Distillation

Distillation
By Farhan Ahmad [email protected]

DEPARTMENT OF CHEMICAL ENGINEERING
Distillation. Introduction
Unit operation Separation process A feed mixture of two or more components is separated into two or more products whose compositions differ from that of the feed.
Driving force Relative volatility

Principle Phase creation (ESA) Feed liquid or vap-liq mixture Product Bottom product (liquid) + Overhead product (liq or vap-liq )
2
Distillation Examples
Separation of binary mixture
Separation of Multicomponent mixture
Vapor Liquid Equilibrium

Equilibrium between vapor and liquid is determined experimentally. Temperature Composition diagram Pressure Composition diagram
T Composition diagram.
Bubble point and Dew point
Bubble point is the point at which first drop of liquid

mixture begin to vaporize.
Dew point is the point at which first drop of gaseous/vapor mixture begins to condense
Partial vaporization and condensation.
Partial Pressure and Daltons Law

The partial pressure PA of component A in a mixture of vapours is the pressure that would be exerted by component A at the same temperature, if present in the same volumetric concentration as in the mixture.
By Daltons law of partial pressures, the total pressure is equal to the summation of partial pressures.
10
Raoults Law
In an ideal gas/vapor, the partial pressure of a constituent is proportional to its mole fraction.
For an ideal mixture, the partial pressure of a constituent is related to the liquid phase concentration by Raoults law.
11
Relations from RAOULTS LAW

If a mixture follows Raoults law, then And So But Therefore
Hence
12
Vapor Pressure Relations (1)

Antoine Equation:
Riedel Equation:
Clapeyron Equation:
Where
13
Vapor Pressure Relations (2)

Reduced form of Riedel Equation:
As
Where
14
Example 11.1
The vapor pressure of nheptane and toluene at 373 K are 106 and 73.7 kN/m2, respectively. What are the mole fractions of nheptane in the vapor and in the liquid phase at 373 K, if the
total pressure is 101.3 kN/m2 ?
15
Example 11.2
The following data have been reported for acetone by AMBROSE et al.(12): Pc = 4700 kN/m2,
Tc = 508.1 K,
Po1= 100.666 kN/m2 when T1 = 329.026 K. What is Po when T = 350.874 K ?
16
Example 11.3
The constants in the Antoine equation, Equation 11.6, are: For benzene: For toluene: k1 = 6.90565 k1 = 6.95334 k2 = 1211.033 k2 = 1343.943 k3 = 220.79 k3 = 219.377
where Po is in mm Hg, T is in oC and log10 is used instead of loge. Determine the vapor phase composition of a mixture in equilibrium with a liquid mixture of 0.5 mole fraction benzene and 0.5 mole fraction of toluene at 338 K. Will the liquid vaporize at a pressure of 101.3 kN/m2?
17
Example 11.4
What is the boiling point of a equimolar mixture of benzene and toluene at 101.3 kN/m2?
18
Example 11.5
What is the dew point of a equimolar mixture of benzene and toluene at 101.3 kN/m2 ?
19
Volatility
Volatility is defined as the ratio of partial pressure of a
component to the mole fraction of that component in liquid

phase.
For ideal system, volatility of a component is numerically

equal to the vapor pressure of the pure component.
20
Relative Volatility
The ratio of these two volatilities is known as the relative
volatility.
Replacing partial pressures in terms of total pressure gives a

relation for ratio of two components in vapor to the ratio of two components in liquid.
21
Relative Volatility
For a binary mixture
This gives relations for determination of composition of liquid or vapor phases, if the composition of the other phase is known.
22
Temperature Dependency of Relative Volatility

varies somewhat with temperature, it remains remarkably steady for many systems.
increases as the temperature falls, so that it is valuable to

operate at reduced pressure in order to decrease the boiling point.
An average value of can be used over whole column if the

relative volatilities at the top and bottom of column vary by less than 15%.
Otherwise
the
equilibrium
curve
must
be
constructed
incrementally by calculating the relative volatility at several points along the column.
23
K-Value (1)
Phase-equilibrium ratio is the ratio of mole fractions of a species in two phases at equilibrium. For vaporliquid systems, the constant is referred to as the K-value or vaporliquid equilibrium ratio.
For many systems K is constant over an appreciable temperature range, So it is often much more useful than the simple vapor
pressure.
Using K-values is particularly useful while dealing with multicomponent systems.
24
K-Value (2)
Relative volatility in terms of K-value:
25
Distillation
Binary system Multicomponent system
Single-stage separation
Multistage separation
Multistage separation of Binary component Mixture

26
Methods of Distillation Binary Mixtures
Differential Distillation Flash or Equilibrium distillation Rectification
27
Differential Distillation (1)

A singlestage process that starts with a still pot, initially full, and heated at a constant rate.
The vapor formed by boiling of liquid is removed at once from the

system. Vapor is richer in more volatile component. Liquid becomes
steadily weaker in more volatile component. Product quality

varies with time. At any instant, liquid is in equilibrium with the vapor formed on that instant. At the end, the remaining liquid is removed as bottom product. A complete separation is possible only at infinite relative volatility.
28

S= number of moles of material in still x= mole fraction of component A in liquid dS= amount of material vaporized from still y= mole fraction of component A in vapor
Material balance of component A
29

Integrating
Integral can be solved graphically using equilibrium relationship between y and x.
Over the range concerned the equilibrium relationship is a

straight line of the form y = mx + c
30
or
31

If remains constant over the range of applicability, then
then
32
Flash or Equilibrium Distillation (1)

Frequently carried out as a continuous process. Feed is usually pumped through a fired heater and enters a still through a valve that causes a reduction in pressure. A part of liquid feed is vaporized in such away that vapor
evolved is in equilibrium with the residual liquid.

The still is a separator vessel that provides sufficient times for the vapor and liquid to reach equilibrium. Vapor is removed from top and usually condensed. Liquid is taken from the bottom.
33

F= molar flow rate of feed V= molar flow rate of vapor S= molar flow rate of liquid x= mole fraction of A in liquid product
y= mole fraction of A in vapor product

xf= mole fraction of A in feed Total material balance
Component A balance
34

Rearranging
Equation of straight line that passes through point (xf ,yf) and has a slope
35
36
Example 11.6
An equimolar mixture of benzene and toluene is subjected to flash distillation at 100 kN/m2 in the separator. Using the equilibrium data given in Figure 11.9, determine the
composition of the liquid and vapour leaving the separator

when the feed is 25 per cent vaporised. For this condition, the boiling point diagram in Figure 11.10 may be used to
determine the temperature of the exit liquid stream.
37
38
Rectification
The term rectification is derived from the Latin words rectefacere, meaning to improve. Distillation process that enables successive vaporization and condensation to be accomplished in one unit.
The essential merit of rectification is that it enables a vapour

to be obtained that is substantially richer in the more volatile component than is the liquid left in the still. Such a unit is known as a fractionating column.
39
Fractionating Column: Schematic
40
Fractionating Column: Major Parts
Rectifying section Stripping section Reboiler
Condenser
Reflux drum / Accumulator
41
Fractionating Column: Streams
Feed stream Overhead product Bottom product
Reflux stream
Boil-up stream Utilities
Hot Cold
42
Fractionating Column: Operation

Fractionating column is a tall cylindrical vessel that is divided into several sections by means of perforated trays. The trays allow the vapor to pass through their perforations in the upward direction. The liquid flows across each tray, then over a weir, and then through a down comer to the next tray in the downward direction. The vapor from top of the column is condensed and then passed to
a reflux drum (or accumulator or reflux divider).

A fraction of the condensed vapor is drawn as top product (distillate). The remainder is returned to the top tray as reflux.
43

The liquid from the bottom of the column is heated by means of hot oil or steam in a reboiler. The bottom product is drawn as liquid that flows over the weir in the reboiler.
Since the bottom product is hot, it may be used top reheat

the incoming feed. The vapor generated in the reboiler is returned to the bottom tray of the column.
44

At each tray, vapor is partially condensed to give a vapor that is richer in more volatile component. Liquid is partially vaporized and becomes weaker in more volatile component. This is because of vaporization of some part of more volatile component from the liquid, and condensation of some part of less volatile component from the vapor. The partial condensation of rising vapor and partial
vaporization of reflux liquid occurs at each stage.

Top vapor, distillate product and reflux liquid have same composition.
45

Feed is introduced on some intermediate tray where the liquid has approximately same composition as the feed. The part of the column above the feed tray is known as rectifying section. The lower portion below the feed tray is known as stripping section. Vapor and liquid leaving from an ideal tray are in equilibrium with each other.
Vapor and liquid entering a tray are not in equilibrium.

Assumptions of equimolar counter diffusion and constant molar overflow are often valid in the system.
46
Equimolar Counter diffusion

When the mass transfer rates of the two components are equal and opposite, the process is said to be one of equimolar counter
diffusion.
It occurs in the distillation column when the molar latent heats of the two components are the same. The more volatile component is transferred from liquid to vapor, and the less volatile components is transferred from vapor to liquid. If the molar latent heats of the two components are equal, the condensation of a given amount of less volatile component releases exactly the amount of latent heat required to volatilize the same molar quantity of the more volatile component.
47
Constant Molal Overflow (CMO)

Heat losses from a distillation column are usually small and may be neglected.
For an ideal system, heat of mixing is zero.

With these assumptions, molar heat of vaporization may be taken as constant and independent of composition. For such systems, if one mole of vapor condenses, exactly one mole of vapor is liberated. With CMO, molar flowrates of liquid and vapor remain constant in the rectifying section (and in stripping section) unless material enters (or is withdrawn from) the column.
48
Number of plates required in a distillation column
Heat and material balances over the trays, the condenser, and the reboiler Thermodynamic Phase equilibrium data
Diameter of the column

Pressure drop Degree of mixing
49
Balances across Single Plate
50
Calculations for Number of plates required
Lewis Sorel Method McCabe Thiele Method
51
Material Balance: Top and Bottom of the Column
52
Top Operating Line

In loop at top (above plate n), total material balance gives For more volatile component
By constant liquid over flow
This is the equation of top operating line.

53
Bottom Operating Line

In loop at bottom (bottom to above plate m), total material balance gives
For more volatile component
This is the equation of bottom operating line.

54
Number of Plates: LewisSorel Method

Start from the top product composition (which is equal to the composition of the top vapor).
Determine the composition of liquid leaving downward from top

stage using equilibrium curve. Determine composition of vapor leaving upward from stage 2 using
top operating line.

Continue using equilibrium curve and top operating line alternatively till you reach the feed composition. Switch to bottom operating line and continue in the same fashion as above till you reach the bottom product composition. The last step represents a partial reboiler, while all the steps above that correspond to theoretical plates in the column.
55
Example 11.7
A mixture of benzene and toluene containing 40 mole per cent benzene is to be separated to give a product containing 90 mole per cent benzene at the top, and a bottom product containing not more than 10 mole per cent benzene. The feed enters the column at its boiling point, and the vapour leaving the column which is condensed but not cooled, provides reflux and product. It is proposed to operate the unit with a reflux ratio of 3
kmol/kmol product. It is required to find the number of

theoretical plates needed and the position of entry for the feed. The equilibrium diagram at 100 kN/m2 is shown in Figure 11.14.
56
57
Number of Plates: McCabe - Thiele Method

This method uses the same assumptions as the LewisSorel method for calculation of theoretical number of plates.
The simplifying assumptions of constant molar heat of vaporisation,

no heat losses, and no heat of mixing, lead to a constant molar vapor flow and a constant molar reflux flow.
Since the top and bottom operating lines are straight lines, so they
can be plotted on the same graph as the equilibrium curve. When all three ( the equilibrium curve and the two operating lines) are on the same graph, number of plates can be determined graphically. Top operatingline is drawn using 2 points. Bottom operating line is drawn using 1 point and its slope
58

The equation of the top operating line is
If xn+1= xd, then top operating line gives
And if xn+1= 0, then
Hence top operating line passes through the points (xd,xd) and
(0,Dxd/Vn).
59

The equation of the bottom operating line is
If xn+1= xw, then bottom operating line gives
Hence bottom operating line passes through the point (xw,xw) and has aslope Lm/Vm.
60

After superimposing the two operating lines on the equilibrium curve, start from point at top (xd , xd).
Draw a horizontal line to the equilibrium curve representing composition of

vapor leaving top stage. From this point, draw a vertical line downward representing composition of liquid leaving downward from top stage. Continue these steps between top operating line and equilibrium curve till the inter section of top and bottom operating lines. Then continue these steps between bottom operating line and equilibrium
curve till the bottom composition.

Count the number of steps (either horizontal or vertical lines) . The lowest step is for a partial reboiler. Each of the steps above correspond to a theoretical plate in the column.
61
62
McCabe Thiele Method : Limitations
The assumption of constant molar overflow must be valid since in very few systems do the molar heats of vaporization differ by more than 10 per cent.
This method should not be employed when:

o Relative volatility is less than 1.3 or greater than 5 o Reflux ratio is less than 1.1 times the minimum, or
o More than twenty-five theoretical trays are required
63
Example : 11.8
Example 11.7 is now worked using McCabe - Thiele method. Thus, with a feed composition, xf = 0.4, the top composition, xd is to have a value of 0.9 and the bottom composition, xw is to
be 0.10. The reflux ratio, Ln/D = 3.
64
Enrichment in Still and Condenser

Conc. of liquor in still 16 16 15 enrichment Conc. of liquid on top plate 2 Conc. of vapors leaving from top
plate 1
Overhead product A The still and condenser together
provide enrichment (16 15) + (1

A), which is equivalent to one ideal stage.
65
The Intersection of the operating lines . (1)

The locus of the point of intersection of the top and bottom operating lines is dependent on:
o Temperature and o Physical condition of the feed

Suppose the top and bottom operating lines intersect at a point
with coordinates (xq , yq ), so this point lies on these operating

lines
Subtracting
66

A material balance over the feed plate gives:
The relation of Lm and Ln is a function of feed condition and temperature. The feed may completely or partially add to liquid, it may have no effect at all, and it can even evaporate some part of liquid
or condense some part of vapor.

If the feed is all in the form of liquid at its boiling point, the reflux Lm overflowing to the plate below will be Ln + F.
67

If however the feed is a liquid at a temperature Tf , that is less than the boiling point, some vapour rising from the plate below
will condense to provide sufficient heat to bring the feed liquor

to the boiling point. To obtain a relation between Ln and Lm , it is necessary to make an enthalpy balance over the feed plate that determine the behavior of the feed when enters the column.
68

Hf = enthalpy per mole of feed, Hfs = enthalpy of one mole of feed at its boiling point = molar latent heat of the vapor
Heat supplied to bring feed to the boiling point = F(Hfs Hf )

Moles of vapor condensed to provide this heat = F(Hfs Hf )/
69

The relation of stripping section reflux liquor and rectifying section reflux liquor is
Where
70

Material balance over the feed plate become
Overall material balance of more volatile component:
After substituting
Rearranging
This equation is known as the equation of the q-line

71
Drawing the q-line
If xq = xf , then yq = xf Thus, the point of intersection of the two operating lines lies on
the straight line of slope q/(q 1) passing through the point (xf ,
xf ) When yq = 0, xq = xf /q. The line may thus be drawn through two easily determined points
72
Slope of q-line and Feed Nature
Cold feed as liquor
q>1
q line /
Feed at boiling point

Feed partly vapor Feed saturated vapor Feed superheated vapor
q=1
0<q<1 q=0 q<0
q line
q line \ q line q line /
73
Effect of feed condition on q-line
74
Reflux Ratio
Ratio of the top overflow to the quantity of product
then
75
Top operating line in terms of Reflux Ratio

Equation of top operating line is
It can be written as
Finally
76
Influence of Reflux Ratio on No. of Plates

The slope and y intercept of top operating line are respectively
Hence the value of reflux ratio changes the slope and intercept of top operating line, and consequently affects the required number of plates If R is known, top operating line can be drawn without calculating Ln and Vn. This is done by using two point (xd ,xd) and (0, xd/(R+1)) of the topoperating line.
77
Total Reflux
If no product is drawn from the top of the column (D=0), then the column is said to be operating under total reflux. Using previously modified equation:
At total reflux, the slope of top operating line is unity and it

coincides with the diagonal x=y line. Since x=y line is the furthest from the equilibrium curve, so it provides a maximum concentration gradient, and consequently the required number of stages is a minimum.
78
Minimum Reflux
If the top operating line intersects the bottom operating line (or
the qline) at the equilibrium curve, the steps become very close
together at liquid compositions near to xf. No enrichment occurs from the feed plate to the plate above. An infinite number of plates is required to pass from xd to xf under these conditions. This condition is known as minimum reflux and denoted by Rm.
79
Reflux between Total and Minimum Reflux
Any increment in R from Rm gives a work able system, where desired separation can be achieved in a finite number of plates. This finite number of plates is greater than the minimum number of plates (that are required at total reflux). The number of plates required for R near Rm is very large.
80
Reflux less than Minimum Reflux
Reflux R less than minimum reflux ratio Rm results in an
intersection of top and bottom operating lines outside the

region bound by equilibrium curve an x=y line. This represents an impossible condition, because it is impossible to cut the equilibrium curve in this direction.
81
Effect of Reflux Ratio on No. of Plates
82
Calculation of Minimum Reflux Ratio . (1)
For a saturated liquid feed, qline is vertical.
The point of intersection of qline and equilibrium curve lies

vertically up from the feed point. Assume that its coordinates are (xf ,yf). The slope of top operating line is calculated using two point formula
83
Minimum Reflux Ratio: Saturated Liquid Feed
84
Calculation of Minimum Reflux Ratio . (2)

For a saturated vapor feed, qline is horizontal.
The point of intersection of qline and equilibrium curve lies

horizontally left from the feed point. Assume that its coordinates are (xc ,yc). The slope of top operating line is calculated using two point formula
85
Minimum Reflux Ratio: Saturated Vapor Feed
86
Underwood and Fenske Equations
Underwood Equation - Minimum Reflux ratio

Fenske Equation Number of Plates at total reflux
87
Underwood Equation : Minimum Reflux Ratio . (1)
Consider a binary mixture of A and B
If xnA and xnB are the mole fractions of two components A and B
in the liquid on any plate n then a material balance over the top portion of the column above plate n gives:
88

Under conditions of minimum reflux, infinite number of plates are required, i.e., there is no platetoplate change in composition. So
Therefore
For plate n
89

Dividing the balance of A with B
By solving the equation for Rm
As separation of the feed is required, the minimum relevant value of Rm is that for the feed plate
90

For binary system
This equation can also be obtained by using the equilibrium relation for constant in the equation for Rm developed for saturated liquid feed.
91
Fenske Method : No. of Plates at Total Reflux . (1)

Consider a system containing binary mixture of A and B Assume the relative volatility is constant for desired separation Since no product is withdrawn from still, then the operating lines become
Stage numbering in the column starts from stage1 just above the reboiler to stage N just before the condenser.
92

For the reboiler acting as a stage
If for two components A and B, the concentrations in the still are xsA and xsB, then the composition on the first plate is given by
Similarly for plate 2 from the bottom
93

For the plate n
If an average value of is used
For total condenser
94

Solving for n + 1
95
Example 11.9
For the separation of a mixture of benzene and toluene, considered in example 11.7, xd= 0.9 xw= 0.1 xf= 0.4
If the mean volatility of benzene relative to toluene is 2.4, what is the number of plates required at total reflux? Determine minimum reflux ratio.
96
Location of feed point in continuous still

When stepping off plates down the top operating line AB, the bottom operating line CE cannot be used until the value of xn on any plate is less than xe. Again it is essential to pass to the lower line CE by the time xn = xb. The best conditions are those where the minimum number of plates is used. From the geometry of the figure, the largest steps in the enriching section occur down to the point of intersection of the operating lines at x = xq . Below this value of x, the steps are larger on the lower operating line. Thus, although the column will operate for a feed composition between xe and xb, the minimum number of plates will be required if xf = xq . For a binary mixture at its boiling point, this is equivalent to making xf equal to the composition of the liquid on the feed plate
97
Location of feed point in continuous still
98
Multiple feeds and Side streams
99
Column with one Sidestream
100
Effect of Sidestream
Consider a binary system with one side stream
S = Flow rate of site stream
Xs = composition of side stream
Assuming constant molal overflow, the top operating line is
Apply balance above the feed plate and the sidestream
101
Generally the sidestream is withdrawn as liquid,
Since Ls < Ln , the middle operating line has a smaller slope than top operating line but higher y-intercept. It intersects the x=y
line at lower point than xd, xd.
Mean molar composition of distillate and sidestream

102
Middle operating line intersect the top operating line at x = xs Same graphical method to calculate the number of stages with the addition of third operating line Withdrawn of sidestream decreases the liquid flow rate below the sidestream. Hence the required number of plates increased. For each additional feed stream or sidestream, there is an additional operating line
103
104
Condition for Varying Overflow in Non-Ideal Binary Systems The Heat Balance
Non ideal systems
Molar latent heat is no longer constant
Heat of mixing
Enthalpy-composition chart Developed by RUHEMANN, PONCHON and SAVARIT
105
H x Chart
Upper curve is dew-point curve Lower curve is bubble point curve Phase mass, enthalpy and composition m = mass x = composition H = enthalpy per unit mass
A+B=C
106
H x Chart
Q = heat addition to mass mA of a phase, the increase in
enthalpy from HA to HC
107
H x Chart
The addition of two phases A and B is shown by point C on the straight line joining the two phases. The difference A B provides point C on the extension of the line AB
108
H x Chart
Considering a phase C in the two phase region, separqted into two phases A and B Tie line AB through point C
109
H x Chart
L = reflux V = vapors Compositions are on mass basis
n = rectifying section
m = stripping section Hv and HL enthalpy per unit mass for vapors and liquids Qc = condenser duty QB = boiler duty
110
H x Chart
111
H x Chart
From material balance
From enthalpy balance
112
H x Chart
Operating line for rectifying section
This operating line passes through common pole N of

coordinate xd
113
H x Chart
114
H x Chart
This operating lines passes through common pole M of
coordinate xw
115
H x Chart
116
No. of plates calculation
117
Minimum Reflux Ratio

Pole N has coordinates
118
Example 11.10
119
Solution
Applying material balance
120
Locations of pole N and M

Nm for min reflux is obtained using Tie line through F that intersect the vertical line x = 0.995 at Nm
Actual reflux
121
Location of Point N
N has ordinate N has abscissa 437 + 1547 = 1984 0.995
Point M is obtained by drawing NF at line x = 0.1
122
Solution
123
Number of Plates
No. of theoretical plates are 5+ No. of plates with efficiency 60 % = 5/0.6 = 8.33 Boiler duty:
Heat input per unit mass of bottom product
124

Distillation

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Distillation

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Distillation

By Farhan Ahmad [email protected]

Driving force Relative volatility

Separation of binary mixture

Separation of Multicomponent mixture

Vapor Liquid Equilibrium

Bubble point and Dew point

Bubble point is the point at which first drop of liquid

Partial vaporization and condensation.

Partial Pressure and Daltons Law

Relations from RAOULTS LAW

Vapor Pressure Relations (1)

Vapor Pressure Relations (2)

total pressure is 101.3 kN/m2 ?

component to the mole fraction of that component in liquid

For ideal system, volatility of a component is numerically

Replacing partial pressures in terms of total pressure gives a

Temperature Dependency of Relative Volatility

increases as the temperature falls, so that it is valuable to

An average value of can be used over whole column if the

Relative volatility in terms of K-value:

Binary system Multicomponent system

Multistage separation of Binary component Mixture

Methods of Distillation Binary Mixtures

Differential Distillation Flash or Equilibrium distillation Rectification

Differential Distillation (1)

The vapor formed by boiling of liquid is removed at once from the

steadily weaker in more volatile component. Product quality

Differential Distillation (2)

Material balance of component A

Differential Distillation (3)

Integral can be solved graphically using equilibrium relationship between y and x.

Over the range concerned the equilibrium relationship is a

Differential Distillation (4)

Differential Distillation (5)

Flash or Equilibrium Distillation (1)

evolved is in equilibrium with the residual liquid.

Flash or Equilibrium Distillation (2)

y= mole fraction of A in vapor product

Flash or Equilibrium Distillation (3)

composition of the liquid and vapour leaving the separator

determine the temperature of the exit liquid stream.

The essential merit of rectification is that it enables a vapour

Fractionating Column: Schematic

Fractionating Column: Major Parts

Rectifying section Stripping section Reboiler

Fractionating Column: Streams

Feed stream Overhead product Bottom product

Fractionating Column: Operation

a reflux drum (or accumulator or reflux divider).

Fractionating Column: Operation

Since the bottom product is hot, it may be used top reheat

Fractionating Column: Operation

vaporization of reflux liquid occurs at each stage.

Fractionating Column: Operation

Vapor and liquid entering a tray are not in equilibrium.

Equimolar Counter diffusion

Constant Molal Overflow (CMO)