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INTRODUCTION TO COLUMN

DISTILLATION
1 Nestor Eduardo Sanchez MSc.
Separation process and NT
Chemical Engineering
DISTILLATION PROCESS

In USA: 1.2 million


90% to 95% of the barrels of crude oil
separations in a day (40.000
industry. distillation
columns).

http://www.youtube.com/watch?v=gYnGgre83CI
DEVELOPING A DISTILLATION CASCADE
If we would like to perform a
separation for the vapor stream we
need to increase the Pressure of the
system

Presssure
Several flash can be extended
into a process that produces
one pure vapor and one pure
liquid product.

If we would like to perform a


separation for the liquid stream we
need to decrease the Pressure of
the system
3
DEVELOPING A DISTILLATION CASCADE
Intermediate streams could be treat
in another flash distillation process.

Larger flash cascade to opérate this


process.

4
DEVELOPING A DISTILLATION CASCADE

Main drawback:
Several compressors

5
Since P1>P2, Pressure of L1 Isothermal column
must be decrease before feed distillation
to stage 2.
DEVELOPING A DISTILLATION CASCADE
• Isobaric processes are cheaper than
isothermal.
• Force the temperatura to vary
• Employ several reboilers
Temperarue decrease

6
DEVELOPING A DISTILLATION CASCADE
Reflux: Top vapor is condensed and
returned to stage 1.

Boilup: Bottom liquid is vaporized and


returned to stage 5

Control the internal flow of the column

7
DEVELOPING A DISTILLATION CASCADE
All the condensation
required for the distillation
we can apply into a top
condenser.

All the heat required for the 8


distillation we can apply
into a bottom reboiler
DEVELOPING A DISTILLATION CASCADE

V2 is partially condesed by L1, while L1 is


partially vaporized.

Since the heat of vaporization per mole is


approximately constant.

Condensation of 1 mole of vapor will


vaporize approximately 1 mole of liquid.

Thus liquid and vapor flow rates tend to


remain constant

9
DISTILLATION COLUMN

Enriching or
rectifying section

Stripping section

10
A component will tend to exit in the vapor if yiV>xiL
If KiV/L>1  tend to exit in the vapor
If KiV/L<1  tend to exit in the bottoms
DISTILLATION EQUIPMENT (TRAY)

11
DISTILLATION EQUIPMENT (SIEVE TRAY)

12

http://articles.compressionjobs.com/articles/oilfield-101/2710-
distillation-columns-towers-column-control-?start=1
DISTILLATION EQUIPMENT (VALVE TRAY)

13

http://articles.compressionjobs.com/articles/oilfield-101/2710-
distillation-columns-towers-column-control-?start=1
DISTILLATION EQUIPMENT (CAP VALVE
TRAY)

14

http://articles.compressionjobs.com/articles/oilfield-101/2710-
distillation-columns-towers-column-control-?start=1
DISTILLATION EQUIPMENT (TRAY)

Table 1. Comparison of types of trays

15
FLOW REGIMES
Bubble

Increase vapor flow rate


Foam

Froth (Optimal)

Spray 16
SPECIFICATIONS
 A number of variables must be specified in a binary
distillation column:

 There are a number of heuristics (recommendations) that


can be followed to choice a variable value.
 In design problems, the desired separation is set, and a
column is designed that will achieve this separation.

17
18
SIMULATION
 In simulation problems, the column has already been built
and we wish to predict how much separation can be
achieved for a given feed.

19
EXTERNAL MASS AND ENERGY BALANCE
Qc

TD
XD
D
RECTIF.
Overall mass balance
SECTION TO
XO F=D+B
TF LO
Volatile component
ZF
FEED Zi F = x D D + x B B
F SECTION
Energy balance
hF F + Q R = hD D + hB B + Q c
Column is adiabatic
STRIPPING
SECTION TB
QR
XB 20
B
EXTERNAL MASS AND ENERGY BALANCE
V1 Qc
y1 TD
XD
D Total Condenser
RECTIF.
Overall mass balance
SECTION TO
XO V1 = D + LO
TF LO
Volatile component
ZF
FEED y1 V1 = xD D + xO Lo
F SECTION
Reflux ratio
Lo
R=
D
STRIPPING
SECTION TB y1 = xo = xD
QR
XB 21
B
EXAMPLE 3-1

22
INTERNAL BALANCES
Qc
V1 D, xD
L𝑜
1
V2 2 L1
Rectification section
VJ J L2

VJ+1 LJ

FEED
F, z SECTION

VF+1 LF

VK F+1 LK−1

VN K Lk Stripping section
N LN
VN+1 23

QR N+1
B, xB
INTERNAL BALANCES
 We already developed the external balance equations.
 We can now proceed down the column in a stage-by-stage
fashion until we reach the bottom.
 This assumes that each stage is an equilibrium stage, but this
assumption may not be true. Vapor and liquid leave the stage
are in equilibrium

D
Qc
V1
Lo
1

V2 2 L1
VJ J L2

LJ 24
VJ+1
INTERNAL BALANCES (TOP SECTION)
Orange Section (First stage) If it is an equilibrium stage:
V2 = L1 + D
H2 = H2 (y1 )
y2 V2 = x1 L1 + xD D h1 = h1 (x1 )
H2 V2 + Q c = h1 L1 + hD D x1 = x1 (y1 )

Six equations with how many unknowns?


L1, V2, x1, y2, H2, and h1.

Write the six equations for the second stage

If it is an equilibrium stage:
Red Section (Second stage)
VJ = L2 + D HJ = HJ (yJ )

yJ VJ = x2 L2 + xD D h2 = h2 (x2 )
x2 = x2 (y2 ) 25
HJ VJ + Q c = h2 L2 + hD D
GENERAL STAGE (TOP SECTION)
Purple Section (General stage) If it is an equilibrium stage:
VJ+1 = LJ + D
HJ+1 = HJ+1 (yJ+1 )
yJ+1 VJ+1 = xJ LJ + xD D hJ = hJ (xJ )
HJ+1 VJ+1 + Q c = hJ LJ + hD D xJ = xJ (yJ )

D
Qc
V1
Lo
1

V2 2 L1
VJ J L2

LJ 26
VJ+1
INTERNAL BALANCES
Qc
V1 D, xD
L𝑜
1
V2 2 L1
Rectification section
VJ J L2

VJ+1 LJ

FEED
F, z SECTION

VF+1 LF

VK F+1 LK−1

VN K Lk Stripping section
N LN
VN+1 27

QR N+1
B, xB
STRIPPING SECTION BALANCE ENVELOPES, PARTIAL
REBOILER
 The partial reboiler acts as an equilibrium contact N+1.
 If xN+1 = xB, the N + 1 equilibrium contacts gives us exactly the
specified separation, and the problem is finished.
 If xN+1 < xB while xN > xB, the N + 1 equilibrium contacts gives slightly
more separation than is required.

VF+1 LF

VK F+1 LK−1 Red Section (Stage F+1)


VN K Lk
LF = VF+1 + B
N LN
VN+1 xF LF = yF+1 VF+1 + xB B
hF LF + Q R = HF+1 VF+1 + hB B
QR N+1

B, xB

28
BINARY STAGE-BY-STAGE SOLUTION
METHODS
 Solve the three balance equations and the three
equilibrium relationships simultaneously in an efficient
manner.
 Sorel (1893): Analytical method.
 Ponchon (1921) and Savarit (1922): graphical solutions of
Sorel’s method.

29
LEWIS METHOD (1922)
Qc
V1 D, xD
L𝑜
Rectification section
1 V1 = V2 = ⋯ = VJ+1 = ⋯ = VF = V
V2 2 L1
L1 = L2 = ⋯ = LJ = ⋯ = LF−1 = L
VJ J L2

VJ+1 LJ

FEED
F, z SECTION

VF+1 LF
Stripping section
VK F+1 LK−1
VF+1 = VK = ⋯ = VN+1 = V
VN K Lk
LF = LK−1 = ⋯ = LN = L
N LN
VN+1 30

QR N+1
LEWIS METHOD (1922)

 Equations will be valid if every time a mole of vapor is


condensed a mole of liquid is vaporized.
 This will occur if:
 The column is adiabatic.
 The specific heat changes are small compared to latent
heat changes:

 The heat of vaporization per mole, λ, is constant; that is,


λ does not depend on concentration.
 Or: The saturated liquid and vapor lines on an
enthalpy-composition diagram (in molar units) are
parallel.
31
LEWIS METHOD (1922)
 For some systems, such as hydrocarbons, the latent heat of
vaporization per kilogram is approximately constant. Then
the mass flow rates are constant, and constant mass
overflow should be used.
 The Lewis method assumes before the calculation is done
that CMO is valid.

32
LEWIS METHOD (1922) (TOP SECTION)

D
Qc
V1
Lo
1

V2 2 L1
VJ J L2

VJ+1 LJ

yJ+1 VJ+1 = xJ LJ + xD D

LJ xD D
yJ+1 = xJ + Since constant molar flow is valid…
VJ+1 VJ+1

𝐋 𝐱𝐃𝐃 OPERATING EQUATION IN THE 33


𝐲𝐉+𝟏 = 𝐱 𝐉 +
𝐕 𝐕 ENRICHING SECTION
LEWIS METHOD (TOP SECTION)
1. Use the column balances to calculate D and B.
2. Then L0 = (L0/D)D and V1 = L0 + D.
3. For a saturated liquid reflux: L0=L1=L2=L y V1=V2=V
4. At the top of the column we know that y1=xD
5. x1 can be calculated from the equilibrium at the stage 1.
6. y2 can be determined from:

7. We then proceed to the second stage, obtaining x2 from


equilibrium and y3 from the operation equation.
8. We continue this procedure down to the feed stage.
34
LEWIS METHOD (1922) (STRIPPING SECTION)
VF+1 LF

VK F+1 LK−1

VN K Lk
N LN
VN+1

QR N+1

B, xB

xF LF = yF+1 VF+1 + xB B

LF xB B
yF+1 = xF − Since constant molar flow is valid…
VF+1 VF+1

𝐋 𝐱𝑩𝑩 OPERATING EQUATION IN THE 35


𝐲𝐅+𝟏 = 𝐱 𝐅 − STRIPPING SECTION
𝐕 𝐕
LEWIS METHOD (1922) THE STRIPPING
SECTION
 At the stage k:

 With CMO, 𝐿 and 𝑉are constant, and the resulting


stripping section operating equation is:

 Once we know 𝐿/𝑉we can obviously alternate between the


operating Eq. and the equilibrium Eq.

36
FEED SECTION
• The phase and temperature of
D, XD the feed obviously affect the
vapor and liquid flow rates in
the column.
RECTIF. • For instance, if the feed is
SECTION liquid, the liquid flow rate
below the feed stage must be
V L greater than liquid flow above
the feed stage: 𝐋 > 𝐋
• If the feed is a vapor: 𝐕 > 𝐕
F
FEED
SECTION MASS BALANCE
F+L+V= V+L
V L
ENERGY BALANCE
hF F + hL L + HV V = HV V + hL L
STRIPPING
SECTION
37
B, XB
THE FEED STAGE
 If we assume CMO neither the vapor enthalpies or the
liquid enthalpies NOT vary much from stage to stage.
Thus:
hL ~hL HV ~HV

 And: FhF + V − V H~ L − L h

 From the mass balance: V − V = L − L − F

 Which can be substituted into the energy balance to give


us:
L − L (H − h)~ H − hF F

 We can now define q (quality) as:


38
L − L H − hF
q= =
F H−h
QUALITY
 Since q can be determined from enthalpies:

L = L + qF

 q is the amount of liquid in feed. Also:

V = V − (1 − q)F

39
MCCABE THIELE METHOD

On this graph the


McCabe and Thiele equilibrium
The operating Eqs. plot
(1925) developed a relationship can be
are straight lines (the
graphical solution solved from the y-x
operating lines) on a y-
method based on Lewis’ equilibrium curve and
x diagram.
method. the mass balances from
the operating lines.

41
MCCABE THIELE METHOD

V1 , 𝑦1 𝐋 𝐱𝐃𝐃
D, XD 𝐲𝐉+𝟏 = 𝐱 𝐉 +
𝐕 𝐕
Lo
R= 𝐋 𝐱𝐃
RECTIF. D
𝐲𝐉+𝟏 = 𝐱 𝐉 +
SECTION Lo , x o 𝐕 (𝟏 + 𝐑)

V L 𝐑 𝐱𝐃
𝐲𝐉+𝟏 = 𝐱𝐉 +
(𝟏 + 𝐑) (𝟏 + 𝐑)
F, Zf
FEED TOP SECTION
SECTION

V L

STRIPPING
SECTION
42
B, XB
MCCABE THIELE METHOD (TOP SECTION)
1
In the top section (Total
0,9
condenser): XD = xo = y1
0,8
Y (vapor mol fraction)

y1 XD
0,7

0,6

0,5

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 43
X (liquid mol fraction)
MCCABE THIELE METHOD (TOP SECTION)
1
𝐑 𝐱𝐃
0,9 𝒚=𝒙 +
(𝟏 + 𝐑) (𝟏 + 𝐑) y1
0,8
Y (vapor mol fraction)

XD
0,7 y2
0,6 x1
0,5
y3

0,4
x2
Operating top
0,3
line:
𝐑 𝐋
0,2 SLOPE: (𝟏+𝐑) = 𝐕
𝐱𝐃
0,1 B: (𝟏+𝐑)
0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1 44
X (liquid mol fraction)

Equilibrium Mass balance


MCCABE THIELE METHOD
 Top operating line is not valid for the stripping
section, while feed modifies the liquid and vapor
flow on the section under the feed stage.

𝐋 𝐱𝑩𝑩
𝐲𝐅+𝟏 = 𝐱𝐅 −
𝐕 𝐕

45
MCCABE THIELE METHOD (TOP SECTION)
1

0,9

0,8
Y (vapor mol fraction)

0,7

0,6 yN
0,5
yN+1
0,4 XN
𝐋 𝐱𝑩𝑩
0,3 𝐲𝐅+𝟏 = 𝐱𝐅 −
𝐕 𝐕
0,2

0,1 XB = XN+1
0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1 46
X (liquid mol fraction)
MCCABE THIELE METHOD (COMPLETE)

(A) optimum feed stage (stage 3);


(B) feed stage too high (stage 2);
(C) feed stage too low (stage 5)

47
MCCABE THIELE METHOD (FEED LINE)
 In any section of the column between feeds
and/or product streams the mass balances are
represented by the operating line.
 The feed stage is similar to a flash distillation,
with an operating line:
q 1
y= x+ zF
q−1 1−q
 If all the feed is saturated liquid: q=1, the slope is
infinitive and the feed line is vertical.
 Let’s check other options…

48
FEED LINE CALCULATION (SUBCOOLED
FEED)
𝐋𝐢𝐪𝐮𝐢𝐝 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞
L=F+L+c
Vapor 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞
V=V+c

c is the vapor condensed


𝐃𝐞𝐟𝐢𝐧𝐢𝐭𝐢𝐨𝐧 𝐨𝐟 𝐪𝐮𝐚𝐢𝐥𝐢𝐭𝐲 (𝐪)

L − L H − hF
q= =
F H−h
Then combined liquid mass balance and q
λ + CPL (Tbubble − TF ) H − hF
q= c= F−F
λ λ
Solving this..
49
λc = FCPL (Tsat − TF )
FEED LINE CALCULATION
(SAT. LIQUID AND SAT. VAPOR)

Sat. liquid Sat. Vapor

50
FEED LINE CALCULATION
(LIQUID AND VAPOR MIXTURE)

𝐋𝐢𝐪𝐮𝐢𝐝 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞


L = 𝐿𝐹 + L
Vapor 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞
V = VF + V
𝐃𝐞𝐟𝐢𝐧𝐢𝐭𝐢𝐨𝐧 𝐨𝐟 𝐪𝐮𝐚𝐢𝐥𝐢𝐭𝐲 (𝐪)

L − L H − hF
q= =
F H−h

L − L = 𝐿𝐹

LF
q=
F
51
FEED LINE CALCULATION
(SUPERHEATED VAPOR FEED)

𝐋𝐢𝐪𝐮𝐢𝐝 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞


L+ϑ= L
Vapor 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞
V =F+V+𝜗
υ is the liquid evaporated

𝐃𝐞𝐟𝐢𝐧𝐢𝐭𝐢𝐨𝐧 𝐨𝐟 𝐪𝐮𝐚𝐢𝐥𝐢𝐭𝐲 (𝐪)


L − L H − hF
q= =
F H−h

CpV (TV − TR ) TR=Dew point


q=
λ
52
MCCABE THIELE METHOD (FEED LINE)
Feed type T* hF q f Slope
Subcooled liquid TF<Tb hF<h q>1 f<0 >1.0
Saturated liquid
L+V mixture
Saturated vapor
Superheated vapor

L − L H − hF
q= = Quality calculation
F H−h

q 1
y= x+ z Feed operating line
q−1 1−q F
53
MCCABE THIELE METHOD (FEED LINE)
Feed type T* hF q f Slope
Subcooled liquid TF<Tb hF<h q>1 f<0 >1.0
Saturated liquid TF=Tb h q=1 f=0 Infinite
L+V mixture Tb<TF<Tr h<hF<H 0<q<1 0<f<1 Negative
Saturated vapor TF=Tr H 0 1 0
Superheated vapor 0<Slope<1.
TF>Tr hF>H q<1 f>0
0

54
MCCABE THIELE METHOD (FEED LINE)

55
MCCABE THIELE METHOD (FEED LINE)
The feed line is the result of the intersection between top
section and stripping section.

(A) changing reflux ratio with constant q;


(B) changing q with fixed reflux ratio. 56
Boilup ratio varies.
EXAMPLE 4-2. FEED LINE CALCULATION

ISSUE q m

A two-phase feed where 80% of the feed is


vaporized under column conditions.
A superheated vapor feed where 1 mole of
liquid will vaporize on the feed stage for
each 9 moles of feed input.
A liquid feed subcooled by 35°F. Average
liquid heat capacity is 30 Btu/lbmol°F and λ
= 15,000 Btu/lbmol.

A mixture of ethanol and water that is 40


mol% ethanol. Feed is at 40°C. Pressure is
1.0 kg/cm2
57
COMPLETE MCCABE THIELE
Example: A distillation column with a total condenser and a
partial reboiler is separating an ethanol-acetone mixture. The
feed is 20 mol% acetone, feed rate is 1000 kmol/h, and feed
temperature is 80°F. A distillate composition of 80 mol%
acetone and a bottoms composition of 2 mol% acetone are
desired. The external reflux ratio is 5/3. The reflux is
returned as a saturated liquid and CMO can be assumed.
Find the optimum feed plate location and the total number of
equilibrium stages required. Pressure is 1 atm.

58
COMPLETE MCCABE THIELE
Variables Unknowns
1. Feed flow 100 kmol/h 1. Distillation flow
2. Feed composition 20% mol ethanol 2. Bottoms flow
3. Feed quality ¿? 3. Number of equilibrium
4. Distillation fraction 80% mol ethanol stages
5. Bottoms fractions 2% mol ethanol 4. Feed stage
6. External reflux R=5/3

ESTRATEGY

Solve Top
Solve external
section Solve feed Solve Stripping Find N and
mass Balance.
(Operating section section feed stage
(Find D and B)
Line)

59
COMPLETE MCCABE THIELE
1. Solve External mass Balance

General mass balance


F=D+B D = 230.8 kmol/h
Acetone mass balance B =769.2 kmol/h
60

zF = xD D + xB B
COMPLETE MCCABE THIELE
2. Solve Top Section
𝐀𝐜𝐞𝐭𝐨𝐧𝐞 𝐦𝐚𝐬𝐬 𝐛𝐚𝐥𝐚𝐧𝐜𝐞:
yV1 = xL1 + xD D

𝐂𝐌𝐎 𝐢𝐬 𝐯𝐚𝐥𝐢𝐝

V = V1 = V0

L = L1 = L0

𝐎𝐩𝐞𝐫𝐚𝐭𝐢𝐧𝐠 𝐋𝐢𝐧𝐞 𝐄𝐱𝐭𝐞𝐫𝐧𝐚𝐥 𝐫𝐞𝐟𝐥𝐮𝐱


yV = xL + xD D 5
L = RD = D
3
L D L xD
y = x + xD V =L+D y= x+
V V V (1 + R)
61
COMPLETE MCCABE THIELE
2. Solve Top Section
1

0,9 L xD
y= x+
V (1 + R)
0,8
𝐱𝐃
0,7
Y, acetone vapor mol fraction

0,6

0,5

0,4 𝐱𝐃
(𝟏 + 𝐑)
0,3

0,2

0,1
62
0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
x, acetone liquid mol fraction
COMPLETE MCCABE THIELE
2. Solve feed Section

Find bubble and dew temperature to compare


with the feed temperature
Dew Temperature: 166°F
Bubble Temperature: 154°F
Feed Tempeture: 80°F
Phase: Subcooled Liquid

63
COMPLETE MCCABE THIELE
2. Solve feed Section
n
kJ
λ= xi λi = 0.2 ∗ 29.1 + 0.8 ∗ 38.6 = 36.7
mol
i=1
n
J
CpL = xi CpLi = 0.2 ∗ 72.2 + 0.8 ∗ 112 = 104.4
molK
i=1

J J
36.7 + 57800 (154°F − 80°F)
q= Kmol kmol. R
J
36.7
λ + CPL (Tsat − TF ) Kmol
q= q = 1.11
λ

Operating Line

q 1
y= x+ z 64
q−1 1−q F
COMPLETE MCCABE THIELE
2. Solve Top Section
1

0,9 L xD
y= x+
V (1 + R)
0,8
𝐱𝐃
0,7
Y, acetone vapor mol fraction

0,6

0,5

0,4 𝐱𝐃
(𝟏 + 𝐑)
0,3
q 1
y= x+ z
0,2 q−1 1−q F

0,1
65
0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
x, acetone liquid mol fraction
COMPLETE MCCABE THIELE
3. Solve Bottom Section
1

0,9 L xD
y= x+
V (1 + R)
0,8
𝐱𝐃
0,7
Y, acetone vapor mol fraction

0,6

0,5

0,4 𝐱𝐃
(𝟏 + 𝐑)
0,3
q 1
y= x+ z
0,2 q−1 1−q F

0,1
66
0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
x, acetone liquid mol fraction
COMPLETE MCCABE THIELE
4. Number of stages and feed stage

67
COMPLETE MCCABE THIELE
Example 2.

We have a distillation column with a total condenser and a total


reboiler separating a feed of 200 kmol/h. The feed is 40 mol% ethanol
and water. The feed is a superheated vapor that evaporated 1 mol of
liquid per 4 mole of feed. We desire a distillate that is 80 mol% of
ethanol and a bottoms that is 5 mol% ethanol. Column Pressure is 1
atm. The boilup ratio is 2.5. Assume CMO. Find L/D, the feed stage
and the number of equilibrium stages. Draw the profiles

68
PROFILES OF BINARY DISTILLATION

69
LIMIT CONDITIONS
70 Nestor Eduardo Sanchez MSc.
Separation process and NT
Chemical Engineering
ANALYSIS OF THE LIMIT CONDITIONS
 We have a distillation column with a total condenser and a
partial reboiler separating a feed of 200 kmol/h. The feed is
40 mol% acetone and ethanol. The feed is a two phase
mixture with q=0.5. We desire a distillate that is 85 mol%
of acetone and a bottoms that is 5 mol% acetone. Column
Pressure is 1 atm. Reflux is returned as a saturated.
 Varies the L/D reflux from 0 to infinite. Analyze each case

71
ANALYSIS OF THE LIMIT CONDITIONS
(CASE 1, R<RMIN)
Feed Line

Top Line

Insufficient reflux is provided

Balance line intersect above the


equilibrium line
72

Even with a infinite number of stages, the


separation cannot be achieved
ANALYSIS OF THE LIMIT CONDITIONS
(CASE 2, R=RMIN)
Feed Line
Top Line

Separation is theoretically possible

Balance line intersects the feed line at a


point just below the equilibrium curve
73

The corresponding reflux is the Rmin,


which requires infinite number of stages
ANALYSIS OF THE LIMIT CONDITIONS
(CASE 3, R>RMIN)
Feed Line

Top Line

Separation is possible

Balance line intersects the feed line below


the equilibrium curve
74

The corresponding reflux is the a*Rmin,


which requires a finite number of stages
ANALYSIS OF THE LIMIT CONDITIONS
(CASE 4, R=INFINITE)
Feed Line

Top Line

Separation is possible, however no products or


feed enters to the column

Balance line intersects the feed line in the


45° line
75

The corresponding reflux is the total reflux,


which requires a minimum number of stages
LIMITING OPERATING CONDITIONS

Minimum Reflux
Total Reflux

76
LIMITING OPERATING CONDITIONS

77
TOTAL REFLUX
 As the reflux ratio increases, the rectifying
section operating line slope increases from L/V<1
to L/V=1.
 As the boilup ratio increases, the stripping
section operating line slope decreases from L V >
1 to L V=1.
 Both operating lines become the y=x line

 Total reflux represents the maximum separation


that can be obtained with a given number of
stages but zero throughput.
 Total reflux also gives the minimum number of
78
stages required.
TOTAL REFLUX

79
MINIMUM REFLUX

 Minimum reflux (Rmin) is defined as the external


reflux ratio at which the desired separation could
just be obtained with an infinite number of
stages.

80
MINIMUM REFLUX

Top section
L R min
=
V min 1 + R min

Stripping section
V 1
=
B L
min −1
V max

81
MINIMUM REFLUX

 Reflux minimum:
 Minimum quantity of liquid refluxed
 Minimum heat on the reboiler
 Infinite number of stages

82
MINIMUM REFLUX

Optimum reflux: 1.05 to 1.25 Rmin 83


HOMEWORK

We have a distillation column with a total condenser and a partial


reboiler separating a feed of 200 kmol/h. The feed is 40 mol%
acetone and ethanol. The feed is a two phase mixture with q=0.5.
We desire a distillate that is 85 mol% of acetone and a bottoms
that is 5 mol% acetone. Column Pressure is 1 atm. Reflux is
returned as a saturated and L/D=1.2Rmin. Assume CMO.

a. Find the optimum feed location and the number of equilibrium


stages.
b. What is the minimum number of stages?

84
HOMEWORK
acetone-ethanol
1

0,9

0,8

0,7
Y, acetone vapor mol fraction

0,6

0,5

0,4

0,3

0,2

0,1

0 85
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
x, acetone liquid mol fraction
EFFICIENCIES
86 Nestor Eduardo Sanchez MSc.
Separation process and NT
Chemical Engineering
GLOBAL AND STAGE EFFICIENCY

Global Efficiency

NEquil
Eo =
NReal

Stage Efficiency

Actual change in vapor concentration


EMV =
Change in vapor concentration for equilibrium stage

87
MURPHREE EFFICIENCY
y j  y j 1
EMV  y*j
y *j  y j 1 yj j
x j  x j 1
EML 
x*j  x j 1
j+1

xj

88
MURPHREE EFFICIENCY

• The efficiency allow to show how the


actual value is different from the
equilibrium value. Fraction of the
vertical line from the operation line.

• Those distances could generate a


pseudo-equilibrium line for each
operating line.

89
MURPHREE EFFICIENCY
 We have a distillation column with a total condenser and a
partial reboiler separating a feed of 200 kmol/h. The feed is
40 mol% acetone and ethanol. The feed is a two phase
mixture with q=0.5. We desire a distillate that is 85 mol%
of acetone and a bottoms that is 5 mol% acetone. Column
Pressure is 1 atm. Reflux is returned as a saturated and
L/D=1.2Rmin. Assume CMO. If murphree efficiency is 80%.

a. Find the optimum feed location and the number of


equilibrium stages.
b. What is the minimum number of stages?.

90
BINARY DISTILLATION: ESPECIAL
CASES
91 Nestor Eduardo Sanchez MSc.
Separation process and NT
Chemical Engineering
CASE I: OPEN STEAM HEATING
This kind of configuration is
used when the feed mixture to
separate is a water based
mixture containing a light
component

Requires less energy than


employing a reboiler

92
CASE I: OPEN STEAM HEATING

93
CASE II: COMPLEX COLUMNS
A complex fractionator is divided into
N+1 sections. The partition between each
two adjacent sections occurs either at a
feed point, or a sidedraw point or a heat
removal/addition point.

1. Multiple feeds
2. Sidedraw feeds
3. Removal/addition feeds
4. Combined problem

94
SIDE STREAMS OR WITHDRAWAL
LINES

A liquid or vapor product with


intermediate composition is required

Additional variables for the stream


must be specified

1. Flow rate
2. Type of side draw (Vapor or Liquid)
3. Stage location or composition

95
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE
1. Draw a figure of the column and label all known variables. Check to see if
CMO is valid.

2. Identify all the systems (sections) presented in the process.

3. For each section:


a. Draw a mass balance envelope. We desire this envelope to cut the
unknown liquid and vapor streams in the section and known streams
(Feed, side products, distilled, bottoms). The fewer streams involved,
the simpler the mass balance will be.
b. Write the overrall and most volatile component mass balances
c. Derive the operating equation
d. Simplify

4. Develop the feed line equation for each line.

96
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE
Case A: The reflux ratio is known or it can be calculated
(pinch point)

1. Solve the external mass balance if it is posible


2. Find the slope and the intercept of the “top line”
3. Solve the internal mass balance from the top to the
bottom (solve the operating and feed equations)
4. If external mass balance is not solved yet. Step off if the
stage location of any feed or side stream is specified (find
concentration)
5. When all operating lines have been plotted, step off
stages.
6. Find optimum feed plates location and total number of
stages.

97
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE
Case B: The boilup ration is known or it can be calculated
(pinch point)

1. Solve the external mass balance if it is posible


2. Find the slope and the intercept of the “bottom line”
3. Solve the internal mass balance from the bottom to the
top (solve the operating and feed equations)
4. If external mass balance is not solved yet. Step off if the
stage location of any feed or side stream is specified (find
concentration)
5. When all operating lines have been plotted, step off
stages.
6. Find optimum feed plates location and total number of
stages.

98
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE.

MULTIPLE FEEDS
We are separating a mixture of acetone and ethanol in a
distillation column operating at 1 atmosphere Pressure. The
column has a total condenser and a partial reboiler. The
distillate is 90 mol% acetone, and the bottoms is 10 mol%
acetone. The reflux is returned as a saturated liquid. Use a
boilup ratio V/B: 2. Two feeds are fed to the column. The first
feed has a flow rate of 75 kmol/h, it is saturated liquid, and it is
60 mol% acetone. The second feed has a flow rate of 100 kmol/h,
it is two phase mixture that is 60% vapor, and it is 40 mol%
acetone. Use the optimum feed location for each feed. Find the
total number of equilibrium stages.

99
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
1. Draw a figure of the column and label all known variables.
Check to see if CMO is valid.

100
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS

2. Identify all the systems (sections) presented in the process.

101
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
a. Draw a mass balance envelope. We desire this envelope to cut the
unknown liquid and vapor streams in the section and known streams
(Feed, side products, distilled, bottoms). The fewer streams involved, the
simpler the mass balance will be.

SOLVE THE EXTERNAL


MASS BALANCE IF IT IS
POSSIBLE

102
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
a. Draw a mass balance envelope. We desire this envelope to cut the
unknown liquid and vapor streams in the section and known streams
(Feed, side products, distilled, bottoms). The fewer streams involved, the
simpler the mass balance will be.

D= 84.4 kmol/h
B= 90.6 kmol/h

103
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
a. Draw a mass balance envelope. We desire this envelope to cut the
unknown liquid and vapor streams in the section and known streams
(Feed, side products, distilled, bottoms). The fewer streams involved, the
simpler the mass balance will be.

104
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
a. Draw a mass balance envelope. We desire this envelope to cut the
unknown liquid and vapor streams in the section and known streams
(Feed, side products, distilled, bottoms). The fewer streams involved, the
simpler the mass balance will be.

105
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
a. Draw a mass balance envelope. We desire this envelope to cut the
unknown liquid and vapor streams in the section and known streams
(Feed, side products, distilled, bottoms). The fewer streams involved, the
simpler the mass balance will be.

106
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
b. Write the overrall and most volatile component mass balances
c. Derive the operating equation
d. Simplify

Overrall mass balance V = L + D

Most volatile c.m.b yV = xL + xD D


L D
Operating equation y = x + xD
V V

107
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
b. Write the overrall and most volatile component mass balances
c. Derive the operating equation
d. Simplify

Overrall mass balance V ′ + F1 = L′ + D

Most volatile c.m.b yV ′ + z1 F1 = xL′ + xD D

Operating equation
L′ D z1 F1
y = x + xD −
V′ V′ V′
108
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 For each section:
b. Write the overrall and most volatile component mass balances
c. Derive the operating equation
d. Simplify

Overrall mass balance L′′ = V′′ + B

Most volatile c.m.b yV′′ + xB B = xL′′


L′′ B
Operating equation y= x − xB
V′′ V′′

109
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
4. Develop the feed line equation for each line.
q 1 L′′ − L′
y= x+ z q=
q−1 1−q F F

Feed 1. Feed 2.
Z1= 60 mol% acetone Z1= 40 mol% acetone
phase: Saturated Liquid phase: Liquid-vapor mixture
q=1, slope: infinity (60% is vapor)

110
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE
Case B: The boilup ration is known or it can be calculated
(pinch point)

1. Solve the external mass balance if it is posible


2. Solve the internal mass balance from the bottom to the
top (solve the operating and feed equations)
3. If external mass balance is not solved yet. Step off if the
stage location of any feed or side stream is specified (find
concentration)
4. When all operating lines have been plotted, step off
stages.
5. Find optimum feed plates location and total number of
stages.

111
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 Case B: The boilup ration is known or it can be calculated (pinch
point)
1. Solve the external mass balance if it is possible. DONE

D= 84.4 kmol/h
B= 90.6 kmol/h

112
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 Case B: The boilup ration is known or it can be calculated (pinch
point)
2. Solve the internal mass balance from the bottom to the top (solve the
operating and feed equations). Plotted your results.

L′′ B
y= x − xB
V′′ V′′

V′′
= 2.0
B
D= 84.4 kmol/h kmol
B= 90.6 kmol/h V ′′ = 2 ∗ 90.6 =181.2 kmol/h
h

kmol
L′′ = V ′′ + B = 271.8
h
113
y = 1.5x − 0.05
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
y = 1.5x − 0.05

114
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 Case B: The boilup ration is known or it can be calculated (pinch
point)
2. Solve the internal mass balance from the bottom to the top (solve the
operating and feed equations)

q 1
y= x+ z
q−1 1−q F

L′′ − L′
q= = 0.4
F2
D= 84.4 kmol/h
2 2
B= 90.6 kmol/h y=− x+
3 3

115
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
y = 1.5x − 0.05

2 2
y=− x+
3 3

116
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 Case B: The boilup ration is known or it can be calculated (pinch
point)
2. Solve the internal mass balance from the bottom to the top (solve the
operating and feed equations)

L′ D z1 F1
y = x + xD −
V′ V′ V′

𝑘𝑚𝑜𝑙
𝐿′ = 231.8
D= 84.4 kmol/h ℎ
B= 90.6 kmol/h 𝑘𝑚𝑜𝑙
𝑉 ′ = 241. 2

1
y = 0.961x + 117
8
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
y = 1.5x − 0.05

2 2
y=− x+
3 3
1
y = 0.961x +
8

118
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
 Case B: The boilup ration is known or it can be calculated (pinch
point)
2. Solve the internal mass balance from the bottom to the top (solve the
operating and feed equations)

D= 84.4 kmol/h
B= 90.6 kmol/h

119
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
y = 1.5x − 0.05

2 2
y=− x+
3 3
1
y = 0.961x +
8

120
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. MULTIPLE FEEDS
y = 1.5x − 0.05

2 2
y=− x+
3 3
1
y = 0.961x +
8

121
GENERAL MC-CABE THIELE ANALYSIS
PROCEDURE. SIDE STREAMS

A distillation column is separating methanol from water. The


column has a total condenser that subcools the reflux so that
1 mole of vapor is condensed in the column for each 3 moles
of reflux. R=3. A liquid side stream is withdrawn from the
second stage below the condenser. The side is withdrawal
rate is 350 kmol/h. The feed is saturated vapor that is 60%
mol methanol. Feed rate is F=1000 kmol/h. A total reboiler is
used, which produces a saturated vapor boilub. We desire a
distillate 94% mol metanol and 2%mol methanol. Assume
CMO. Rmin can be calculated with the feed line. Find:

a. The total number of equilbrium stages.


b. Optimal feed stage
c. The composition of the side stream.

122
INTERMEDIATE CONDENSERS AND
REBOILERS
 Intermediate reboilers removes a liquid side stream,
vaporizes it, and reinjects it into the column,
 Intermediate condenser removes a vapor side stream,
condenses it, and reinjects it into the column.
 Optimum use of energy resources
 Intermediate condenser is operated in the top section
 Intermediate reboiler is operated in the stripping
section
 Increases the efficiency of the trays by reducing the
amount of “lost work”
 During normal operation, they should cause no
problems.
 Starup may be difficult.
 The use of an intermediate condenser or reboiler 123
gives us four operating lines in the column.
INTERMEDIATE CONDENSERS AND
REBOILERS

124
INTERMEDIATE CONDENSERS AND
REBOILERS
 A distillation column is separating methanol from
water. The column has a total condenser. A vapor
side stream is withdrawn from the first stage above
the reboiler. This side stream is condensed and
returned in the optimal feed stage. The side is
withdrawal rate is 150 kmol/h. The feed is saturated
liquid that is 20% mol methanol. Feed rate is F=1000
kmol/h. A partial reboiler is used, which produces a
saturated vapor boilub. The boilup ratio is 0.8. We
desire a distillate 90% mol metanol and 2%mol
methanol. Assume CMO.

a. The total number of equilbrium stages.


b. Optimal feed stage for both feed stream 125
CASE III: CONDENSERS REFLUX

Total Condenser Partial Condenser


Distilled Liquid (xD) Vapor (yD)
Equilibrium stage NO YES
Reflux type Saturated Liquid Saturated Liquid
126
Subcooled Liquid
CASE III: CONDENSERS REFLUX
Saturated liquid reflux Subcooled liquid reflux

L1 xD D
y= x+
V2 V2

L1 xD D
y= x+
V V

L1 = 𝐿𝑜 + 𝑐 Liquid mass balance

V2 = 𝑉1 + 𝑐 Vapor mass balance


CMO is valid for the vapor,
then V1 = V2 = V L1 1 + fc R
=
V2 1 + 1 + fc R
CMO is valid for the liquid,
then L1 = Lo = L Fc=fraction condensed
127
CpL (TB − TR )
fc =
λ
CASE III: CONDENSERS REFLUX
 We are separating metanol and water. Calculate
the internal reflux ratio inside the column L1/V2
for the following cases:
a) Distillate product is 100% mol methanol.
External reflux is R=1.2. Reflux is cooled to 40
°C. (L1/V2=0.56)
b) Repeat part a except for a saturated liquid
reflux. (L1/V2=0.54)

128
CASE IV: REBOILERS

Total Reboiler Partial Reboiler


Total reboiler Partial reboiler
Bottoms Liquid (xB) Liquid (xB)
Equilibrium stage NO YES
129
Boilup type Saturated Vapor Saturated Vapor
Superheated
CASE V: STRIPPING AND ENRICHING
COLUMNS

130