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KIL 2008

Separation Processes 1

3 – Continuous Distillation with Reflux & McCabe-Thiele Method

Hanee Farzana Binti Hizaddin


Department of Chemical Engineering
University of Malaya

hanee@um.edu.my

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Learning outcomes
At the end of this class, you should be able to:
• Explain the purpose of reflux in a distillation process
• Explain the purpose of multiple stage equilibrium separation
• Derive the general operating line equation for multiple stage equilibrium
separation
• Familiarize with McCabe-Thiele method and derivation of related operating
line equations
• Apply the McCabe-Thiele method to determine the theoretical number of
stages
• Estimate the condenser and reboiler duty

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Introduction to Distillation with Reflux
• Comparable to a series of flash-vaporization stages arranged in a
series such that the vapor and liquid products from each stage flow
countercurrent to each other.
• https://youtu.be/M7AL7-44YTc

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Distillation with Reflux (Binary Mixtures)
• Same principle is applied as in simple distillation, but this time involves multiple sequential stages of
vaporization and condensation
• Feed enters somewhere in the middle of the column. The feed can be in
liquid, vapor or a mixture of liquid-vapor phase

• The column is divided into a series of stages (cascades of equilibrium


stages)

Rectification • Liquid flows down the column from stage to stage and contacted by the
section – vapor is vapor flowing upward
enriched by contact
with the reflux • In each stage, vapor and liquid enter, mix and reach equilibrium, and the
liquid vapor and liquid leaving the stage are at equilibrium

• The concentration of the more volatile component (lower boiling


component) is being increased in the vapor from each stage going
upward and decreased in the liquid going downward
Stripping section –
liquid portion of • The final vapor product is condensed and a portion of the liquid is
the feed serve as removed whereas the remaining is returned to the column as reflux
reflux in this and enters the top tray of the column
section
• The liquid leaving the bottom trays enter a reboiler where it is partially
vaporized. The vapor from the reboiler enters the bottom tray and the
remaining liquid is withdrawn as a bottom product
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Derivation of the Operating Line equation
L0 V1 Let the total number of stages = N

1 For a total number of stages N, the overall inlet and outlet are:
Liquid inlet = L0 ; Vapor inlet = VN+1 Rearrange Eq 4 to find yn+1:
L1 V2 Liquid outlet = LN ; Vapor outlet = V1

2 𝐿𝑛 𝑥 𝑛 𝑉 1 𝑦 1 − 𝐿0 𝑥 0
Total overall balance for N stages: 𝑦 𝑛+1= +
L2 V3 𝑉 𝑛+1 𝑉 𝑛+1
L0 + VN+1 = LN + V1 Eq 1

Overall component balance for N stages: The operating line


Ln-1 Vn
L0x0 + VN+1yN+1 = LNxN + V1y1 Eq 2
n • The operating line relates the
Vn+1 For the first n stages, the overall inlet and outlet are: concentration yn+1 in the V stream with
Ln
Liquid inlet = L0 ; Vapor inlet = Vn+1 xn in the L stream passing it
Liquid outlet = Ln ; Vapor outlet = V1
• The terms V1, y1, L0 and x0 are
LN-1 VN Total overall balance for the first n stages: constant and usually known or can be
N determined from Eqs 1 – 4
L0 + Vn+1 = Ln + V1 Eq 3
VN+1
LN Overall component balance for the first n stages:

L0x0 + Vn+1yn+1 = Lnxn + V1y1 Eq 4 5


McCabe-Thiele Method
• McCabe and Thiele has developed a mathematical-graphical method to determine the number of
theoretical trays or stages needed for separation of a binary mixture A and B (always refer to A as the
more volatile component in this lecture)

• Main assumptions:
• Both components have equal and constant molar enthalpies of vaporization (latent heats). Lead to constant molal
• Sensible heat, CpΔT, is negligible compared to latent heat. overflow assumption
• Column is insulated (no heat loss on each stage).
• Column pressure is constant (thermodynamics can be done at a single pressure).

McCabe-Thiele Method:

• Rectifying section operating line Determine the number of


• Stripping section operating line theoretical trays and the
• Feed condition & the “q” line feed tray location
Rectification section

Stripping section

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Rectifying Section Operating Line
Total material balance: Component material balance:

𝑉 𝑛+1 =𝐿𝑛 + 𝐷 𝑉 𝑛+1 𝑦 𝑛+1= 𝐿𝑛 𝑥 𝑛 + 𝐷 𝑥 𝐷


V1
y1
Rearrange to obtain the operating line: 𝐿𝑛 𝐷
𝑦 𝑛+1= 𝑥𝑛 + 𝑥
𝐿𝑛 𝑉 𝑛+1 𝑉 𝑛+1 𝐷
L D Using 𝑅=
1
xD xD
𝐷
L1 x1 𝐿𝑛 𝐷
y2 𝐿𝑛 𝐿𝑛 𝐷 𝐷 1 𝐷
2 𝑅𝐷
= = = = = =
L2 𝑉 𝑛 +1 𝐿𝑛 + 𝐷 𝐿𝑛 𝐷 𝑅 +1 𝑉 𝑛 +1 𝐿𝑛 + 𝐷 𝐿𝑛 𝐷 𝑅 +1
x2 + +
yn 𝐷 𝐷 𝐷 𝐷
n
Ln xn 𝑅 1
yn+1 V Substitute into the operating line: 𝑦 𝑛+1= 𝑥𝑛 + 𝑥
n +1 n+1
𝑅 +1 𝑅 +1 𝐷

F
zF

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Stripping Section Operating Line
Total material balance: Component material balance:

F 𝑉 𝑚+1 =𝐿𝑚 − 𝐵 𝑉 𝑚+1 𝑦 𝑚 +1=𝐿𝑚 𝑥𝑚 − 𝐵 𝑥 𝐵


zF

Rearrange to obtain the operating line:

m Assume constant molal overflow, 𝐿𝑚 =𝐿 𝑁 =constant and 𝑉 𝑚+1 =𝑉 𝑁 =constant


Lm x m Vm+1 ym+1
m+1

yN
N
xN
yB
LN

xN
B
xB

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1. What is the purpose of reflux in a distillation column?
2. What is the advantage of multiple stage distillation vs. single stage?
3. List the major parts of a distillation column.

Think Think of the answers to the above questions


(3 min)

Pair Discuss the answer with your pair (3 min)

Share Share the answers (3 min)

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q-line and feed condition
• Condition of the feed stream F entering the tower determines the relation between the vapor V m in the stripping section and Vn
in the rectifying section; as well as between L m and Ln

• E.g. if the vapor is part liquid and part vapor, the vapor will add to V m to give Vn

Rectification
section

Stripping
section

Cold liquid feed Saturated liquid feed Partially vaporized Saturated vapor feed Superheated vapor
feed feed

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Feed condition
• In cold liquid feed, the entire feed
streams add to the liquid flowing
down the column • When the feed is
• In addition, some vapor condenses saturated liquid, it is at
to heat the feed to the bubble point its bubble point
• This makes the liquid flow even • No condensation is
greater in the stripping section and required to heat the feed,
decreases the flow of vapor to the so
rectifying section

Saturated liquid feed


Cold liquid feed

Part of the liquid


Feed partly vapor
The entire in the rectifying
 liquid portion of
feed section is
the feed becomes
becomes vaporized to cool
part of L and vapor
part of V the feed to a state
fraction becomes
of saturated vapor
part of V

Saturated vapor feed Superheated vapor feed


Partially vaporized feed 11
q-line and feed condition
• The condition of the feed can be represented by the quantity q defined as:

heat needed to vaporize 1 mol of feed at entering condition


𝑞=
molar latent heat of vaporization of feed

• HV = enthalpy of the feed at


• If the feed is a mixture of liquid and vapor,
𝐻𝑉− 𝐻𝐹 dew point
𝑞= is the fraction that is liquid
𝐻𝑉 − 𝐻 𝐿 • HF = enthalpy of the feed at its
entrance condition • The value of for cold-liquid feed:
• HL = enthalpy of the feed at
bubble point / boiling point

• For superheated vapor:


• Cold liquid feed:
• Saturated liquid feed (feed at bubble point):
• Partially vaporized feed:
• Saturated vapor feed (feed at dew point):
• Superheated vapor feed:

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Derivation of the q-line equation
• q can also be defined as the number of moles of saturated liquid produced on the feed plate by each mole of
feed added to the tower
Material balance:
𝐿𝑚 =𝑞𝐹 + 𝐿 𝑛 𝑉 𝑛=𝑉 𝑚 + (1 −𝑞 ) 𝐹

The point of intersection of the rectifying and stripping operating lines can be derived
by using the component material balance equations, without the tray subscripts
(because the intersection will have the same values of x and y)
𝑉 𝑛 𝑦= 𝐿𝑛 𝑥+ 𝐷 𝑥 𝐷 𝑉 𝑚 𝑦= 𝐿𝑚 𝑥 − 𝐵 𝑥 𝐵

Subtracting:
( 𝑉 𝑚 −𝑉 𝑛 ) 𝑦 =( 𝐿 𝑚 − 𝐿𝑛 ) 𝑥 − ( 𝐷 𝑥 𝐷 + 𝐵 𝑥 𝐵 )
Recall overall component
material balance over the whole
column: Derive the q-line equation:

𝐹 𝑧 𝐹 =𝐷 𝑥 𝐷 + 𝐵 𝑥 𝐵 𝑞 𝑧𝐹
𝑦= 𝑥−
𝑞−1 𝑞−1
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Finding theoretical number of stages, feed location …
• To determine the number of theoretical
trays, the rectifying and stripping
operating lines are drawn to intersect with
the q line

• Given the specification of the distillate


product composition xD, start to step off
the tray count from the top at xD

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Theoretical number of stages & feed location
• To determine the number of theoretical
trays, the rectifying and stripping operating
lines are drawn to intersect with the q line

• Assume total condenser and partial


reboiler is used

• Given the specification of the distillate


product composition xD, start to step off the
tray count from the top at xD

• Feed stage is normally located where the


stripping, rectifying and q lines intersect
a) improper location of feed tray
• However, engineering judgement is required
to locate the optimum feed location, taking
into account the feed condition and tray
efficiency

b) proper location of feed tray


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Example 2: Rectification of a Benzene-Toluene mixture
A liquid mixture of benzene-toluene is to be distilled in a fractionating tower at 101.3 kPa pressure. The feed of
100 kg mol/h is liquid, containing 45 mol% benzene and 55 mol% toluene, and enters at 327.6 K. A distillate
containing 95 mol% benzene and 5 mol% toluene and a bottoms containing 10 mol% benzene and 90 mol%
toluene are to be obtained. The reflux ratio is 4:1. Calculate:
a) The kg moles per hour distillate and bottoms
b) The number of theoretical trays needed

Average heat capacity of the feed is 159 kJ/kmol.K and the average latent heat is 32099 kJ/kmol. VLE data:

Mole fraction of benzene


Vapor pressure (kPa)
T (K) at 101.325 kPa
Benzene Toluene xA yA
353.3 101.32 1.000 1.000
358.2 116.9 46.0 0.780 0.900
363.2 135.5 54.0 0.581 0.777
368.2 155.7 63.3 0.411 0.632
373.2 179.2 74.3 0.258 0.456
378.2 204.2 86.0 0.130 0.261
383.8 240.0 101.32 0 0
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Example 2: Solution
Given F = 100 kmol/h; xF = 0.45; xD = 0.95; xB = 0.10; R = 4

𝐹 =𝐷+ 𝐵

𝐹 𝑥 𝐹 =𝐷 𝑥 𝐷 + 𝐵 𝑥 𝐵

Solve for D and B D = 41.2 kmol/h and B = 58.8 kmol/h

From the rectifying section 𝑦 = 𝑅 𝑥 + 1 𝑥 𝑦 𝑛+1=


4
𝑥𝑛 +
1
( 0.95 )
𝑛+1
operating line 𝑅 +1 𝑛 𝑅 +1 𝐷 4+ 1 4+ 1
𝑦 𝑛+1=0.8 𝑥𝑛 +0.19
Determine the value of q. From the boiling point diagram (T-x-y), at x F=0.45, the boiling point of the feed is ~367 K.

𝑞=
𝐻𝑉− 𝐻𝐹 𝐻 𝑉 − 𝐻 𝐿 =latent heat=32099 kJ / kgmol
𝐻𝑉 − 𝐻 𝐿
𝐻 𝑉 − 𝐻 𝐹 =( 𝐻 𝑉 − 𝐻 𝐿 ) + ( 𝐻 𝐿 − 𝐻 𝐹 )
𝐻 𝐿 − 𝐻 𝐹 =𝐶 𝑃𝐿 ( 𝑇 𝐵 − 𝑇 𝐹 )
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390

380

370

360
T (K)

350

340

330
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

xA, yA

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Example 2: Solution
𝐻 𝐿 − 𝐻 𝐹 =𝐶 𝑃𝐿 ( 𝑇 𝐵 − 𝑇 𝐹 ) 𝑇 𝐵 =boiling temperature of the liquid feed =367 K
𝑇 𝐹 =feed temperature =327.6 K
𝐻 𝑉 − 𝐻 𝐹 ( 𝐻 𝑉 − 𝐻 𝐿 ) + 𝐶 𝑃𝐿 ( 𝑇 𝐵 −𝑇 𝐹 )
𝑞= =
𝐻𝑉 − 𝐻 𝐿 𝐻𝑉 − 𝐻 𝐿

32099+159 ( 367 −327.6 )


𝑞= =1.195
32099

𝑞 𝑧𝐹 1.195 0.45
𝑦= 𝑥− 𝑦= 𝑥−
𝑞 −1 𝑞 −1 1.195− 1 1.195 −1
𝑦 =6.13 𝑥 −2.31

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Example 2: Solution
1

0.9
y-x equilibrium curve
0.8 Rectifying section operating line

0.7 q line
y=x line (45° line)
0.6

0.5
yA

0.4

0.3

0.2
Stripping section operating line
0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

xA
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1

0.9

0.8

0.7

0.6

0.5
yA

0.4

0.3

0.2

0.1

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

xB=0.10 xF=0.45 xA xD=0.95


Example 2: Solution
• Draw the rectifying operating line starting from x=y=x D=0.95 to the y-intercept when x=0, i.e. (0, 0.19)

• Draw the q-line starting from x=y=xF=0.45 to another point calculated using the q-line equation

• The rectifying operating line and the q line will intercept.

• The stripping operating line is drawn starting at the point x=y=x B=0.10 to the point of intersection between the rectifying
operating line and the q line.

• Start to count the number of stages by stepping off at x D=0.95 until xB=0.10

• The feed location is the stage where one side lies on the rectifying line and one side lies on the stripping line. In this example,
the feed stage is located at stage no. 5

• Note: partial reboiler is an equilibrium stage. Thus, the total number of theoretical stage obtained from the graph must minus
the partial reboiler stage.

• In this example, we obtain a total of 7.6 stages. Thus, there are 6.6 theoretical stage after taking out the reboiler.

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Heating and cooling requirement
If saturated steam is used as the heating medium, the
• Heat loss from a large insulated column is steam required at the reboiler is:
relatively small, and the column itself is
essentially adiabatic 𝑉𝜆
˙ 𝑆=
𝑚
𝜆𝑆

• The heat effects of the entire unit are confined to


𝑚
˙ 𝑆=steam consumption
the condenser and the reboiler 𝑉 =vapor rate ¿ reboiler
𝜆 𝑆=latent heat of steam
𝜆=molal latent heat of mixture
• If the average molal latent heat is λ and the total
sensible heat in the liquid stream is small, the If water is used as the cooling medium in the condenser and the
heat added in the reboiler, q, is Vλ (unit: Watts or
condensate is not subcooled, the cooling water requirement is:
Btu/hour)
𝑉𝜆
˙ 𝑊=
𝑚
• When the feed is liquid at its bubble point (q=1), ( 𝑇 2 −𝑇 1 ) 𝑐 𝑃𝑊
the heat supplied in the reboiler is approximately
equal to that removed in the condenser. This is
not true for other values of q. 𝑚
˙ 𝑊 =flow rate of cooling water
( 𝑇 2 − 𝑇 1 ) =temperature rise of cooling water
𝑐 𝑃𝑊 =specific heat of cooling water

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Example 3 – McCabe-Thiele Method
A continuous fractionating column is to be designed to separate 30 000 kg/h of a mixture of 40 wt.% benzene and 60 wt.% toluene
into an overhead product containing 97 wt.% benzene and a bottom product containing 98 wt.% toluene. A reflux ratio of 3.5 mol to
1 mol product is to be used. The molal latent heats of benzene and toluene are 7 360 and 7 960 cal/mol, respectively. Benzene and
toluene form a nearly ideal system with a relative volatility of about 2.5. The equilibrium data is given. The feed has a boiling point
of 95°C at a pressure of 1 atm.

a) Calculate the moles of overhead product and bottom product per hour

b) Determine the number of ideal plates and the position of the feed plate

i. If the feed is liquid and at its boiling point


ii. If the feed is liquid and at 20°C (specific heat 0.44 cal/g.°C)
iii. If the feed is a mixture of two-thirds vapor and one-third liquid

c) If steam at 20 lbf/in2 (1.36 atm) gauge is used for heating, how much steam is required per hour for each of the above three
cases, neglecting heat losses and assuming the reflux is a saturated liquid? (Hint: use steam table to get the heat of vaporization of
steam at this condition)

d) If cooling water enters the condenser at 25°C and leaves at 40°C, how much cooling water is required, in cubic meters per hour?

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Example 3 – McCabe-Thiele Method
Equilibrium data:

Mole fraction of benzene at


Vapor pressure (kPa)
T (°C) 101.325 kPa
Benzene Toluene xA yA
80.1 101.32 1.000 1.000
85 116.9 46.0 0.780 0.900
90 135.5 54.0 0.581 0.777
95 155.7 63.3 0.411 0.632
100 179.2 74.3 0.258 0.456
105 204.2 86.0 0.130 0.261
110.6 240.0 101.32 0 0

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Example 3 – Answers
a) Overhead product: 153.4 kmol/h; Bottom product: 196.6 kmol/h

b) Number of ideal plates and the location of feed plate for each case.

Rectifying operating line:

i. q=1; q line: (vertical line)


ii. q=1.37; q line:
iii. q=1/3; q line:

c) Steam required for each case


iv. 10 520 kg/h
v. 12 500 kg/h
vi. 6 960 kg/h

d) Cooling water needed in cubic meters per hour: 367.5 m3/h

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Reflection
• What is the purpose of reflux in a distillation column?
• What is the advantage of multiple stage distillation vs. single stage?
• What is Constant Molal Overflow? What is the implication of this assumption?
• List the major parts of a distillation column.
• What are total condenser and partial condenser? When to use which? Which one is
an equilibrium stage?
• Why is partial reboiler counted as an equilibrium stage but not total condenser?
• What are the five possible feed conditions? How does the feed condition affect the
cooling and heating requirement?
• What are the lines necessary to count the number of stages in a distillation column?
• What can we deduce from the number of stages in a distillation column?

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