3 - Distillation Final

6P2X0: Separation technology
Distillation
Prof. dr. ir. Kitty Nijmeijer
Membrane Materials and Processes

Department of Chemical Engineering and Chemistry
Eindhoven University of Technology
Information in this lecture is taken from:

Industrial Separation Processes -
Fundamentals
André B. de Haan, Hans Bosch
2013, De Gruyter GmbH, ISBN 978-3-11-030669-9
Recap: Continuous flash distillation
a12 x
y=
(a12 - 1) x + 1
KB KA
q = -z - (1 - z )
1- KB 1- KA
/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 1

From flash drums to a column
2.3 Multi
Fig. 2.10 General flowchart of a plate distillation column.
Although a significant advance, this multiple flash drum

industrially. Operation and design is easier if part of t
/ Department of Chemical Engineering and Chemistry condensed and returned to the first stage, reflux,
28-02-18 PAGE 2 and if p
stream is evaporated and returned to the bottom stage, boi
• Relative volatility: α > 1.2

• Feed at equilibrium stage
• Trays and packings to maximize
contact
• Number of stages N < 100
• Tmax = 300-400 oC (high pressure
steam)
• Tmin = 40-50 oC (coolant: water)
• Column pressure: 2 mbar < Ptot <
50 bar
• Temperature also determined by
pressure (P< → T<)

Continuous distillation
• Separation of F into D and B:

• Distillation separates a feed F into a
distillate D and a bottom B.
• For binary mixtures, F, D and B are

used for the mole fraction of the
most volatile component (xF, xD, xB).

Mass balances
30 2 Evaporation and distillation
• If the molar enthalpy for vaporization

is equal for two components:
• Constant liquid and vapor flows
• No energy balance
• Mass balance and vapor-liquid

equilibrium are of importance.
Fig. 2.12 Distillation column overall mass balance envelope.
/ Department of Chemical Engineering and Chemistry In binary distillation the specification of xDPAGE
28-02-18 and 6xB for the
nent fixes the distillate and bottoms flow rates D and B
Mass balances
• Overall mass balance:

• F=D+B
• Mass balance volatile component
• xF . F = xD . D + xB . B
• If F and xF are known:
and
/ Department of Chemical Engineering and Chemistry In binary distillation the specification of xDPAGE
28-02-18 and 7xB for the
nent fixes the distillate and bottoms flow rates D and B
Equilibrium curve
• Relative volatility:
g 1 P1sat K1 y/x
a12 = = =
g 2 P2sat
K 2 (1 - y ) / (1 - x )
• Equilibrium curve:
a12 x
y=
(a12 - 1) x + 1
• The equilibrium curve: relation between composition of
a liquid on a tray and the composition of the vapor with
which it is in equilibrium.
The equilibrium curve: from x to y
• The equation for the equilibrium curve

can be applied to every stage:
• And so on…

Sections
• ‘Equal molar overflow’

• Rectifying section
• The flow rates of V’ and L’ are
constant.
• Feed section
• V’ and L’ are replaced by V’’ and
L’’.
• Stripping section
• The flow rates of V’ and L’ are
constant.
• Whilst flow rates are constant,
composition is not!
Operating line rectifying section
• Mole balance volatile

component (V’ and L’ constant):
• Operating line rectifying section:

• Relationship between yn+1 and xn,

both on the same tray.
• Yields a straight line with slope L’/V’.
• The slope is always < 1.
• Because in the rectifying section:
V’>L’
• Passes through the point (xD, xD).
• Which occurs when y = x.

Reflux ratio, R
• Reflux is necessary to remove the last traces of

high-boiling component from the overhead stream.
• External reflux ratio
• L’/D = R
• Internal reflux ratio
• L’/V’

Reflux
• Because V’ = L’ + D, the operating line can be related

to the reflux ratio (R = L’/D):

Reflux
• Using the expressions from the last slide, the operating

line for the rectifying section can be modified:
• Setting R is the freedom of the designer.

• A certain value of R results in fixed values of the slopes
of the operating lines (L’/V’ and L’’/V’’).

• Operating line:
• Straight line
• Intercepts x = y at y = xD.
• xD and R may be chosen freely.

Operating line stripping section
• Mole balance over total

section:
• Operating line stripping

section:

• Relationship between ym+1 and xm

• Yields a straight line with slope L’’/V’’.
• The slope is always > 1:
• Because in the stripping section: L’’>V’’
• Passes through the point (xB, xB).


Operating lines
• Operating lines represent the mass balances in the

column.
• An increase or decrease in feed influences the slope
and point of interception of the operating lines.
• An increase in feed flow rate increases the liquid
flow rate in the stripping section and/or increases
the vapor flow rate in the rectifying section.
• Temperature and pressure influence the flow rates of
both liquid and vapor.
• This may be quantified by a mass balance over the feed
tray.

From x to y to x to y…
a12 x
Equilibrium curve y= Operating line
(a12 - 1) x + 1
xB

Feed stage: FL and Fv
L” = L’ + FL L
q=
FL = q.F F
L”-L’ = q.F L” = L’ + qF
V’ = V” + FV V
1− q =
Fv = (1-q).F F
V”-V’= -(1-q).F V” = V’ - (1-q)F

Feed line: interception between the
operating lines
• Rectifying section:
• Stripping section:
• With L”-L’ = q*F

V”-V’= -(1-q)*F Because: F = D + B

Feed line: interception between the
operating lines 34 2 Evaporation and distillation
• Straight line with slope –q/(1-q).

• Passes through the point (xF,xF).
• Graphically; the point of interception
between the operating lines.
Fig. 2.15 (a) Mass balance envelope and (b) q-line for the feed stage.
• When R is changed, the point of
interception shifts, but it will never leave
the q-line. Fh + V h + L h = L h + V h F
″
V
′
L
″
L
′
V (2.2
Rewriting the mass balance Eq. 2.27 in terms of V ″ − V ′ and substitution in
the energy balance gives:
FhF + (L ″ − L ′ ) hV − FhV = (L ″ − L ′ ) hL (2.3
which is easily rearranged to yield:
L″ − L′ hV − hF
q≡ = (2.3
/ Department of Chemical Engineering and Chemistry F hV − hL 28-02-18 PAGE 24
Energy balance
• Energy balance (in case 0 < q < 1):

FhF + V hV + LhL = L hL + V hV
'' ' '' '
• Combining with:
V -V = L - L - F
'' ' '' '
• This results in:

FhF + ( L - L ) hV - FhV = ( L - L ) hL
'' ' '' '
L'' - L' hV - hF hV - hF
q= = =
F hV - hL DH vap
• This is the heat needed to evaporate 1 mole of feed.

Sub-cooled or superheated feed
• Sub-cooled liquid:
• The feed condenses a part of V’’.
• FL > F and V’ < V”
• FV < 0, so q > 1
• Superheated vapor:
• The feed evaporates a part of L’.
• FV > F and L’’<L’
• FL < 0, so q < 0

Slope of the feed line
L
q=
F
V
1− q =
F

Determination of the amount of trays
• Equilibrium curve, operating line and q-line known.

• The operating line relates the solute concentration in
the liquid going downward between two trays.
• The equilibrium curve relates the solute concentration
in the vapor leaving a certain tray to the solute
concentration in the liquid leaving the same tray.

• Equilibrium curve, operating line and q-line known.

• Determination of the amount of equilibrium stages.
• Determination of the position of the feed tray.
• Construct a staircase between the equilibrium curve
and the operating line.
• From (xB, xB) to (xB, yB) to (yB, xN) to (xN, yN) and so
forth…

• Convention: draw from top (xD, xD) to bottom (xB, xB).

(y1, x1)
(xD, xD)
(y2, x2)
(y2, x1)
Feed stage
Equilibrium curve

McCabe-Thiele diagram

Optimal feed stage position
• The feed is introduced at the stage which bridges

both the operating lines.

Suboptimal feed

Staircase ‘steps’ versus stages
• 5 separation steps • 4 theoretical stages
Reboiler
stage

R and N
• For every distillation, there is an

infinite amount of combinations of
the reflux ratio R and the
theoretical amount of stages N.
• A higher R means that N is lower.
• Higher energy consumption.
• A minimal reflux results in the
lowest energy consumption.
In binary distillation the specification of xD and xB for th

/ Department of Chemical Engineering and Chemistry nent fixes the distillate and bottoms
28-02-18
flowPAGE
rates35 D and B
overall component material balance:
Stages versus reflux ratio
• Minimum number of • Minimum reflux ratio

theoretical
38 stages
2 Evaporation and distillation
Operating lines are equal to

the equilibrium curve Lower R
Fig. 2.18 Determination of (a) minimum number of theoretical stages and (b) minimum
reflux ratio in a McCabe-Thiele diagram.
Optimal reflux ratio, Ropt
• Industrially: 1.1Rmin < Ropt < 1.5Rmin

• Higher R:
• Recirculation of liquid
• Less trays, lower investment
• Higher column diameter

Limitations to the McCabe-Thiele
approach
• Limitations • Adaptations
• Binary mixtures • Experimental VLE data
• Ideal behaviour • Fictive mole masses
• Equal molar overflow • Stage efficiencies
• Equilibrium at every
stage

Assignment
• Separation of components A (most volatile) and B

• Relative volatility: α = 3
• Liquid boiling feed with xF = 0.35
• Bottom product: xB = 0.05
• Top product: xD = 0.98
• Reflux ratio: R = 2
• Required:
• Amount of equilibrium steps and amount of stages.
• Minimum number of theoretical stages (Nmin at R = ∞)
• Minimum reflux ratio (Rmin at N = ∞)

Construct a McCabe-Thiele diagram
• Equilibrium curve: a12 x

y=
(a12 - 1) x + 1
• Feed line:
• Liquid boiling feed: q = 1
• Operating line
rectifying section:
• Operating line stripping section:

• Straight line through (xB, xB) and the point of
interception between the operating line of the rectifying
section and the feed line.
Construct a McCabe-Thiele diagram
(xD, xD) = (0.98, 0.98)
(xF = 0.35)
(xB, xB) = (0.05, 0.05)

Number of stages
N = 12
Number of stages = 11
(one for the reboiler)

Minimum number theoretical stages, Nmin
Nmin = 6
Number of stages = 5

Minimum reflux ratio, Rmin
• Point of interception between the equilibrium line

and the feed line: (0.35, 0.618)
• So the operating line of the rectifying section passes
through (xD, xD) (xD = 0.98) and (0.35, 0.618):
• Rmin = 1.354

Depropanizer - working pressure: 13 bar
• Calculate B and D.
• Calculate α.
• Calculate Nmin (R = infinite).
• Calculate Rmin and Ropt.
• Determine N.
• Calculate H.
• Calculate the energy
consumption.
Propane Butane
80
A = 4.53678 A = 4.35576
B = 1149.36 B = 1175.581
C = 24.906 C = -2.071
Depropanizer - working pressure: 13 bar
• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 1: Calculate B and D
• Overall mass balance: F = D + B

• B=F–D
• Mass balance volatile component: xF.F = xD.D + xB.B
• Using the given values for F and xF:

Assignment: Depropanizer
(working pressure: 13 bar)
• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 2: Calculate α
B
• Antoine equation: 10
log P ( bar ) = A -
C + T (K)
• Propane: A = 4.53678, B = 1149.36, C = 24.906

• Butane: A = 4.35576, B = 1175.581, C = -2.071
• Two options for αavg:

• Calculate α at Tavg.
• Calculate α at Ttop and Tbottom and calculate the average:
!"#$ = !& ' !(

Step 2: Calculate α
21.2
• At Tavg = 60 a= = 3.3
oC:
6.4
13.7
• At Ttop = 40 C:
o
a= = 3.6
3.8 !"#$ = 3.3
31.3
• At Tbottom = 80 C: a =
o
= 3.0
10.2

Check the working pressure!
• Top pressure: P = 0.95 ×13.7 + 0.05 × 3.8 = 13.2
• Bottom pressure: P = 0.10 × 31.3 + 0.90 ×10.2 = 12.3
• So the working pressure is 13 bar!
• Of course, we used: P = å xi Pi sat

• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 3: Calculate Nmin
• Construct the equilibrium curve with α = 3.3.
a12 x
y=
(a12 - 1) x + 1

• When Nmin is reached:

• R=∞
• D = B = 0 (total reflux)
• Operating line rectifying section:
yn+1 = xn
=1 =0
• Operating line stripping section:
ym+1 = xm
=1 =0
• So on the operating line, the following is valid:

y2 = x1 and y3 = x2 and yn+1 = xn
• Also, because there is equilibrium on every tray:

y1
y1 = K A x1 = K A y2
Fill in
x1 y2
y2 = K A x2 = K A y3
x2 y3
y1 = ( K A ) yn+1
n x3

• At the top: y1 = xD
• At the bottom: yn+1 = xB Fill in
y1 = ( K A ) yn+1
n
xD = ( K A ) xB and 1 - xD = ( KB ) (1 - xB )
n n
• So:
xD = ( K A ) xB
n N min
xD æ KA ö xB
=ç ÷
1 - xD = ( KB ) (1 - xB ) 1 - xD è K B ø 1 - xB
n

• From the last slide:

N min
xD æ KA ö xB KA
=ç ÷ with a AB =
1 - xD è K B ø 1 - xB KB
• We now apply the Fenske equation:
é æ xD ö æ xB ö ù
ln êç ÷ ç ÷ú éæ 0.95 ö æ 0.10 ö ù
ln êç ÷ ç ÷ú
ë è 1 - xD ø è 1 - xB ø û = ë
è 1 - 0.95 ø è 1 - 0.10 øû
N min = = 4.3
ln a AB ln 3.3
• Nmin = 5

Graphical McCabe-Thiele determination
of Nmin
Nmin = 5

• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 4: Calculate Rmin
• At the pinch, the operating line and the q-line

intercept on the equilibrium curve.
• Infinite number of trays pinch
• Minimum R

• Mass balance over the top:

V yn +1 = Lxn + DxD
' '
V ' (1 - yn +1 ) = L' (1 - xn ) + D(1 - xD )

• Infinite number of trays
• The composition at tray n is nearly
equal to the composition at tray n+1.
• This implies:
yn+1 = y¥ and xn = x¥


V yn +1 = Lxn + DxD
' '
V ' (1 - yn +1 ) = L' (1 - xn ) + D(1 - xD )
yn+1 = y¥ and xn = x¥
y∞ L' x∞ + Dx D x∞
= ' = α AB
1− y∞ L (1− x∞ ) + D 1− x D 1− x∞ ( )
y∞ L' x∞ + Dx D x∞
= ' = α AB
1− y∞ L (1− x∞ ) + D 1− x D 1− x∞ ( )
y
KA =
x
KB =
1− y y∞ L' x∞ + Dx D x∞
1− x = ' = α AB
1− y∞ L (1− x∞ ) + D 1− x D
( ) 1− x∞
KA
α AB =
KB
• From the last slide:

y¥ L' x¥ + DxD x¥
= ' = a AB
1 - y¥ L (1 - x¥ ) + D (1 - xD ) 1 - x¥
• We may now apply the Underwood equation:
xD 1 - xD
- a AB 0.95
- 3.3
0.05
æ L' ö x¥ 1 - x¥
Rmin =ç ÷ = = 0.40 0.60 = 0.92
è D ømin a AB - 1 3.3 - 1
• With x∞ = xF if q = 1
• Rmin = 0.92
Graphical determination of Rmin
• Rmin: From the slope:
• We find that Rmin = 0.92

Step 4: Calculate Ropt
• Conventionally, distillation at Ropt = 1.2 Rmin
• Ropt = 1.1

• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 5: Determine N
• The slope of the rectifying section is given by:

Ropt/(Ropt+1) = 0.53

Step 5: Determine N
N=9

Step 5: Stage efficiency
• Usually, equilibrium has not been fully approached

on each tray.
• The Murphree vapor efficiency (EMV) may be used to
construct a pseudo-equilibrium curve:
yn - yn +1
EMV = *
yn - yn +1
• In this equation, yn* is the hypothetical equilibrium

composition.

Step 5: Pseudo-equilibrium

• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 6: Calculate H
• We now know:
• Equilibrium on each tray: N = 9
• Height of one stage: HT = 0.60 m
• Stage efficiency: EMV = 0.70
N 9
• Actual number of stages: NT = - 1= - 1 = 11.8
• N = 12 EMV 0.70
T
• Height of the column: H = N × H = 12 × 0.60 = 7.2

T T
• H = 7.2 meter

• Calculate α.
• Determine N.
• Calculate H.
consumption.
80

Step 7: Energy consumption
• Energy balance over the column:

Reboiler in = Condenser Out
QR = QC
QC = D.(R+1).ΔHvap
• If steam is used for heating in the reboiler:
QR × M steam
fm,steam =
DH vap , steam
• If cooling water is used for cooling in the condenser:

QC
fm,C =
CP, water (Tout - Tin )
• Given:
• Steam: ΔHvap = 2100 kJ/kg (Mw = 0.018 kg/mol)
• Propane: ΔHvap = 425 kJ/kg (Mw = 0.044 kg/mol)
• Butane: ΔHvap = 386 kJ/kg (Mw = 0.058 kg/mol)
• Mass balance over the reboiler and the feed stage:

V = L - B = qF + L - B = qF + RD - B
'' '' '
• Apply q = 1:
V '' = F + RD - B = 500 + 1.1×176 - 324 = 370 mol/s

• Energy consumption of the reboiler:

E = xB ×V × M prop × DH vap, prop + (1 - xB )V × M but × DH vap,but
'' ''
E = 0.10 × 370 × 0.044 × 425 + 0.90 × 370 × 0.058 × 386 = 8147 kJ/s
• Steam consumption:
QR × M steam
fm,steam =
DH vap , steam
8147
fm,steam = = 3.9 kg/s
2100

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6P2X0: Separation technology

Prof. dr. ir. Kitty Nijmeijer

Membrane Materials and Processes

Information in this lecture is taken from:

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 1

Fig. 2.10 General flowchart of a plate distillation column.

Although a significant advance, this multiple flash drum

• Relative volatility: α > 1.2

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 4

• Separation of F into D and B:

• For binary mixtures, F, D and B are

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 5

• If the molar enthalpy for vaporization

• Mass balance and vapor-liquid

Fig. 2.12 Distillation column overall mass balance envelope.

• Overall mass balance:

• If F and xF are known:

• The equation for the equilibrium curve

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 9

• ‘Equal molar overflow’

• Mole balance volatile

• Operating line rectifying section:

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 11

• Relationship between yn+1 and xn,

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 12

• Reflux is necessary to remove the last traces of

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 13

• Because V’ = L’ + D, the operating line can be related

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 14

• Using the expressions from the last slide, the operating

• Setting R is the freedom of the designer.

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 15

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 16

• Mole balance over total

• Operating line stripping

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 17

• Relationship between ym+1 and xm

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 18

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 19

• Operating lines represent the mass balances in the

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 20

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 21

V”-V’= -(1-q).F V” = V’ - (1-q)F

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 22

• With L”-L’ = q*F

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 23

• Straight line with slope –q/(1-q).

• Energy balance (in case 0 < q < 1):

• This results in:

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 25

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 26

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 27

• Equilibrium curve, operating line and q-line known.

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 28

• Equilibrium curve, operating line and q-line known.

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 29

• Convention: draw from top (xD, xD) to bottom (xB, xB).

Operating line rectifying section

Operating line stripping section

/ Department of Chemical Engineering and Chemistry 28-02-18 PAGE 30