Separation equipment—

design and costs

• Chapter 15
• Max Peters, Klaus Timmerhaus, Ronald West, Plant
Design and Economics for Chemical Engineers Fifth
Edition,McGraw-Hill, 2002
Use of Separation Units
Separation
Reaction
Hydrodealkylation
of Toluene

T+H2→B+CH4
side reaction
2B→
Biphenyl+H2

• Reactor Effluent
• T=1,350F
• P = 500 psia
 Reactor Effluent
Reaction Conditions
T=1,350F
P = 500 psia Component kmole/hr
Hydrogen 1292
Methane 1167
Benzene 280
Toluene 117
Biphenyl 3
Total 2859
After Flash to 100F @ 500 psia
Effluent Vapor Liquid
Component kmole/hr kmole/hr kmole/hr
Hydrogen 1292 1290 2
Methane 1167 1149 18
Benzene 280 16 264
Toluene 117 2 115
Biphenyl 3 0 3
Total 2859 2457 402

Recycled Reactants
 Separation

• Vapor Separation
– CH4 from H2
• Liquid Separation
 Further Separation
What separation units should be used?

Liquid Separation Gas Separation

• Toluene, BP=110.6ºC • Hydrogen

• Benzene, BP=80.1ºC • Methane
• What happens to the • what happens to the
Methane (BP= - Toluene and Benzene
161.5ºC) and impurities?
Biphenyl
(BP=255.9ºC)
impurities?
 Criteria for the Selection of a
Separation Method
• Energy Separation • Mass Separation
Agent (ESA) Agent (MSA)
– Phase condition of feed – Phase condition of feed
– Separation Factor – Choice of MSA
– Cost Additive
I – Separation Factor
C 1 – Regeneration of MSA
I
C – Cost
SF = 2
C1II Phases I and II,
II
C 2 Components 1 and 2 (light key and heavy key)
9
10
 Direct
Distillation
Sequence
Distillation
14
 Distillation
• Relative Volatility α=KL/KH

• Equilibrium Line
 Distillation
• Rectifying Section
– R= reflux ratio
– V=vapor flow rate
• Stripping Section
– VB= Boil-up ratio

• Feed Line
SEPARATION BY DISTILLATION

• There are two basic approaches used in distillation column design, namely,
1. Design
2. Rating.
• The former approach involves the design of a new column to determine the
column diameter and height required to achieve a specified separation.
• This approach utilizes stage-to-stage calculations for determining the number of
equilibrium stages.
• The rating approach involves the retrofit of an existing column in which the
column diameter and height are fixed and the flow capacity and separation are to
be determined.
• Since the rating approach has convergence advantages, it is most often used in
computer algorithms which do stage-to-stage calculations.
Types of Columns
Types of Columns
 Plate Types
• Bubble Cap Tray • Sieve Tray
Plate Types

Bubble Sieve Valve

 Packed Towers
• Random Packing

• Structured Packing

Note: Importance of
Distributor plate
24
25
Tray Efficiency = 60 to 85 %

26
 COLUMN DESIGN: EIGHT
PRACTICAL STEPS
Define Define product specification(s)
Choose Choose an operating pressure
Choose Choose appropriate VLE data
Calculate Calculate the number of theoretical trays
Select Select a tray efficiency
Select Select appropriate tower internals
Perform Perform tower sizing and tray hydraulics
Select Select a process control scheme
 STEP 1: DEFINE
PRODUCT
SPECIFICATION(S)
• Select light key and heavy key
components There are three ways of
specifying a desired product A
percentage recovery of a feed
component in the overhead or bottom
streams
• A composition of one component in
either product
• A specific physical property, such as
vapor pressure, for either product
 STEP 2: CHOOSE AN
OPERATING
PRESSURE

• Operating pressure impacts all aspects

of column design
• Some considerations, as pressure
increases…
1. relative volatility mostly decreases,
making separation more difficult
2. the minimum number of stages
increases
3. required exchanger sizes may
decrease
4. The column may get mechanically
more costly
STEP 2: CHOOSE AN OPERATING PRESSURE
 STEP 3: CHOOSE VLE AND ENTHALPY
DATA

• Choose correct VLE and

enthalpy data ranges for
property calculations
• Choose correct methods for
calculating properties
• Inappropriate methods,
models or data ranges can
lead to poor results
• Close boiling systems are
especially finicky to
converge
• Watch for non-ideality!
 STEP 4: NUMBER OF
THEORETICAL TRAYS
• Calculate the minimum number of
theoretical trays with the Fenske
equation
• For a better tray count estimate,
assume a reflux ratio and run cases
in a simulator
• In Aspen Plus, use DISTWU model
• In HYSYS, use Shortcut Column
model
• All column design work is typically
done with theoretical trays
STEP 5: TRAY EFFICIENCY TYPICAL VALUES
 • Efficiency estimates in
established processes are trouble-
free with conventional internals
STEP 5: TRAY • With “high capacity” internals,
EFFICIENCY be conservative with efficiency
LESSONS • With first-of-a-kind systems, be
LEARNED conservative with efficiency
• There is always a learning curve
with new “improved” internals --
- be cautious
STEP 6: SELECT TOWER
INTERNALS
Tray Column Design
Symbols Characteristic dimensions
of industrial tray designs

a downcomer
b tray support
c sieve trays
d man way
e outlet weir
f inlet weir
g side wall of
downcomer
h liquid seal

Aac active area

Ad downcomer area
Dc column diameter
dcap, v, h bubble cup, valve,
hole diameter
H, z tray spacing
hcl height of down-
comer clearance
hw weir height
lw weir length
lL length of liquid
flow path
 relative free area

Sources: A. Mersmann, M. Kind, J. Stichlmair: Thermal Separation Technology. Berlin,

Heidelberg: Springer 2011; D.W. Green (ed.): Perry´s Chemical Engineers´
Handbook, New York: McGraw-Hill 2008
 Tower with Structured-Packed
Tower with Structured Packing Top Bed and Random-Packed
Bottom Bed
Symbols

a liquid distributor
b liquid collector
c structured packing
d support grid
e man way
f liquid re-distributor

Sources: A. Mersmann, M. Kind, J. Stichlmair: Thermal Separation Technology. Berlin,

Heidelberg: Springer 2011; D.W. Green (ed.): Perry´s Chemical Engineers´
Handbook, New York: McGraw-Hill 2008
 Examples of Distillation Column Internals

Sieve Tray

Tunnel Cap Tray

Bubble Cap Tray

Structured Packing
Source: GEA Wiegand GmbH, Ettlingen
 Examples of Distillation Column Internals

Detail of Varioflex valve tray

Source: Koch-Glitsch, Inc.

Floating valve tray with rectangular-shaped valves

(BDH™ valve)

Source: Sulzer Chemtech AG

• Common random
packing particles
• Made of metal, plastic,
ceramic

• Source: Koch-Glitsch,
Inc.
Examples of Distillation Column Internals
Historical Development of Characteristic Random Packings
First Generation (Raschig Ring, Berl Saddle)
Third Generation (Net/Grid Structures, IMPT Ring)
1895 to the 1950s
late 1970s to the 1990s
simple shapes with closed surfaces, robust
framework structure, large free cross section,
and stable design, cost-effective production
low pressure drop, high efficiency

Second Generation (Pall Ring, Intalox Saddle) Fourth Generation (Raschig Super-Ring)
late 1950s to the early 1970s late 1990s until present
surfaces with cutted windows and bent tongues, lower pressure drop and better mass transfer
improved area distribution lowering pressure efficiency
drop and enhancing capacity
 Common Types of Structured Packings

Structured packing of corrugated metal

sheets

Fitting structured packing elements Flexipac to a large-diameter tower

Structured packings Mellapak Sources: Sulzer Chemtech AG; Koch-Glitsch, Inc.

made of metal and plastic
 Overall View of a Distillation Unit
Condenser

Cooling Water

Distillate Cooling Water

Feed Distillate
Distillate
Cooler
Distillate
Pump
Steam
Reboiler

Pump Feed

Feed Preheater
Bottom Product
Bottom Product
Cooler
Cooling Water
Source: GVWU mbH, Norderstedt
 Piping and Instrumentation Diagramm of a Distillation Unit

Source: Baerns, M. et al.: Technische Chemie. Weinheim: WILEY-VCH 2006

45
46
47
48
Tray Efficiency = 60 to 85 %

49
50
51
52
53
54
55
56
57
58
Separation Processes

59
Separation Processes
61
Separation Processes

62
Separation Processes

63
Separation Processes

64
Separation Processes

65
Separation Processes

66
Separation Processes

67
Separation Processes

68
 Iterative Tray Design

• Step #1: Determine the number of theoretical plate and vapor and
liquid flow-rates separately both in top and bottom sections.
• Step #2: Obtain the physical properties of the system
• Step #3: Select a trial plate spacing
• Step #4: Estimate the column diameter based on flooding
considerations
• Step #5: Decide the liquid flow arrangement (reverse, single-pass, or
multiple-pass).
• Step #6: Make a provisional tray layout including downcomer area,
active area, perforated area, hole area and size, weir height, weir length
• Step #7: Check the weeping rate, if not satisfactory go back to step #6
and reselect tray layout
 Iterative Tray Design

• Step #8: Check the plate pressure drop, if too high return to step #6
• Step #9: Check downcomer back-up, if too high go back to step #6 or
#3
• Step #10: Decide plate layout including calming zones and
unperforated areas and check hole pitch, if unsatisfactory return to step
#6
• Step #11: Recalculate the percentage of flooding based upon selected
tower diameter
• Step #12: Check for entrainment, if too high then return to step #4
• Step #13: Optimize design: repeat steps #3 to #9 to find smallest
diameter and plate spacing acceptable to get the lowest cost for the
specified application
• Step #14: Finalize design: draw up the plate specification and sketch
the layout
 Problem 1

• A distillation column is to separate 4750 mol/h of feed composed of

37% n-butane, 32%. iso-pentane, 21% n-pentane and 10% nhexane.
• The column operates at an average pressure of 2 atm a and will
produce distillate product containing 95% n-butane and 5% iso-pentane.
• The bottom product is allowed to contain no more than 570 mol/h of
n-butane.
• Use Underwood’s method to determine the minimum reflux for the
required separation.
• Feed is 25% (by mole) vapour.
• Assume ideal vapour–liquid equilibrium. All compositions are mole
%.
 Problem 2

• A valve tray tower has been designed to separate a mixture of 60 mol

percent benzene and 40 mol percent toluene into an overhead product
containing 96 mol percent benzene and a bottom product containing 25
mol percent benzene. Calculations have shown that 6.1 theoretical
stages will be required to obtain the desired separation conducted
essentially at atmospheric pressure. The temperature at the top of the
column is 82.8oC while at the bottom of the column it is 100.5oC.
Assuming the reboiler acts as one theoretical stage, estimate the
number of actual trays required. To simplify the calculation, assume that
mixtures of benzene and toluene may be considered as ideal. At an
average temperature of 91.6oC. the vapor pressure of pure benzene is
1070 mmHg. and the vapor pressure of pure toluene is 429 mmHg.
 Problem 3

• Design a continuous distillation column (plate) to recover acetone

from a 50-50 mole % acetone-water mixture available at 30°C.
• The feed stream flow rate is 25,000 kg/h.
• The top product should contain at least 95 mole% acetone and the
bottom product should contain <1 % acetone by mole.
• Consider reboiler as equivalent to one stage.
• This column is operated at atmospheric pressure (top tray).
• Column efficiency of 60% and pressure drop per plate of 1.25 kPa
may be assumed.
• You can take the minimum liquid flow as 70% of the maximum rate
both above and below the feed plate.
• The vapor liquid equilibrium (VLE) data for the acetone-water system
at atmospheric pressure is provided in Table.
 Data
Latent heat of water= 41,360 J/mol;
Latent heat of acetone= 28,410 J/mol
Specific heat of water=75.3 J/mol°C (mean);
Specific heat of acetone 128 J/mol°C (mean)