where instead of trays, pickings are used to enhance
(reflux)
contact between vapor and liquid.
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CHAPTER TWO Distillation CHAPTER TWO Distillation
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where, yA = mole fraction of component ‘A’ in the vapor, xA = mole fraction provided the average relative volatility (ɑavg).
of component ‘A’ in the liquid, yB = mole fraction of component ‘B‛ in the
vapor and xB = mole fraction component ‘B’ in the liquid
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CHAPTER TWO Distillation CHAPTER TWO Distillation
PA Experimental VLE data for most multicomponent mixtures are not available and have to be
xA
AB (2.5) computed by using the variable equations.
PB
xB The calculation becomes pretty simple if we have an ideal multicomponent system so that Raoult's
law is applicable.
where PA is the partial pressure of component A in the vapor, PB is the
partial pressure of component B in the vapor and P is the total pressure of Hydrocarbons of a relative series form nearly ideal solutions.
the system. For the ith component in an ideal solution, we can write as follows.
n
Note: if the relative volatility between two components is equal to one, y j P p j x j Pj v and P p i (2.6)
i 1
v
pj x j Pj
separation is not possible by distillation. y j n
(2.7)
p
P
i
i 1
The larger the value of ɑ, above 1.0, is the easier the separation. where, Pj* is vapour pressure of component j at the given temperature, xj is liquid composition and
yj* is vapour composition
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xj xj ij xi
y j n
n
n
(2.8)
1
Pj v
xP
i 1
i j
v
i 1
ij xi
k 1
ki xk
Once the equilibrium vapour phase mole fractions are known, the partial pressures and the total pressure can
be calculated from equation 2.6
For hydrocarbon mixtures, a quantity called equilibrium vaporization ration (denoted by Ki for the ith
component) is a extensively used for VLE computation. It is defined as:
yi Pi v
Ki (2.9)
xi P
Distillation calculations, including the bubble and dew point calculations, can be done using the K-
values, if available.
The DePriester chart may be conveniently used to obtain K-values for lower hydrocarbon at
different temperatures and pressures. Figure of DePriester chart- at high temperature range
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CHAPTER TWO Distillation CHAPTER TWO Distillation
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Figure: VLE curves for azeotropic systems: (a) for maximum boiling point,
(b) for minimum boiling point
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Batch distillation columns and their process calculations Example 1: Calculation on Batch Distillation
In batch operation, the feed is introduced batch-wise to the column. A mixture of 40 mole % isopropanol in water is to be batch-distilled at 1 atm
The concentration changes can be analyzed using the phase diagram, and until 70 mole % of the charge has been vaporized. Calculate the composition
detailed mathematical calculations carried out using the Rayleigh of the liquid residue remaining in the still pot, and the average composition
Equation. of the collected distillate. VLE data for this system, in mole fraction of
As the process is unsteady state, the derivation is based on a differential isopropanol, at 1 atm are given in Table below:
approach to changes in concentration with time.
Based on the material balance calculation Rayleigh Equation for batch is:
L x1 dx
ln 1 (2.10)
L2 x2 y x
Continuous distillation columns and their process calculations Single Stage Continuous distillation and its process calculations
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This method uses the equilibrium curve diagram to determine the number Feed condition (temperature, composition),
of theoretical stages (trays) required to achieve a desired degree of Distillate and bottom compositions; and
It assumes constant molar overflow and this implies that: liquid over the distillate product.
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It is defined as the quantity of liquid returned to the distillation column b) Determination the feed condition (q).
over the quantity of liquid withdrawn as product from the column, i.e. c) Determination of the feed section operating line (q-line).
The reflux ratio (R) is important because the concentration of the more e) Determination of the stripping section operating line (SOL).
volatile component in the distillate (in mole fraction xD) can be changed f) Determination of number of theoretical stage.
Determination of the Rectifying section operating line (ROL). Determination of the Rectifying section operating line (ROL).
Consider the rectifying section as shown in the Figure below and from As shown in Figure below. If xn = xD, then◦yn+1 = xD, the operating line
passed through the point (xD, xD) on the 45 diagonal line.
the material balances, the rectifying section operating line (ROL) When the reflux ratio R changed, the ROL will change.
equation also derived below.
L D R 1
yn1 xn xD xn xD (2.12)
LD LD R 1 R 1
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Determination the feed condition (q). Determination the feed condition (q).
The feed enters the distillation column may consists of liquid, vapor or a Table of limitations of q-value as per feed conditions
Calculation of q-value when feed is partially vaporized Calculation of q-value when feed is cold liquid or superheated vapor
In case of partially vaporized mixture, the q-value can be obtained from q can be alternatively defined as the heat required to convert 1 mole of
enthalpy balance around the feed plate. feed from its entering condition to a saturated vapor; divided by the
By enthalpy balance one can obtain the q-value from the following form molar latent heat of vaporization.
HV H F
q (2.13)
HV H L
where HF, HV and HL are enthalpies of feed, vapor and liquid respectively which can
be obtained from enthalpy-concentration diagram for the mixture.
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Calculation of q-value when feed is cold liquid or superheated vapor Determination of the feed section operating line (q-line)
Based on this definition, one can calculate the q-value from the following Consider the section of the distillation column (as shown on Figure ‚a‛
Equations for the case whereby q > 1 (cold liquid feed) and q < 0 below) at the tray (called feed tray) where the feed is introduced.
(superheated vapor feed) as: In the feed tray the feed is introduced at F moles/hr with liquid of q
fraction of feed and vapor of (1-f) fraction of feed as shown on Figure ‚b‛
For cold liquid feed For superheated vapor feed: below.
C p , L (Tbp TF ) C p ,V (Tdp TF )
q (2.14) q (2.15)
where Tbp is the bubble point, is the latent heat of vaporization and Tdp is the
a) b)
dew point of the feed respectively.
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CHAPTER TWO McCabe-Thiele Method CHAPTER TWO McCabe-Thiele Method
Determination of the feed section operating line (q-line) Determination of the feed section operating line (q-line)
From overall material balance around the feed tray and Different values of q will result in different slope of the q-line.
Component balances for the more volatile component in the rectifying Different q-lines for different feed conditions are shown in Figure below.
and stripping sections.
The feed section operating line Equation is given as follows:
q 1
y x xF (2.16)
1 q 1 q
For a given feed condition, xF and q are fixed, therefore the q-line is a
straight line with slope -q / (1-q) and intercept xF/(1-q).
At y = xF condition the q-line passes through the point (xF, xF) on the 45◦
diagonal. Figure: Different q-lines for different feed condition
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Determination of the stripping section operating line (SOL) Determination of number of theoretical stage
The stripping section operating line can be derived from the material
balance around the stripping section of the distillation column. Once the three lines (ROL, SOL and q-line) are drawn;
The stripping section of a distillation column is shown in Figure below.
The re-boiled vapor is in equilibrium with bottoms liquid which is The number of theoretical stages required for a given separation is then
leaving the column.
the number of triangles that can be drawn between these operating lines
L' B
y ' x ' xB (2.17)
L B L B and the equilibrium curve.
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The Drickamer-Bradford empirical correlation: theoretical number of stages with the actual trays in a distillation
column or absorber.
Eo 13.3 66.8log ( ) (2.19)
This efficiency can be based upon the liquid or the vapor composition on
The correlation is valid for hydrocarbon mixtures in the range of 342 K < T < a particular stage at its conditions of temperature and pressure.
488.5 K, 1 atm < P < 25 atm and 0.066 < µ < 0.355 cP For a given component, it can be expressed as:
yn yn 1 xn xn 1
Eo 50.3( ) 0.226 (2.20) EMV (2.21) EML (2.22)
yn yn 1 xn xn 1
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xF xB xD xF The right hand side of the Equation (2.23) represents the slope of the
(2.23)
Q QC straight line passing through the points (xF, HF) and (xD, HD-QC/D).
HF HB R HD HF
R D
The amount of distillate as per Equation (2.23) is proportional to the which it operates is described in the enthalpy-composition diagram as
horizontal distance and the amount of bottoms is proportional to shown in Figure (b).
the horizontal distance , then from the overall material balance it (a) (b)
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Stepwise procedure to determine the number of theoretical Stepwise procedure to determine the number of theoretical
trays For Ponchon-Savarit Method trays For Ponchon-Savarit Method
Step 5: Step off the trays graphically for the rectifying section. Then the point of
composition x1 of liquid of top tray is to be determined from the equilibrium
relation with y1 of vapor which is leaving the tray and locate it to the HL-x curve.
Then the composition y2 is to be located at the point where the line of points ΔR
and x1 intersects HV-y curve. This procedure is to be continued until the feed plate is
reached.
Step 6: Similarly follow the same rule for stripping section. In the stripping section,
the vapor composition yB leaving the re-boiler is to be estimated from the
equilibrium relation. Then join the yB and ΔS to find the xN. The vapor composition
yN is to be determined by extending a tie line to saturated vapor curve HV-y. The Fig. Representation of estimation of no of stages by Ponchon-Savarit Method
procedure is to be continued until the feed tray is attained. 77 78
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Determination of the reflux rate Under Ponchon-Savarit Determination of the reflux rate Under Ponchon-Savarit
Method Method
The reflux rate can be calculated from the energy balance around the The internal reflux ratio between any two stages in rectifying section can
condenser as: be expressed as:
V1 HV ,1 LD H D DH D QC (*)
Q
Ln ( H D C ) HV ,1 R HV , n 1
By substituting V1 = LD + D into Equation (*) and rearranging, it can be D (2.25)
Vn 1 ( H QC ) H R H L ,n
written as: D D L ,n
QC
LD ( H D D
) HV ,1 H Whereas in the stripping section it can be expressed as:
R V ,1 (**)
D HV ,1 H D HV ,1 H D
Q
Lm 1 ( HV ,m ( H B R )
B (2.26)
Where and are the lengths of lines between points ΔR and HV,1 and HV,1 and Vm QR
( H L , m 1 ( H B )
B
HD.
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CHAPTER TWO Ponchon-Savarit Method CHAPTER TWO Ponchon-Savarit Method
Overall Material Balance Under Ponchon-Savarit Method Minimum number of trays in Ponchon-Savarit Method
The relationship between the distillate and bottom products in terms of In this method, if D approaches zero, the enthalpy coordinate (HD +QC/D) of the
compositions and enthalpies can be made from the material balance difference point approaches infinity.
around the overall column which can be written as: Other way it can be said that Qc becomes large if L becomes very large with
respect to D.
FH F QR DH D BH B QC (2.27) Similarly enthalpy coordinate for stripping section becomes negative infinity as
Overall material balance F = D + B combining with Equation (2.27) yields B approaches zero or liquid loading in the column becomes very large with
respect to B.
QR
D H F (H B B xF S
) Then the difference points will locate at infinity. In such conditions, the trays
(2.28)
B ( H QC ) H xF R required for the desired separation is referred as minimum number of trays.
D D F
The thermal state of the feed has no effect on the minimum number of trays
required for desired separation.
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The minimum reflux for the process normally occurs at the feed tray. END OF THE CHAPTER
The minimum reflux rate for a specified separation can be obtained by
THANK YOU!
extending the tie line through the feed composition to intersect a vertical
line drawn through xD.
Extend the line to intersect the xB composition line determines the boil up
rate and the re-boiler heat duty at minimum reflux.