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Phase separation Phase separation Phase separation Phase separation

(Ref: GPSA Eng Data Book; Biegler et al., 1997)


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Lecture outline Lecture outline Lecture outline Lecture outline
The Onion model
Common phase separation
processes
Uses of gas/liquid separators
Separation principles
Separator design & sizing
Linear mass balance for flash unit
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The The The The Onion diagram Onion diagram Onion diagram Onion diagram
Reactor
Separation &
recycle
Heat exchange
network
Utilities
(Linnhoff et al., 1982,
Smith, 1995, 2005)
Leave it until H83RED
(Reactor Design)
Current focus
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Introduction Introduction Introduction Introduction
The lecture handout (extracted from Gas Processors
Supplier Association GPSA Engineering Data Book) is a
courtesy of Dr Murugan Selvan, WinSimInc., Texas US.
5 types of phase separation problems:
Liquid droplets from vapour/gas (our focus)
Liquid droplets from immiscible liquid
Solid particles from gas/vapour
Solid particles from liquid
Solid particles from other solid particles
Some common denominations:
Flash tank: gas/liquid separation based on P
Knockout drum: to remove liquid droplets from gas
Liquid-liquid separator: 2 immiscible liquid phases
Three phase separator: removal of gas from 2 immiscible liquids
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 5
Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators
After partial condenser on distillation column overheads
Serve 2 purposes:
Vapour/liquid separation
Liquid hold-up for reflux purpose
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Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators
Product recovery via condensation
Effluent from reactor has 2 phases
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Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators
Refrigeration loop
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Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators Uses of gas/liquid separators
To protect high speed machinery e.g. compressors
Drum 1 protects machine from upstream operations (often known as
dry drum)
Drum 2 & 3 are needed to prevent any liquid that may formed due to
inter-cooling.
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 9
Separator design & parts Separator design & parts Separator design & parts Separator design & parts
3 types of separator designs:
Vertical
Horizontal
Spherical
4 important parts of a separator:
Primary separation section - to separate the
main portion of free liquid in the inlet
stream.
Gravity section designed to utilise gravity
force to enhance separation of entrained
droplets.
Coalescing section utilises coalescer / mist
extractor to remove the very small droplets
of liquid from the gas by impingement on a
surface where they coalesce.
Liquid collection section acts as receiver
for all liquid removed from the gas
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 10
Factor for selection of separator Factor for selection of separator Factor for selection of separator Factor for selection of separator
configuration configuration configuration configuration
How well will extraneous material (e.g. sand, mud,
corrosion products) be handled?
How much plot space will be required?
Will the separator be too tall for transport if skidded?
Is there enough interface surface for 3-phase separation
(e.g. gas/hydrocarbon/glycol liquid)?
Can heating coils or sand jets be incorporated if required?
How much surface area is available for degassing of
separated liquid?
Must surges in liquid flow be handled without large
changes in level?
Is large liquid retention volume necessary?
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 11
Particle characteristic Particle characteristic Particle characteristic Particle characteristic
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 12
Vertical separator Vertical separator Vertical separator Vertical separator
Selected when:
gas-liquid ratio is high; or
total gas volumes are low
Level control is not critical &
liquid level can fluctuate
several inches without
affecting operating efficiency.
Mist extractors significantly
reduce the required diameter
Occupies a small amount of
plot space
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 13
Horizontal separator Horizontal separator Horizontal separator Horizontal separator
Most efficient when:
large volumes of total fluids
large amounts of dissolved gas are present with the liquid.
Large liquid surge volume leading to longer retention time
More surface area per liquid volume better degassing
Handle a foaming liquid better than a vertical.
The liquid level responds slowly to liquid inventory
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 14
Spherical separator Spherical separator Spherical separator Spherical separator
High
pressure
service
Compact
size is
desired
Liquid
volumes
are small
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 15
Principles of separation Principles of separation Principles of separation Principles of separation
3 principles used to achieve physical separation:
Gravity settling Liquid droplets settle out from
gas phase when gravitational force > drag force of
gas flowing around the droplet
Momentum:
Separation occurs when a 2 phases (of different
densities) stream changes direction sharply, greater
momentum prevent the heavier particles to turn as
rapidly as the lighter fluid
Employed for 2 phases bulk separation
Coalescing:
Very small droplets (fog or mist) cannot be separated by gravity coalesced
to form larger droplets that will settle by gravity.
Coalescing devices force gas to follow a tortuous path. The momentum forces
the droplets to collide & form larger droplets settle out by gravity.
Examples: wire mesh screens, vane elements, and filter cartridges
Any separator may employ 1 or > principles, but fluid phases must be
immiscible & of different densities.
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 16
Design of separator without mist Design of separator without mist Design of separator without mist Design of separator without mist
extractors extractors extractors extractors
To design a separator without a mist extractor, the
minimum diameter droplet to be removed must be set
typically in the range of 150 - 2,000 microns.
Gravity settling is utilised as the sole mechanism for
separating the liquid and gas phases.
Calculation of vessel length:
Assumption: the time for the gas to flow from inlet to outlet = time
for the liquid droplet of size D
p
to fall from the top of the vessel
liquid surface.
Then relate the length (L) of the separator to its diameter (D
v
) as a
function of this settling velocity (V
t
):
Ratio of L/D
v
is in the range of 2:1 4:1
v t
A
4
D V
Q
L

=
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 17
Gravity settling Gravity settling Gravity settling Gravity settling
Forces acting on the particle can be described
mathematically using the terminal or free settling velocity:
Combining:
Drag coefficient C is a function of:
Particle shape (considered as solid & rigid sphere)
Reynolds number, given as:
( )
C A
gM
V
t

=
p g l
g l p
2

g t p
1488
Re
V D
=
2
p
p
3
p
p
l
p
2
and
2 3
4

= =
D
A
D
V
m

( )
C
gD
V

=
g
g l p
t
3
4


Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 18
C CC C of Rigid Spheres of Rigid Spheres of Rigid Spheres of Rigid Spheres
( )
2
g l
3
p g
8
2
10 x 95 . 0
(Re)


=
D
C
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 19
Gravity settling Gravity settling Gravity settling Gravity settling limited case limited case limited case limited case
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 20
Example 1 Example 1 Example 1 Example 1 - -- - Separator design Separator design Separator design Separator design
(without mist extractors) (without mist extractors) (without mist extractors) (without mist extractors)
A horizontal gravity separator (without mist
extractor) is required to remove all entrainment
with D
p
> 150 microns from a 60 million standard
cubic feet per day (MMscfd) of gas.
Gas property:
MW = 21.72
Pressure = 500 psig
Temperature = 100F
Viscosity = 0.012 cp
Ideal gas compressibility (Z) = 0.9
Liquid specific gravity = 0.50
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 21
Example 1 Example 1 Example 1 Example 1 Solution Solution Solution Solution

H2O
(American unit)
1 ft = 12 in
lb-mole 379 ft
3
3600 s 24 hr day
21.72 lb 1 lb-mole 1 hr 1 day 60 x 10
6
ft
3
1 micron = 0.00003937 in
100 + 460R
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 22
Example 1 Example 1 Example 1 Example 1 Solution Solution Solution Solution
( )
2
g l
3
p g
8
2
10 x 95 . 0
(Re)


=
D
C
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 23
Example 1 Example 1 Example 1 Example 1 Solution Solution Solution Solution
L
D
v
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 24
Example 1 Example 1 Example 1 Example 1 Solution Solution Solution Solution
Vessels up through 24 in. diameter have nominal pipe dimensions
Larger vessels are rolled from plate with 6 in. internal increments in diameter.
Seider et al. (2003)
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 25
Example 2 Example 2 Example 2 Example 2 - -- - Separator design Separator design Separator design Separator design
(without mist extractors) (without mist extractors) (without mist extractors) (without mist extractors)
What size vertical separator
without mist extractor is
required to meet the conditions
used in Example 1?
Solution:
Area:
Diameter:
Hence, ID of 90 in is needed
2
t
A
ft 7 . 41
46 . 0
2 . 19
= = =
V
Q
A
in 87 ft 9 2 . 7
4
4
2
= = =

A
D
D
A
D
v
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 26
Separator with mist extractor Separator with mist extractor Separator with mist extractor Separator with mist extractor
Wire mesh pads are frequently used as entrainment separators for the removal
of very small liquid droplets (< 10 microns) higher overall percentage
removal of liquid.
The pressure drop across a wire mesh pad is negligible. The effect of the P
becomes significant only in the design of vacuum services & for equipment
where the prime mover is a blower or a fan
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 27
Separator with mist extractor Separator with mist extractor Separator with mist extractor Separator with mist extractor
Wire mesh pads can be used in horizontal vessels.
The orientation of the mesh pad is preferred in the horizontal plane.
Less efficient in vertical orientation
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 28
Design of separator (with mist Design of separator (with mist Design of separator (with mist Design of separator (with mist
extractors) extractors) extractors) extractors)
Vertical separator with mist
extractors:
Critical velocity equation:
Souders & Brown correlation:
Horizontal separator > 10 ft with
mist extractors:
Critical velocity equation:
Souders & Brown correlation:
Ratio of L/D
v
is in the range of
2:1 4:1
56 . 0
g
g l
10

=
L
K V
t


g
g l


= K V
t
( )
56 . 0
10
g l g m

=
L
C G
( )
g l g m
= C G
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 29
Example 3 Example 3 Example 3 Example 3 - -- - Separator design Separator design Separator design Separator design
(with mist extractors) (with mist extractors) (with mist extractors) (with mist extractors)
What size vertical separator
equipped with a wire mesh mist
extractor is required for the
conditions used in Example 1?
Solution:
K = 0.28 ft/s
Critical velocity:
Area:
Diameter:
Hence, ID of 60 in is needed
ft/s 05 . 1
07 . 2
07 . 2 2 . 31
28 . 0
t
=

= V
2
t
A
ft 3 . 18
05 . 1
2 . 19
= = =
V
Q
A
in 8 5 ft 8 . 4
4
4
v
2
v
= = =

A
D
D
A
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 30
Separator with vane type mist Separator with vane type mist Separator with vane type mist Separator with vane type mist
extractors extractors extractors extractors
When fouling or hydrate formation is
possible/expected, mesh pads are not used
vane or centrifugal type separators are
more appropriate.
Vane type separator designs are proprietary
& not easily designed with standard
equations consult manufacturers.
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 31
Separators with centrifugal Separators with centrifugal Separators with centrifugal Separators with centrifugal
elements elements elements elements
Advantage of a centrifugal separator
over a filter separator: much less
maintenance
Disadvantages of centrifugal
separators:
Some designs do not handle slugs
well
Efficiency is not as good as other
types of separators
P tends to be higher than vane
or clean knitted mesh mist
extractors
Narrow operating flow range
for highest efficiency
Designs are proprietary consult
manufacturers
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 32
Filter separator Filter separator Filter separator Filter separator
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 33
Filter separator design Filter separator design Filter separator design Filter separator design
Higher separation efficiency than the centrifugal separator,
but it uses filter elements, which must periodically be
replaced.
The approximate filter surface area for gas filters can be
estimated from based on applications such as molecular
sieve dehydrator outlet gas filters. For dirty gas service the
estimated area should be increased by a factor of 2 or 3.
Removal efficiency:
Most dry solid particles 10 microns are removable
Particles of < 10 microns: ~99%
For heavy liquid loads, or where free liquids are contained in the
inlet stream, a horizontal filter separator with a liquid sump, which
collects and dumps the inlet free-liquids separately from coalesced
liquids, is preferred.
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 34
Filter separator design Filter separator design Filter separator design Filter separator design
Pressure drop:
Efficiency depends on the proper design of the filter pack, i.e., a
minimum P while retaining an acceptable extraction efficiency.
P ~ 1-2 psi is normal in a clean filter separator.
If excessive solid particles are present, it may be necessary to clean
or replace the filters at regular intervals when a P > 10 psi is
observed.
Rule of thumb to change filters: maximum P of 25 psi, otherwise
cartridge units might collapse.
Removal of the filter pack is easily achieved by using a
quick-opening closure.
Critical velocity equation:
g
g l
t
3 . 1


= V
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 35
Approximate gas filter capacity Approximate gas filter capacity Approximate gas filter capacity Approximate gas filter capacity
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 36
Example 4 Example 4 Example 4 Example 4 Filter separator Filter separator Filter separator Filter separator
A filter separator is required to handle a flow of 60 MMscfd
at conditions presented in Example 1. Estimate the diameter
of a filter separator.
Solution:
Critical velocity equation:
Area:
Diameter:
Hence, ID of 30 in is needed
ft/s 88 . 4
07 . 2
07 . 2 2 . 31
3 . 1
t
=

= V
2
t
A
ft 93 . 3
88 . 4
2 . 19
= = =
V
Q
A
in 26.9 ft 2 . 2
4
4
v
2
v
= = =

A
D
D
A
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 37
Linear mass balance (MB) Linear mass balance (MB) Linear mass balance (MB) Linear mass balance (MB)
A flowsheet has many non-linear equations
describing:
Connectivity of units through process streams
Equations for each unit, e.g. internal M/E balances,
equilibrium relationships
Physical properties, e.g. enthalpy, equilibrium constant,
thermo properties, etc.
It will be useful (e.g. manual calculation during
preliminary process design) to linearise these
equations subject to the following approximations:
Ideal solution in all calculations
Most streams are available as saturated vapour/liquid
(valid for equilibrium staged operations)
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 38
Linear MB for flash unit Linear MB for flash unit Linear MB for flash unit Linear MB for flash unit
Most fundamental & important in a flowsheet building
block for equilibrium staged operations, e.g. distillation,
absorption.
Consider a flash model to separate n
comp
components, the
overhead split fraction (recovery) of component k (
k
) is
given as:
V, y
k
v
k
= V y
k
L, x
k
l
k
= L x
k
F, z
k
f
k
= F z
k
k
k
k
f
v
=
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 39
VLE approximations VLE approximations VLE approximations VLE approximations
Approximation for VLE:
Antoine equation for vapour pressure:
Raoults law: y
k
P = x
k
P
o
k
, or defined as K-value as:
With respect to key component n, relative volatility of component
k is defined as:
Rearrange the approximations give the relation between
recovery of component k in terms of key component n:
k
k
k k
C T
B
A P
+
=
o
ln
k
k
k
k
K
P
P
x
y
= =
o
o
o
n
k
n
k
P
P
K
K
n
k
= =
( )
n
n
k
n
k
n
k

1 1 +
=
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 40
VLE approximations VLE approximations VLE approximations VLE approximations
At bubble point (saturated liquid effluent stream):

i
y
i
=
i
K
i
x
i
= 1
Given the average relative volatility =
i

i/n
x
i
,
K-value is redefined as a simplified bubble point
equation:
For T fixed & P unknown, P can be calculated from:
For P fixed & T unknown, T can be calculated from:
a
~
o
n
k
P
P
K
k
k

= =
) (
a
~
o
T P P
k
n
k

=
P T P
n
k
k
a
~
) (
o

=
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 41
Calculation steps for fixed T , P Calculation steps for fixed T , P Calculation steps for fixed T , P Calculation steps for fixed T , P
1. Pick a key component n and guess
n
2. Calculate K
k
,
k/n
@ specified T
3. Evaluate
k
for each component k by:
4. Reconstruct mass balance & calculate mole
fractions:
v
k
=
k
f
k
= y
k

k
v
k
l
k
= (1
k
) f
k
= x
k

k
l
k
5. If the bubble point equation is satisfied, calculation
is stop. Otherwise, re-guess
n
and go to Step 3.
( )
n
n
k
n
k
n
k

1 1 +
=
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 42
Example 5 Example 5 Example 5 Example 5 Flash calculation Flash calculation Flash calculation Flash calculation
Calculate the flowrate and mole fractions of the top &
bottom product streams of a flash drum that operated @ 1
bar & 390K.
Component flowrates of the feed stream, as well as their
boiling points (BP) & Antoine coefficients are given in the
table.
59.44 3395.57 16.1156 418 40 O-xylene (X)
53.67 3096.52 16.0137 383 50 Toluene (T)
52.34 2788.51 15.9008 353 30 Benzene (B)
C
k
B
k
A
k
BP (K) f
k
(kmol/h) Comp, k
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 43
Example 5 Example 5 Example 5 Example 5 Solution Solution Solution Solution
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 44
Example 5 Example 5 Example 5 Example 5 Solution Solution Solution Solution
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 45
Steps for Steps for Steps for Steps for
k kk k
& fixed T (or P) & fixed T (or P) & fixed T (or P) & fixed T (or P)
1. Guess T (or P)
2. Follow Steps 2 for fixed T & P case
3. Follow Steps 3 for fixed T & P case
4. Follow Steps 4 for fixed T & P case
5. 2 cases:
For T fixed:
For P fixed, solve for T from
P T P
n
k
k
a
~
) (
o

=
) (
a
~
o
T P P
k
n
k

=
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 46
Problem for revision 1 Problem for revision 1 Problem for revision 1 Problem for revision 1
Feed to a flash tank consists of 25 moles pentane, 40
moles cis-2-butene & 35 moles n-butane.
Find the recovery of n-butane @ P = 200 kPa & T = 300K
If the flash tank operates @ 100 kPa, at what
temperature could you recover 60% cis-2-butene in the
vapour?
Remark: Make your own effort to obtain Antoine
coefficients!
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 47
Problem for revision 2 Problem for revision 2 Problem for revision 2 Problem for revision 2
A flash vessel is used to separate a mixture that consists of
propane, n-pentane and n-hexane. Component flowrates
and Antoine coefficients are shown in the following table.
Tasks:
Find the components mole flowrates and fractions in the overhead
stream when the flash vessel is operated at 5 atm and 90C (1 atm
= 760 mmHg).
If the flash tank operates @ 8 atm, at what temperature could you
recover 60% n-pentane in the vapour?
(Final exam 2007, Q5)
224.210 1168.720 6.870 50 n-Hexane (C
6
H
14
)
233.205 1075.78 6.876 30 n-Pentane (C
5
H
12
)
246.990 803.810 6.804 20 Propane (C
3
H
8
)
C B A (kmol/h)
Antoine coefficients Flowrate Component
Copyright@Dominic Foo H82PLD - Plant Design Phase Sep - 48
Problem for revision 3 Problem for revision 3 Problem for revision 3 Problem for revision 3
A flash vessel is used to separate a mixture that consists of ethane,
propane, butane, n-pentane and n-hexane. Component flowrates and
Antoine coefficients are shown in the following table.
Tasks:
Find the components molar flowrates and fractions in the overhead stream
when the flash vessel is operated at 7 atm and 363K (1 atm = 760 mmHg).
If the flash tank operates at 358K, at what pressure could we recover 60%
of n-butane in the vapour stream?
(Final exam 2008, Q1)
-48.80 1171.17 6.8760 20 n-Hexane (C
6
H
14
)
-40.19 1064.84 6.8529 30 n-Pentane (C
5
H
12
)
-34.42 935.86 6.8089 20 n-Butane (C
4
H
10
)
-26.16 804.00 6.8034 20 Propane (C
3
H
8
)
-16.42 663.72 6.8291 10 Ethane (C
2
H
6
)
C
k
B
k
A
k
(kmol/h)
Antoine coefficients Flowrate Component k

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