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3.4
3.4.1
Introduction
Removing liquids and solids from a gas stream is very important in refining
and gas processing applications. Effective removal of these contaminants can
prevent
costly
problems
and
downtime
with
downstream
equipment
like
entrainment of any liquid droplets in the vapor as it exits the top of the vessel. The
figure bellow shows the simple illustration of vapor-liquid separator.
3-2
During the production of phthalic anhydride, vapor-liquid separator is used to
separate liquid and vapor from the mixture because only liquid form of phthalic
anhydride is needed for the production. There are mainly two types of separator that
can be used which is the vertical separator and the horizontal separator.
3-3
production. When large quantity of loads, horizontal separator is applied because
the separator consequently hold up will set the size of production. Horizontal flash
separator also comes best when three phases are involved in the production.
A complete separator must have the following (Perry. H., et al., Chemical
Engrs. Handbook, 4th Ed., McGraw-Hill, New York (1963):
1. A primary separation section to remove the bulk of the liquid from the gas.
2. Sufficient liquid capacity to handle surges of liquid and to adequately degas
the liquid.
3. Sufficient diameter and length (height) to allow the small droplets to settle out
by gravity (to prevent undue entrainment).
4. A means of reducing turbulence in the main body of the separator so that
proper settling may take place.
5. A mist extractor to capture entrained droplets and those too small to settle by
gravity.
6. An inlet device to absorb the momentum (kinetic energy) of the entering
fluids.
7. Vortex breaker on liquid outer nozzle(s).
8. A method of solids removal, e.g. sand jets.
9. Manways or hand-holes to access the vessels for inspection and cleaning.
10. Proper pressure and level controls, alarms and shutdowns.
3.4.2
Process Description
In order to get the better and higher percent of product in liquid form which is
Phthalic Anhydride, two-phase separator is used after the reaction occur in the
reactor. Calculations need to be done in order to determine the sizing of the stream
that will enter the separator and flow out to the bottom or top outlet of the separator.
According to our production plant, the separation includes two phases which are
heavy liquid and vapour. The separator operates only at the low pressure and
temperature at 150 kPa and 53 C. The figure shows the separator that we used in
our production.
3-4
3.4.3
3-5
In choosing the type of reactors, it depends on the production of the plant. There two
kinds of separators which are usually used in industry which are the two phase
separator and a 3 phase separator. A simple way to describe a two phase separator
is it was used to separate a mixture of components which exist in two phase. In the
design of separator, a two phase separator is chosen since the production involves
two phase of compound which is the vapor and liquid. In two phase separator it is
needed to determine which orientation is the best which will provide a higher
separation efficiency. There are three orientation involved which is vertical,
horizontal and spherical separator. Spherical design can withstand a high
temperature and pressure. From the operating temperature and pressure of
separator, the design of spherical can be neglected since the separator operates at
a lower temperature and pressure. Thus, the focus is on horizontal and vertical
separator. In order to obtain a higher amount of production of phthalic anhydride
several criteria and consideration need to be followed:
1. Availability of plot area
2. Economics
3. Special Consideration
Then, all the factors should be check first before choosing type of separator
that is suitable for our production. According to W.D Monnery, the orientation of the
vessel depends on its vapor to liquid ratio. If the ratio of vapor is much larger it can
be said that the vessels are vertical in orientation.
Table 3.4.1: Advantages of vertical and horizontal separator
Vertical
Generally
used
in
gas
dominated
Horizontal
Generally used in liquid dominated
Smaller footprint.
of liquid level
Level vs. liquid inventory relationship is
Less headroom
linear
3-6
The information and the data that were needed in order to obtain the gas mixture
density is the critical temperature and the critical pressure. From the data and the
information, the compressibility factor can be determined, Z. All the data that were
needed to determine the value of Z, is being shown in table below.
Molecular Weight
Formula
Phthalic Anhydride
Water
Carbon Monoxide
Carbon Dioxide
Oxygen
Maleic Anhydride
o-Xylene
Nitrogen
(kg/kmol)
148.100
18.016
28.010
44.010
32.000
98.060
106.16
14.007
C6H4(CO)2O
H2O
CO
CO2
O2
C4H2O3
C8H10
N2
Temperature
Pressure Critical
Phthalic Anhydride
Water
Carbon Monoxide
Carbon Dioxide
Oxygen
Maleic Anhydride
o-Xylene
Nitrogen
Critical, Tc (K)
148.100
18.016
28.010
44.010
32.000
98.060
106.16
14.007
Pc (bar)
C6H4(CO)2O
H2O
CO
CO2
O2
C4H2O3
C8H10
N2
Feed
Top outlet
Bottom Outlet
Pressure (kPa)
Temperature (C)
Mass Flow (kg/h)
Mole Flow
180
55
28872
1368
(vapour)
52.21
100
18614
1115
(liquid)
150
52.35
10258
242
(kgmole/hr)
Vapour Fraction
Component Mole
0.84
1.0000
0.0000
3-7
Fractions
Oxygen (O2)
Phthalic anhydride
0.00336
0.02878
0.00409
0.0000
0.0000
0.16102
(C8H4O3)
Maleic anhydride
0.00398
0.0000
0.02230
(C4H2O3)
Water (H2O)
Carbon dioxide
0.14285
0.06317
0.0000
0.02156
0.7994
0.0000
(CO2)
Carbon
0.0177
0.02156
0.0000
(CO)
Nitrogen (N2)
0.7371
0.89743
0.0000
O-xylene
0.00310
0.00000
0.01734
monoxide
Pcm = Pc y +...
Equation 3.184
T cm = T c y +...
3.185
Where,
Tr
T c ,m
Pr =
P
P c, m
= Mole Fraction
Equation
3-8
n
Pc ,m =
Pc y i
n=1
Pr =
P
P c, m
1
36.692
= 0.02725
Temperature of gas out:
n
T c, m =
T c yi
n=1
Tr
T
T c ,m
373.15
= 138.412
= 2.696
Thus, with the value of 0.02725 bar and 2.5696 K, the value of Z is 0.972
approximately according to Felder and Rosseau (2005).
3-9
Specific volume of the gas:
PV = znRT
V
n
= Z (RT/ P)
(Equation 3.186)
(Equation
3.187)
Where,
P = absolute pressure, bar
V = volume, m3
n = number of moles
T = absolute temperature, K
Z = compressibility factor
R = universal gas constant, 0.083 bar.m3/kmol
V
n
= Z (RT/ P)
1.5
m3
0.972(0.083 .
x 325.65 K )
kmol
= 16.689 m3 / kmol
pg
MW avg
V
n
(3.188)
3-10
16.689 kg /kmol
17.515 m3 /kmol
= 0.9528 kg/ m3
Thus, the density of gas mixture is 0.9528 kg/ m3
Component
O-xylene
Phthalic
Bottom outlet
Molecular
Mole
Density
Density
x/density
weight
fraction, x
(kg/m3)
(kmol/m3)
(m3/kmol)
(kg/kmol)
106.16
148.13
(kmol/kmol)
0.01734
016102
861
1530
8.111
10.329
0.00214
0.01559
98.06
0.02230
1480
15.093
0.00148
18.016
0.7994
1000
55.556
0.01440
anhydride
(C8H4O3)
Maleic
anhydride
(C4H2O3)
Water (H2O)
Pl =
MW avg /
x
p
3-11
kg
kmol
= 42.28
/ 0.03361
m3
kmol
kg
m3
= 1257.96
Q=
(3.189)
Where,
Qg
g
pg
18614
0.9528
kg
x 60 min
m3
= 325
kg
hr
m
min
3-12
For Liquid Phase:
Ql =
l
pl
10258
1257.96
= 0.13591
kg
hr
kg
x 60 min
m3
m3
min
V 1 = 0.1359
m
min
x 30 min
3-13
Holdup time and surge volume are calculated from holdup and surges time which
are selected from the guidelines (W.D Monnery, 1993). From the guidelines and
information given the holdup time and residence time is 5 min and 3 min
respectively. The holdup volume and surge volume are then calculated as below:
V H =(T
)(QL )
(3.190)
VH = (5)(0.13591)
= 0.679 m3
V s=(T s )(QL )
(3.191)
3-14
Vs = (3)(0.13591)
= 0.408 m3
The low liquid level height, H LL were obtained from the low liquid level height
information provided by (W.D Monnery, 1993). At diameter of 1.611 m the H LL is
0.381 m. Then, the height of from low liquid level to normal liquid level and the
height from normal liquid level to high liquid level were calculated:
HH =
HH =
VH
( ) D2v
4
0.679
(1.6112 )
= 2.24 m
HH =
Hs=
VS
( ) D2v
4
0. 408
(1.611 2)
= 1.34 m
0 P 1724
1732 P 3447
3454 P
3-15
L/D
Based from the table above and at operating pressure 200 kPa, the ratio of L/D is 3
where,
Lv
Dv
=3
Lv = 3 Dv
cyl=
D2v Lv
4
(3.192)
Next, substitute Lv into the volume equation to get,
cyl=
3 D3v
4
(3.193)
8.155 m3
Dv=
= 1.611 m
So, the vessel diameter is 1.611 m.
3-16
V
cyl=
D2v Lv
4
2
( 1.611 m ) ( 4.83 m)
4
= 9.845 m3
New volume of the vessel is 9.845 m3.
3-17
objective of sizing a gas liquid. The diameter must be determined first meanwhile the
height is calculated to dampen the flow rate variations of the liquid streams by
permitting sufficient time. The vapour bubbles to flow upwards before it stuck to the
outlet of the bottom those liquid heights.
All of the separators equations are derived from gravity setting equation. The
critical must be determined using the equation given below,
Lv
10
p l pg
pg
V c =K
( 3.194)
Where,
Vc
= empirical constant
Lv
Based on the table 3.3, the value of K obtained is 0.107. The value are taken based
on the orientation on the separator which is horizontal or vertical. The value of the
critical gas velocity are then performed as below
Lv
10
p l pg
pg
V c =K
3-18
= 0.107
kg
kg
0.9528 3
3
m
m 4.83 0.56
(
)
kg
10
0.9528 3
m
1257.96
= 3.17 m/s
The value of critical gas velocity calculated, Vc is 3.17 m/s.
K factor (m/s)
0.122 to 0.152
0.061 to 0.107
0.055 to 0.107
pad)
At atmospheric pressure
0.101
At 2100 kPa
0.091
At 4100 kPa
0.082
At 6200 kPa
0.064
At 10300 kPa
Wet steam
Most vapours under vacuum
Salt and caustic vapours
0.076
0.061
0.046
(Source: IPS-E-PR-880, 1997)
Area of vapour
Ag = Qg/Vc
(3.195)
Qg = 325 m3/min
= 5.42 m3/s
Vc = 3.17 m/s
Ag = Qg/Vc
= 1.7 m2
3-19
Area of liquid
Total area of the vessel is
2
A v=
D
4
A v=
(1.611 m)
4
A v =2.039m2
Al = 2.039 1.7
= 0.34 m2
Vapor/Liquid Ratio
Vapor / liquid ratio of the vessel is
ratio=
Qg
Ql
(3.196)
m3
min
3
m
0.1359
min
325
= 2391
3-20
how the horizontal separator is chosen. The table below shows the summary of
chemical design of flash separator.
Vertical Separator
3.17 m/s
2.039 m2
1.7 m2
0.34 m2
1.611 m
Column, Dv
Length of the Vessel
Volume of the Vessel
Vapour/liquid Ratio
Surge Volume
Holdup Volume
Low Liquid Level
LLL to NLL, HH
NLL to HLL, HS
4.83 m
9.845 m3
2391
0.408 m3
0.679 m3
0.381 m
2.24 m
1.34 m
3.4.5
Mechanical Design
3-21
4)
5)
6)
7)
There two codes that most widely recognized pressure code in worldwide
(Perry, J.H., 1963). That is, ASME Section VII Division 1 and 2 and BS 5500. In
mechanical design of a separator several steps and specification need to be
followed from the standard codes, That is:
I.
II.
III.
IV.
V.
VI.
VII.
VIII.
IX.
X.
10 x 1.5
P design=
1.65
0.165 N /mm
3-22
Criteria
Material of Construction
Aluminium
Stainless
Carbon
Lead
Copper
3-23
Melting
660
Steel 304
1371 - 1399
Steel
1540
327
1084
Point (0C)
Density
2700
8300
7900
11340
8940
(kg/m3)
Corrosion
Low
High
High
Low
Low
Resistance
/tonne
900
1600
300
400-700
800
From the data provided the best materials that is chosen is carbon steel. Carbon
steel have a high corrosion resistance and the highest melting point. From the table
3.5.1 it can be seen that the cost of the carbon steel is the lowest compared to other
metal. This proves that carbon steel is the best metal can be chosen.
3-24
Since the temperature is 850C, the interpolation has to do to get the more accurate
design stress and tensile strength. The interpolation is been calculated as shown
below
( 1000 C850 C )
( 125f ) N /mm2
0
0
2
(100 C50 C ) ( 125135 ) N /mm
=
3-25
Figure 3.4. 7: Guideline for Minimum Wall Thickness with its Vessel Diameter
(Sinnott, 2005)
t=
P i Di
+C
2 Jf Pi
Where,
N
0.165
(1611 mm)
(
mm )
t=
+2 mm
N
N
2 ( 1 ) 129
( mm )(0.165 mm )
2
= 3.032 mm 3 mm
(3.197)
3-26
Following the guideline for minimum wall thickness with its vessel diameter (Sinnott,
2005), the minimum thickness of wall according to the vessel diameter of vessel at
1.611 mm, the diameter should be 7 mm. So, 7 mm is taken to as the wall thickness
since it larger than 3mm that been calculated.
During the separator design for phthalic anhydride production, the type of heads and
closures need to be determined. In this case, Ellipsoidal heads are chosen because
it is commonly used by the industrial and it can stand up to 15 bar of operating
pressure (Sinnott, 2005).
Ellipsoidal Heads
Most standard ellipsoidal heads are manufactured with a major and minor axis ratio
of 2 : 1 (Sinnott, 2005). For this ratio, the following equation can be used to calculate
the minimum thickness required.
e=
Where,
J = joint factor
f = design stress
P i Di
2 Jf 0.2 Pi
(3.198)
3-27
Table 3.4.11: Welded Joint Efficiencies
Join
A,B,C,D
A,B,C,D (See ASME code for limitations)
A,B,C
A,B,C (See ASME code for limitations)
B,C (See ASME code for limitations)
A,B (See ASME code for limitations)
1
0.9
NA
NA
NA
NA
t
type
1
2
3
4
5
6
e=
0.85
0.8
NA
NA
NA
NA
0.7
0.65
0.6
0.55
0.5
0.45
P i Di
2 Jf 0.2 Pi
N
(1611 mm)
mm 2
N
N
2 ( 1 ) 129
0.2( 0.165
)
2
mm
mm2
(
(
0.165
= 1.030 mm
W v =240C v D m ( H v + 0.8 Dm ) t
(3.199)
Where,
3-28
Dm=
Mean diameter, Dm :
D m=(Di +t x 103)m
( 3.200)
(1.611+7 x 10 )m
1.618 m
Though the equation only applies strictly to vessel with uniform thickness, it can be
used to get a rough estimate of the weight of this vessel by using the average
thickness in the equation, 11 mm.
Therefore,
Weight of Insulation
In this production, mineral wool has been chosen for insulation for two-phase
separator due to its capability to absorb heat.
Mineral wool density = 130 kg/m3
Thickness of insulation = 75 mm
V i= Di H v t i
(3.201)
3-29
= ( 1.611 m ) ( 4.83 m )( 0.075 m )
= 1.834 m3
Weight of insulation,
W i=V i pg
(3.202)
1.834 m3 (130
kg
m
)(9.81 2 )
3
m
s
= 2339 N =2.339 kN
Weight of Demister Pad
Stainless steel pads was chosen as the material for the demister pad
Demister pad density = 150 kg/m3
Demister pad thickness = 144 mm
Pad area,
A=
( r 2 ) m2
(3.203)
=
( x 0.80552 ) m2
= 2.038 m
Weight of pad,
W p= A x p x t x g
2.038 m2 x 144
kg
kg
x 0.15 m x 9.81 3
3
m
m
= 431.85 N=0.431 Kn
(3.204)
3-30
W T =W v +W i +W p
(3.205)
28.253+2.339 kN +0.431 kN
31.023kN
1
W o = p air V o2
2
1
(1.225 kg /m3 x (23.61m/ s)2)
2
341
kg
m s2
= 341 N/m2
= 2.164 m
Loading (per linear metre),Fw = 341 x 2.164
= 737.924 N/m
Bending moment at bottom tangent line:
M x=
(3.207)
737.924
2
x 4.83
2
Fw
x H v2
2
(3.206)
3-31
8607.48 Nm
L=
0.165
Pi D i
4t
(3.208)
Pi D i
2t
(3.209)
N
x 1611 mm
mm2
4 x 7 mm
9.494 N /mm2
h=
0.165
N
mm x 1611 mm
2 x 7 mm
2
18.987 N / mm2
w=
Wc
( D i +t ) t
(3.210)
28.256 x 103
( 1611+7 ) 7
D o=1611+ 2 x 7=1625 mm
I v=
3-32
b =
0.600 N /mm 2
z= L + w b
w
(3.211)
z and h .
The greatest difference between the principal stresses will be on the down-wind side
3-33
Skirt thickness
The skirt thickness must be sufficient to withstand the dead weight loads and
bending moments imposed on the vessel.
approximate weight= x
1.611
x 4.83 x 1000 x 9.81
4
96582.202 N =96.582 kN
weight of vessel=31.023 kN
Total weight =96.582+ 31.023=127.605 kN
(Height ( skirtvessel))2
2
6.832
=17.19 kNm
2
(3.212)
3-34
Height of vessel as calculated before = 4.83 m
Height of skirt = 2m
Bending stress in skirt,
bs
bs=
4 Ms
(D s+t s )D s t s
0.557 N /mm
ws =
Where
W
(Ds +t s )t s
W =total weight ( weight of vesseldead weight )=127.605 kN
ws (test )=
127.605 x 103
( 1611+15 ) 15
1.67 N /mm
Where
ws
W v =weight of vessel=28.253 N
ws ( operating )=
28.253 x 103
(1611 +15 ) 15
0.37 N / mm2
Maximum
Maximum
s ( tensile ) f s J sin
3-35
0.187
N
N
( 1 ) 129
sin 90
2
mm
mm2
0.187
N
N
129
2
mm
mm2
s ( compressive ) 0.125 E
ts
sin
Ds
2.227
N
15
0.125 x 200000(
)sin 90
2
1611
mm
0.035
N
N
232
2
2
mm
mm
Both criteria are satisfied, by adding 2 mm for corrosion allowance. Then, the design
thickness of skirt is 17 mm.
Db = 1.8
= 5654.89 mm
5654.89 mm
600 mm
9.424
125 N /mm2
3-36
area of bolt , A b=
1 4 Ms
(
W )
N b f b Db
(3.213)
4 ( 17.19 x 103 )
1
(
31.023 x 10 3)
1.8
12 ( 125 )
= 4.5mm2
4.5 mm2 4
= 2.3 mm
pV 2<1400 kg /m s2
pV 2<2100 g/ m s 2
Inlet device
pV <1500 kg /m s
For Outlet:
Gas Outlet
3-37
Liquid Outlet
pV 2<2 m/s
Qg =325
m
min
Q l= 0.1359
m
min
3
Qtotal=Q g+ Ql=325
m
m
+0.1359
min
min
3
= 325.13590
m
min = 5.418
m
s
pg =0.9528
kg
m3
kg
m3
pl= 1257.96
pmixture=
p g Q g+ p l Q g
Q g+ Q l
(3.214)
0.9528
kg
m3
kg
m3
325
+
1257.96
(0.1359
)
min
min
m3
m3
m3
m3
(325
+0.1359
)
min
min
)(
)(
1.478 kg / m3
3-38
Assume half pipe inlet device:
pV 2=2100 kg/m s 2
Allowable
Allowable velocity,
v = p V 2 / p
kg
)
m3
= 37.694 m/s
So then the nozzle area,
A=Q total /v
5.418
m
/ 37.694 m/s)
s
0.1437 m2
d nozzleinlet = 4 A /
4 (0.1437 m2)/
0.428 m
Qg =325
m3
min
= 5.417
m3
s
3-39
Gas outlet density:
pg =0.9528
Allowable
kg
m3
pV 2=1500 kg/m s 2
Allowable velocity,
v = p V 2 / p
(3.215)
kg
)
m3
= 39.68 m/s
Thus the nozzle area,
A=Q g /v
A=(5.41 m3 / s) / (39.68m/s)
A=0.13651m 2
Required nozzle diameter,
dnozzle gas=
dnozzle gas=
4 (0.13651)/
4 A /
(3.216)
3-40
Ql=0.13591 m3 /min
0.00227 m3 /sec
l=1257.96 kg /m
Allowable Velocity
v =2.0 m/s
A=Q l /v
A=(0.00227 m 3 /sec ) /(2.0 m/s)
A=0.00114 m 2
Required nozzle diameter
d nozzleliquid= 4 A /
d nozzleliquid= 4 (0.00114)/
d nozzleliquid=0.03810 m=38.098mm
3-41
Table 3.4.13 shows the flange design of the separator, for the feed inlet and
the outlet of the gas, the value of the nozzle is high which is 418 and 426 mm
3-42
respectively. Based on table 3.4.12, the highest value is 300 mm, thus the data for
the feed inlet and outlet gas are taken at nozzle sizing of 300mm.
Nom
Pipe
o.d.
Inlet
Size
300
d1
323.
Outlet
Gas
Outlet
Flange
Raise d
Boltin
g
Faced
d4
f
440
22
44
365
300
9
323.
440
22
44
365
40
9
48.3
130
14
26
80
Liquid
3.4.6
Drilling
Bos
No.
d2
s
d3
M20
12
22
395
355
M20
12
22
395
355
M12
14
100
70
Value
0.165 N/mm2
358.05K
Carbon Steel
129 N/mm2
360 N/mm2
7mm
1.030mm
28.253 kN
Skirt Support
3-43
References
Sinnot, R.K., Coulson, J.M., Richardson, J.F., (2005), Chemical Engineering Design,
4th Edition, Vol. 6, UK: Butterworth-Heinemann.
IPS-E-PR-880, (1997), Engineering Standard for Process Design of Gas (Vapour)Liquid Separators, Original Edition.
Barker, W.F., Oil and Gas J. (1982), p. 186.
Polderman, H. G., Bourna, J. S., and H. van der Poel, Design Rules for Dehydration
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