CHEMICAL DESIGN
5.1
PIPE REACTOR
5.1.1
Introduction
2
The concept of the plug flow reactor or pipe reactor denotes an ideal tubular reactor, in
which all fluid elements travels in one direction with exactly the same speed. A PFR
may be used for both liquid phase and gas phase reactions, for both laboratory-scale
investigation of kinetics and a large-scale production. The reactor itself may consist of
an empty tube or vessel, or it may contain packing or a fixed bed of particles.
The output of a chemical reactor depends, among other things, on the residence time
(the average length of time the material is in the reactor), the temperature, and the fluid
dynamics. These conditions may make designing a single reactor to handle both the
initial and final flow rates undesirable. However, sometimes this can be done by
installing a vertical reactor and initially maintaining it only partially full.
A pipe reactor is similar to a CSTR in being flow reactor, but is different in its mixing
characteristics. It is different from batch reactor in being a flow reactor, but it similar in
the progressive change of properties, with position replacing time. The flow through the
vessel both input and output streams, is continuous but not necessarily at constant rate.
There is no axial mixing of fluid inside the vessel. There is complete radial mixing of
fluid inside the vessel; thus, the properties of the fluid, including its velocity, are uniform
in this plane.
This pipe reactor is designed to produce ammonium nitrate with a capacity of 100000
MT per year. The process is considered exothermic reaction. There are a few
advantages by using this pipe reactor such as:
a) Low investment cost with no preneutralizer and low recycle ratio.
b) A lower operating cost with no low electric power consumption and a high
efficiency of ammonia consumption.
c) A high adaptability in the use of feed stocks- nitric acid from various origin and
concentrations can be used.
d) A higher operating flexibility and stability
e) A low environment impact because of the low emission of gases.
3
5.1.2
N H 3 ( g ) + HN O3 ( aq ) N H 4 N O3 (aq)
H=145
kJ
( gmole
)
To ensure the validity of the reactions and equations used in designing the reactor.
These assumptions that been made are:
1. The reaction is in steady state condition.
2. The reaction rate is valid for the above reaction
3. Irreversible reactions.
4. Density of the component remain constant throughout the reactor, = 0.
5. The temperature is assumed as constant (Isothermal reaction)
5.1.2.2 Effect of Temperature: Arrhenius Equation and Activation Energy
The theory of the temperature effect on the reaction rate originated from the
temperature effect on the equilibrium constant. It is known that:
d ln K H
=
Equation5.1
R
1
d
T
( )
d ln k A E A
=
Equation5.2
dT
RT2
Where EA is a characteristic (molar) energy which is called as the energy of activation.
Since (-rA) (hence kA) increases with increasing T almost every case, EA is a positive
quantity. Integration of equation (5.2) on the assumption that EA is independent of T
leads to or
ln k A =ln A
k A = A exp
EA
Equation5.3
RT
( ERT ) Equation5.4
A
k A = A exp
( ERT )
A
k A =1.327 exp
3.2744 x 10
1.98588 x 453.15
k A =1.33
l
mole . sec
Start
End
Phase
Temperature
Pressure
Stream In
Stream Out
Mixture
86.04 oC
600 kPa
(Operating condition)
Mixture
180 oC
540 kPa
7
Molar Flow
Mass Flow
Component
436 kgmole/h
1.418 x 104 kg/h
290.6kgmole/h
1.418 x 104 kg/h
Molar Flowrate
Molecular
Mass Flowrate
Mass
(kgmole/h)
Weight
(kg/h)
Fraction
222.11
145.45
17
63
3782.5
9165.4
0.2667
0.6263
145.45
80
11643
0.821
Properties
Flowrate (kg/hr)
Molar Flowrate
Ammonia
3782.5
222.11
Nitric Acid
9165
145.45
Water
1233
68.448
(kmol/hr)
Mass Fraction
Density (kg/m3)
0.2667
616.07
0.6463
1523.64
0.0869
997.99
Reactant
Ammonia
Nitric Acid
Product
Ammonium
Nitrate
i i
14180.5
Flowrate in m3/hr =
( hkgr )
kg
1235.76 3
m
( )
=11.48 m3/hr
: 12.67 kmol/m3
8
Ammonia,
: 19.35 kmol/m3
Water
: 5.96 kmol/m3
The reactor is made of a main reaction, which is reaction to produce ammonium nitrate.
The reactions are:
N H 3 ( g ) + HN O3 ( aq ) N H 4 N O3 (aq)
From basic equation:
A + B C
The kinetic reaction of this reaction is:
r c =k C nA C mB
Equation 5.5
Equation 5.6
EA = Activation energy
R = Ideal gas constant
T = Temperature of the reaction
Substituting 5.5 into 5.6
From the reaction between ammonia and nitric acid and produce ammonium nitrate:
N H 3 ( g ) + HN O3 ( aq ) N H 4 N O3
9
The reaction rate given by Gerhard Kramm et al., (1994)
r=1.33 exp
3.2744 x 102
C 0.81 C 0.4
1.98588 x 406.17 HN O N H
0.4
r=1.33 C 0.81
HN O C N H
3
Equation 5.7
r =1.33
The reaction rate based on the kinetic experimental data under integral regime will be
inserted to the performance equation under Levenspiel, 1999 pg. 111:-
10
1
r A
() d X A
XA
=C A 0
0
1.33
1
0.99
=C HN O
12.6712.67 X HNO3
19.3512.67 X HNO3
1.33
12.67
0.99
=
0
CHNO3/-rNH4NO3
0.37239
0.39340
0.41671
XHNO3
0.55
0.60
0.65
CHNO3/-rNH4NO3
0.76513
0.85009
0.95504
11
0.44272
0.47194
0.50496
0.54258
0.58582
0.63600
0.69494
0.15
0.20
0.25
0.30
0.35
0.40
0.45
0.70
0.75
0.80
0.85
0.90
0.95
0.99
1.08799
1.26196
1.49973
1.84528
2.39683
3.43237
23.57769
1.2
XHNO3
=C HNO3
( rNH 41 NO 3 ) d X HNO3
h=
ba
n
F=f o
= 3 [F+ L+ 4 R+2 E]
12
L=f n
n1
R= f i=f 1 +f 3+ +f n1
i=odd
n2
E=
i =even
f i=f 2 +f 4 ++ f n2
Let take n= 5
h=
0.990
5
0.198
N
X
Fn
0
0
0.372395
1
0.198
0.4707
2
0.396
0.631692
3
0.594
0.941161
F=f o=0.372395
L=f n=23.57769
R=f 1 +f 3 = 0.470700 + 0.941161 = 1.411861
E=f 2 + f 4=0.631692+1.779774=2.411466
0.99
=C HNO3
(r
1
NH 4 NO 3
)d X
HNO 3
4
0.792
1.779774
5
0.990
23.57769
13
0.198
[ 0.372395+23.57769+ 4 ( 1.411861 ) +2 ( 2.411466 ) ]
3
2.3 s
0.99
=C HNO3
(r
1
NH 4 NO 3
)d X
HNO 3
=C HNO3 x 2.3
O
=12.67 x 2.3 s
29.14 s
5.1.2.8 Calculation of the Volume, V of the reactor
To find the volume of the pipe reactor,
C HN O
V=
F HN O
C HN O
=
3
V
F HN O
V=
12.67
hr
3600 s
V =0.093 m
V = r L
Radius of the reactor to be taken as 0.2 m, therefore, the height of the reactor is,
14
0.093
L=
m = 0.065 m L
0.093 m 3
2 2
0.065 m
L=7.007 m
L=7 m
Villard et. al state that the diameter of most the pipe flow reactor generally used are
between 200 mm and 10 mm and a length ranging between 1.5 m and 10 m. the ratio
of length/diameter is usually not below than 50. So the diameter and length from the
calculation are valid.
15
Nitric
Acid
Product to
separator
Ammonia
5.2.1
The main purpose of this gas liquid separator vessel is to increase the concentration of
ammonium nitrate into 94%. The separator also act as knockout drum were the
pressure of the inlet stream is reduced from 6 bar to 5.4 bar.
Vertical Separator
16
Bellow are the summary equation used for vertical separator design:
Summary equation for vertical separator design:
Vv'=vvA
Equation 5.10
kv = 0. 1 ft/s (0.03045 m/s) with no mist eliminator
kv = 0.35 ft/s (0.107 m/s) with a mist eliminator
A = TI D2/4
LL A = VL' ts where the minimum value of LL is 2 ft (0.610 m)
3 < ts < 5 min
L = LL+1.5D+1.5ft or
L = 8.5 ft (2.59 m) whichever is larger
If L/D < 3.0, then recalculate L so that L/D > 3.0 by letting L/D = 3.2. If L/D >5 use a
horizontal separator.
Splash Plate: prevent the corrosion of vessel wall opposite the feed point.
Radial vane vortex breaker: ensure gases are not entrained with the exiting
liquid.
17
Summary equation for horizontal separator design:
Vv' = 0.5vvA
Equation 5.11
kv = 0.10 ft/s (0.0305 m/s) with no mist eliminator
kv = 0.35 ft/s (0.107 m/s) with a mist eliminator
A = 7iD2/4 minimumD = 5.5 ft(1.67m)
0.5LA = VL'ts
7.5 <ts< lOmin
If L/D < 3.0, then recalculate L so that L/D > 3.0 by setting L/D = 3.2. If L/D > 5.0, then
recalculate D so that L/D < 5.0 by setting L/D = 4.8
5.2.2
First, we assume to design a vertical gas liquid separator. This is because in this
vessels requred less space for installation compare to the horizontal vessel and have
high efficiency for separating vapor phase and liquid phase product by only utilize their
specific gravity.
Uvapor max = K[(rL -rv )/ rv ]0 5
where
U = Velocity, ft/sec
r = Density of liquid or vapor, lbs/ft3
K = System constant
(WL/Wv)(rv/rL)0.5
where
W = Liquid or vapor flow rate, lb/sec
For a horizontal vessel KH = 1.25Kv.
(WL/Wv)(rv/rL)0.5 = ( 3.3528kgs-1/0.585 kgs-1)/(2.7493/1225)0.5
= 0.273
18
0.2106m3/s
1.88543m/s
= 0.11147m2
Assume that vapor occupied 20% from the total area during full liquid volume
Total cross sectional Area, Atotal = 0.11147m2 / 0.2 = 0.5573m2
Minimum internal diameter, Dmin = (4x 0.5573m2 /)0.5 = 0.8426m
Dmin in Standard Pipe size : 33.25in = 0.8447m
Liquid volume requirement = 0.00274m3/ s x 5 min x 60 s = 0.82109m3
Liquid level holdup, LL = (VLts)/ Atotal
= (0.00274m3 s-1.300s)/ 0.5573m2
= 1.475 m
Vessel Height, L = LL+1.5D+1.5ft
= LL+1.5D+0.457m
= 1.475 m + 1.5(0.8445) + 0.457m
= 3.197m
Standard Height Design available: 10ft 6in. = 3.200m
19
L/D = 3.2/0.8445 = 3.7892 is in 3<L/D <5
Design is acceptable because the length and diameter ratio is acceptable. The length
and diameter ratio is an indicator to sizing any vessel design in order to standardize
with the standard vessel design.
5.3 HEAT EXCHANGER
5.3.1 Introduction
Heat exchanger is a device to change the heat between two fluids that have different
temperature. The two fluids did not mix each other because they were separated by a
solid medium. Heat exchangers are widely used in engineering application like air
conditioning, power production, waste heat recovery and chemical processing.
5.3.1.1 Flow arrangement
Heat exchangers may be classified according to their flow arrangement. There are two
main flow arrangements which are parallel-flow and counter-current flow. In counter
flow heat exchangers the fluids enter the exchanger from opposite ends. This flow
arrangement usually used for liquid-liquid, condensing and gas cooling applications.
Units are usually mounted vertically when condensing vapour and mounted horizontally
when handling high concentrations of solids.
20
other side. Compared both flow arrangements, the counter current design is most
efficient, in that it can transfer the most heat from the heat transfer medium. So that, we
choose counter current flow as our heat exchanger flow arrangement for production of
Ammonium Nitrate.
21
No
Types
Functions
.
1.
Double
pipe
heat
exchanger
cooling.
2.
exchanger
3.
Plate exchanger
Plate-fin exchanger
Spiral
4.
5.
heat
exchanger
6.
Air cooled
Direct contact
Agitated vessels
Fired heaters
7.
8.
9.
22
5.3.1.4 Basic Principles of Design
The principal design parameters that are evaluated at this stage involve all the
operating conditions and basic exchanger configurations. Others parameters also
includes are tubes and shell conditions (diameter, length, layout, baffles), coolant flow
rate, pressure drop at shell and tube side, heat transfer rate and lastly heat transfer
area.
5.3.1.4.1 Design Criteria for Process Heat Exchangers
The criteria that a process heat exchanger must satisfy are easily enough stated if we
confine ourselves to a certain process. The criteria include:
1) The heat exchanger must meet the process requirements. This means that it
must effect the desired change in thermal condition of the process stream
within the allowable pressure drops.
2) The heat exchanger must withstand the service conditions of the environment
of the plant which includes the mechanical stresses of installation, start up,
shutdown, normal operation, emergencies and maintenance. Besides, the
heat exchanger must also resist corrosion by the environment, processes and
streams. This is mainly a matter of choosing materials of construction, but
mechanical design does have some effect.
3) The heat exchanger must be maintainable, which usually implies choosing a
configuration that permits cleaning and replacement. In order to do this, the
limitations is the positioning the exchanger and providing clear space around
it. Replacement usually involves tubes and other components that may be
especially vulnerable to corrosion, erosion, or vibration.
4) The cost of the heat exchanger should be consistent with requirements.
Meaning of the cost here implement to the cost of installation. Operation cost
and cost of lost production due to exchanger malfunction or unavailable
should be considered earlier in the design.
5) The limitations of the heat exchanger. Limitations are on length, diameter,
weight and tube specifications due to plant requirements and process flow.
23
There are heater,cooler,condenser and reboiler in production of Ammonium Nitrate from
reaction between ammonia and nitric acid. In this chapter, we only show the detail
calculation for designing a cooler which is E-106. The function of E-106 is to exchange
the temperature between the stream 18 and stream 19 from 204.3C to 100C.
5.3.1.6 Selection of Basic Heat Exchanger Type
Shell and tube heat exchangers are the most widely used equipments in chemical
industry. They are mostly used as heat transfer equipments but in few cases they are
also used as Reactors and Falling Film Absorbers. However, in the case of recovering
Sulphur from Sour Water, shell and tube heat exchangers was chosen as the heat
exchanger.
Sizes of various part of shell and tube of heat exchangers like shell, tubes, tie-rods are
standardized. Standards developed by Tubular Exchanger Manufacturers Association,
USA (TEMA) are universally used for design of shell and tube heat exchangers.
5.3.1.6.1 Shell
Shell is the costliest part of heat exchanger. The cost sensitively changes with change
in the diameter of shell. Using TEMA standard, shell size ranges from 6 in
(152 mm) to 60 in (1520 mm). Standard pipes are available up to 24 in (608 mm). Thus,
shell greater than 24 in (608 mm) is fabricated by a rolling plate. Shell diameter
depends on tube bundle diameter. For fixed tube sheet shell and tube heat exchanger,
the minimum gap between shell and tube is ranging from 10 mm to 20 mm. For
maximum pull through floating head heat exchanger the range is from 90 mm to 100
mm.
5.3.1.6.2 Tube
Tube size ranges from in (6.35 mm) to 2.5 in (63.5 mm) in shell and tube heat
exchanger. Data for the standard tubes are given in TEMA standard. For the standard
tubes, its size is equal to outer diameter of tube. Thickness of standard tubes is
expressed in BWG (Birmingham Wire Gauge). Increase in BWG means decrease in
thickness of tube. For no phase change heat exchangers and for condensers, in
(19.05 mm) OD tube is widely used in practice. Tubes are available in standard lengths
like 6 ft (1.83 m), 8 ft (2.44 m), 12 ft (3.66 m), 16 ft (4.88 m) and 19.67 ft (6.00 m).
24
Tube side passes are provided to decrease the tube side flow area and to decrease
tube side velocity thereby to improve the tube side heat transfer coefficient, at the
expense of pressure drop. This is true only if there is no phase change on tube side.
Hence, more number of tube side passes are recommended only if there is no change
in phase of the tube side fluid.
5.3.1.7 Fluid Allocation Factor
According to the following factors, cooling water as cooler at tube side while organic
solvent on shell side only if there is no phase change in shell side and tube side. Fluid
allocation depends on following factors:
Table 5.4: Fluid allocation factor
Factor
Fluid Allocation
Corrosion
Fouling
Fluid
Very hot or very cold liquid is place in tube side to avoid the
temperatur
Operating
pressure
Fluid
rate
and
viscosity
5.3.2
Chemical Design
25
2. Collect the fluid physical properties required: density, viscosity and thermal
conductivity
3. Decide the type of heat exchanger to be used
4. Select the trial value for the overall coefficient, Uo
5. Calculate the mean temperature different, Tlm and heat transfer area required
6. Decide the heat exchanger layout and calculate the individual coefficient
7. Calculate the overall coefficient and compare with the trial value. If the calculated
value differs from the estimated value, substitute the calculated for the estimated
value and return to step 4
8. Calculate the heat exchanger pressure drop; if unsatisfactory return to the step
above.
5.3.2.1 Process Condition
The process condition for designing tube heat exchanger as follows.
Table 5.5: Process condition of the tube side
Inlet
Properties
0
Temperature ( C)
Pressure (kPa)
Specific heat (kJ/kg0C)
Thermal conductivity, Kf (W/m0C)
Density (kg/m3)
Viscosity (N sm-2)
(stream 18)
204.3
520
3.157
65
1138
0.7013
Mean
152.15
525
2.9737
70.74
1239
0.8414
Outlet
(stream 19)
100
530
2.79
76.48
1340
0.9815
Table 5.6 was shown the process condition consideration in designing shell for heat
exchanger.
Table 5.6: Process condition of shell fluid (cooling water)
Properties
Temperature (0C)
Pressure (kPa)
Specific heat (kJ/kg0C)
Thermal conductivity, Kf (W/m0C)
Density (kg/m3)
Viscosity (N sm-2)
Inlet
25
101.3
4.2
166.89
997
0.8904
Mean
49.5
101.3
4.2
174.335
986
0.6349
Outlet
74
101.3
4.2
181.78
975
0.3793
26
As mention before, we have decided to choose type of shell and tube as our heat
exchanger. Table 5.7 was shown the design criteria for shell and tube heat exchanger.
Table 5.7: Criteria design of Shell and Tube Heat Exchanger
Heat exchanger type
Design type
Heat exchanger orientation
Tube inlet direction
Tube side inlet stream
Tube side outlet stream
Tube side
Shell side inlet stream
Shell side outlet stream
Shell side
Heat duty (kW)
5.3.2.3 Heat Load
27
The flow arrangement for the heat exchanger is counterflow and the type of
construction is one shell pass and two tube passes.
Table 5.8: Temperature for shell and tube
Tube or Shell side
Tin (C)
Tout (C)
Tlm
Logarithmic mean temperature,
Tube
204.3
100
Shell
25
74
(T1 t2 ) (T2 t1 )
(T t )
In 1 2
(T2 t1 )
Equation 5.12
28
Tube Dimension
5m
0.01905m
0.01483m
14
= 5(0.01905)
= 0.2992 m2
Using the area needed from the duty and the area for each tube, we can calculate the
number of tube needed, Nt.
29
30
Nusselt number, Nu = jh x Re x (Pr)0.33
= 0.032 x 4149.19 x 0.04
= 5.31
The tubes in a heat exchanger are usually arranged in an equilateral triangular, square
or rotated square pattern. The triangular and rotated square patterns five higher heat
transfer rates. Here we use the triangular pattern.
Tube pitch is the distance between tube centers and formulated as,
Pt = 1.25 x OD
31
= 0.0238 m
From Table 12.4 (R Sinnott,2009),
Triangular pitch, K1 = 0.249
(4 passes), n
=
2.207
Pt
32
Vt = Wwater/water
= (19409.91/3600)/988.15
= 0.0055 m3/s
Shell side velocity, Us = Vt/As
= 0.0055/0.0021
= 2.62 m/s
Reynolds number, Re = ( x Us x De)/
= (988.15 x 2.62 x 0.0135)/(0.6349/1000)
= 55049
Prandtl number, Pr = (Cp x )/Kf
= [( 4.2 x 1000) x (6.349 x 10-4)]/174.335
= 0.0153
Use segmental baffles with 25% cut.
From figure 12.29 (R Sinnott, 2009), the value of heat transfer factor, jh is 0.0027 by
neglecting the viscosity correction.
The heat transfer coefficient on shell side,
hs = (Kf/De) x jh x Re x Pr0.33
= (174.335/0.0135) x 0.0027 x 55049 x 0.01530.33
= 483183 W/m2oC
From figure 12.24 (R Sinnott, 2009), the value of heat transfer factor, jf is 0.0056.
Pressure drop on shell side,
Ps = 8 x jf x (Ds/De) x (L/IB) x (Ut2/) x (/w)0.14
= 18025.4 N/m2
The relationship between overall coefficient and individual coefficients is given by:
1
1
1
ODln(OD/ID ) 1
=
+
+
+
U o h s h od
2k w
h id
OD
ID
1 OD
(
)
h t ID
Equation 5.13
Where,
Uo = the overall coefficient based on the outside area of the tube, W/m2. C
hs = tube heat transfer coefficient W/m2. C
ht = shell heat transfer coefficient W/m2. C
33
hid = inside dirt coefficient W/ m2 . oC
hod = outside dirt coefficient W/ m2. oC
kw = thermal conductivity of the tube wall material W/m2.C
OD =tube inside diameter, m
OD = tube outside diameter, m
Table 5.10: Heat transfer coefficient
hs (W/m2.oC)
483183
Ht (W/m2.oC)
25329.02
hod (W/m2.oC)
5000
hid (W/m2.oC)
5000
kw (W/m.oC)
16
ID (m)
0.01483
OD (m)
0.01905
Overall heat transfer coefficient can be calculated by using the formula using Equation
5.13 abbove:
1
1
1
ODln(OD/ID ) 1
=
+
+
+
U o h s h od
2k w
h id
OD
ID
1 OD
(
)
h t ID
= 0.00162
Uo = 617.28 W/m2.oC
Error pencentage = Uassumed Ucalculated x 100
Ucalculated
= 750 617.28 x 100
617.28
= 21.5 %
Hence, the calculation accepted because the percentage is less than 30%.
5.3.2.8 Summary of Chemical Design and Sizing for Heat Exchanger
Table 5.11 shown the summary for design and sizing of shell and tube heat exchanger.
Table 5.11: Chemical Design and Sizing for Heat Exchanger
Parameter
Item No
Function
34
204.3 0C (stream 18) to 100 0C
Heat Duty, Q (kW)
Hot Fluid Properties
Flowrates (kg/hr)
Inlet temperature (C)
Outlet temperature (C)
(stream 19)
1109.6 kW
Process Stream from 18 to 27
12880.00
204.3
100.0
Utility (water)
19409.91
25.0
74.0
16.24
58
0.01483
0.01905
5.0
219.8
0.23
25329.02
483183
coefficient, (W/ m C)
Overall Coefficient,
2
617.28
Uo (W/ m . C)
% error
Tube Pressure Drop (N/m2)
Shell Pressure Drop (N/m2)
5.4
5.4.1
introduction
21.5
17205.6
18025.4
Distillation separates two or more liquid components in a mixture using the principle of
relative volatility or boiling points. The greater the difference in relative volatility the
greater the non-linearity and the easier it is to separate the mixture using distillation
process. The process involves production of vapor by boiling the liquid mixture in a
distillation column and removal of the vapor from the distillation column by
condensation. Due to differences in relative volatility or boiling points, the vapor is rich
in light components and the liquid is rich in heavy components.
35
Often a part of the condensate is returned (reflux) back to the still and is mixed with the
outgoing vapor. This allows further transfer of lighter components to the vapor phase
from the liquid phase and transfer of heavier components to the liquid phase from the
vapor phase. Consequently, the vapor stream becomes richer in light components and
the liquid stream becomes richer in heavy components.
Different types of devices called plates, trays or packing are used to bring the vapor and
liquid phases into intimate contact to enhance the mass transfer. Depending on the
relative volatility and the separation task (i.e. purity of the separated components) more
trays (or more packing materials) are stacked one above the other in a cylindrical shell
to form a column. The distillation process can be carried out in continuous, batch or in
semi-batch (or semi-continuous) mode.
5.4.1.1 Continuous Distillation
Ammonia Recovery Column (ARC) T-101 is a distillation column. ARC operates in
continuous mode. Continuous distillation is an ongoing separation in which a mixture is
continuously (without interruption) fed into the process and separated fractions are
removed continuously as output streams. The feed of ARC contains three components;
ammonia, ammonium nitrate, and water which are more than two components; called
multi-component column.
In the distillation process, volatile vapor phase and a liquid phase that vaporizes are
involved. The liquid mixture (feed), which is to be separated into its components, is fed
into the column at one point along the column. Liquid runs down the column due to
gravity while the vapor runs up the column. The vapor is produced by partial
vaporization of the liquid reaching the bottom of the column. The remaining liquid is
withdrawn from the column as bottom product rich in heavy components. The vapor
reaching the top of the column is partially or fully condensed. Part of the condensed
liquid is refluxed into the column while the remainder is withdrawn as the distillate
product. The column section above the feed tray rectifies the vapor stream with light
components and therefore is termed as rectifying section. The column section below
the feed tray strips heavy components from the vapor stream to the liquid stream and is
termed as stripping section.
36
37
installed, or an oversized diameter is used. Either option is expensive. Cartridge
trays also run into leakage and hold-down problems. Packing is normally a
cheaper and more desirable alternative.
b) Corrosive systems
The range of packing materials is wider than that commonly available for trays.
Ceramic and plastic packings are cheap and effective. Trays can be
manufactured in nonmetals, but packing is usually a cheaper and more
desirable alternative.
The main disadvantage is the difficulty in getting good liquid distribution,
particularly for large diameter columns or very tall columns. Even if liquid is spread
evenly over the packing at the top of the column, liquid tends to move toward the wall
and to flow through the packing in preferred channels. The following factors generally
factor favored trays compared to structured packings, but usually not compared to
random packings.
a) Material of Construction
Due to the thin sheets used in structured packings, their materials of
construction need to have better resistance for oxidation or corrosion. For a
service in which carbon steel is usually satisfactory with trays, stainless steel
may be required with structured packings.
b) Column Wall Inspection
With structured packings, it is often difficult to inspect the column wall without
damaging the structured packings. Due to their snug fit, structured packings are
easily damaged during removal.
c) Washing and Purging
Thorough removal of residual liquid, wash water, air, or process gas trapped in
structured packings at startup and shutdown is more difficult than with trays.
Inadequate removal of these fluids may be hazardous.
38
5. Size the column: diameter, number of real stages.
6. Design the column internals: plates, distributors, packing supports.
7. Mechanical design: vessel and internal fittings.
Distillation consumes huge amounts of energy, both in terms of cooling and heating
requirements. The best way to reduce operating costs of existing units is to improve the
efficiency and operation via process optimization and control.
5.4.2
Ammonia (NH3)
Product
Feed inlet
Distillate
Bottom
Stream 15
Stream 16
Stream 18
75.0530
0.0075
145.4499
39
145.4500
74.9850
0.0553
Water (H2O)
68.4480
0.0075
68.4448
Total
288.9510
75.0000
213.9500
The minimum number of stages is calculated by using Fenske Equation (Fenske, 1932)
since McCabe-Thiele method is only applicable for two components system, not
applicable in determining minimum number of stages for multicomponent system.
5.4.2.2.1
A saturated liquid is at its bubble point where any rise in temperature will cause a
bubble of vapour to form whereas a saturated vapour is at its dew point where any drop
in temperature will cause a drop of liquid to form. Therefore, the determination of bubble
point and dew point temperature is crucial in order to calculate the minimum number of
stages, as well as the condenser and reboiler temperatures.
Dew points and bubble points can be calculated from the vapour-liquid equilibrium for
the system. In terms of equilibrium constants, bubble and dew point are defined by
equations
40
yi Ki xi 1.0
Bubble point :
xi
Dew point
yi
1.0
Ki
ln P* a
b
d ln T eT
T c
Equation 5.14
where a, b, c, d, e and f are the Antoine constant taken from HYSYS simulation, P in
kPa and T in Kelvin.
Ki
P*
P
Equation 5.15
Table 5.13: Antoine constant
Component
NH4NO3
NH3
H2O
a)
a
219.862
59.655
65.9278
b
-23155.8
-4261.5
-7227.53
c
0.00
0.00
0.00
d
-27.1074
-6.9048
-7.17695
e
1.70 x 10-17
1.00 x 10-5
4.03 x 10-6
f
6.00
2.00
2.00
By using goal seek in the excel program, the value of the dew point temperature is
369.6 K with the constant operating pressure is 450 kPa.
41
Table 5.14: Dew point temperature data
Component
NH4NO3
NH3
H2O
Total
b)
Y
0.0001
0.9998
0.0001
1.0000
P* (kPa)
0.0488
5815.6343
88.9981
K
0.0001
12.9236
0.1978
y/K
0.9227
0.0774
0.0005
1.0006
X
0.6798
0.0003
0.3199
1.0000
P* (kPa)
56.4429
30603.3974
1480.5590
K
0.1085
58.8527
2.8472
xK
0.0738
0.0152
0.9109
0.9999
K LK
K HK
Equation 5.16
where KLK
KHK =
Ki
yi
xi
Equation 5.17
42
Where yi
xi
Component
Distillate
Bottom
Distillate
Bottom
Average
NH4NO3
0.0001
0.1085
0.0005
0.0381
0.0046
NH3
12.9236
58.8527
65.3456
20.6702
36.7519
H2O
0.1978
2.8472
1.0000
1.0000
1.0000
5.4.2.2.3
The Fenske equation (Fenske, 1932) can be used to estimate the minimum stages
required at total reflux. This equation is applicable for multicomponent systems. The
minimum number of stages can be obtained by equation:
x LK x HK
x HK d x LK
log LK
log
N min
Equation 5.18
where LK
average relative volatility of the light key with respect to the heavy key
xLK
xHK
N min
0.9998 0.3199
log
0.0001 0.0003
log 36.7519
N min 4.5
N min 5
stages
Then, the theoretical number of stage is given by equation:
43
N T 2N min
Equation
5.19
N T 2(5)
N T 10
stages; including reboiler.
5.4.2.2.4 Calculation for Minimum Reflux Ratio, Rmin
Colburn (1941) and Underwood (1948) have derived equations for estimating
the minimum reflux ratio for multicomponent distillations. As the Underwood
equation is more widely used it is presented and the equation can be stated
in the form:
i xi,d
R min 1
Equation 5.20
where,
i
Rmin =
xi, d
i xi, f
1 q
Equation 5.21
where,
xi,f
44
q
The value of must satisfy the relation HK < < LK. By assuming the feed is enter at
its boiling where q = 1, the value of is determined using goal seek in excel application.
i xi, f
xf
xf
xf /
NH4NO3
0.0046
0.5034
0.0023
-0.0012
NH3
36.7519
0.2597
9.5445
0.2736
H2O
1.0000
0.2369
0.2369
-0.2725
[xf / ( )]
-0.0001
Xd
xd
xd /
NH4NO3
0.0046
0.0001
0.0000
0.0000
NH3
36.7519
0.9998
36.7446
1.0534
H2O
1.0000
0.0001
0.0001
-0.0001
[xd / ( )]
R min
i x i,d
i
1.0533
45
R min 1.0533 1
R min 0.05
The minimum reflux ratio can also be determined by using the Underwood equation,
R min
x d , LK
x d , HK
x
f , HK
f , LK
Equation 5.22
where xd,LK =
xd,HK =
xf,LK =
xf,HK =
R min
0.9998
1
0.0001
36.7519
36.7519 1 0.2597
0.2369
R min 0.11
Since the value of Rmin calculated using Underwood equation is bigger than the previous
calculation, therefore the value of R min = 0.11 will be used for the next calculations. For
many systems, the optimum reflux ratio will lies between 1.2 to 1.5 times the minimum
reflux ratio. Optimum reflux ratio, R = 0.11 x 1.5 = 0.16.
5.4.2.2.5
Plate Efficiency
The OConnell correlation shown in Figure 4.3 can be used to estimate the overall
column efficiency. The equation correlated with the product of the relative volatility of
the light key and the molar average viscosity of the feed with estimated at the average
column temperature. Eduljee (1958) has expressed the correlation in the form of
equation:
46
E o 51 32.5 log( a a )
Equation
5.23
where a
The average viscosity can be found by using equation below where T is the average
temperature.
1
1
T VISB
log VISA
Equation 5.24
where T
Tavg
(T at top + T at bottom)/2
(1.192+204.3)/2
375.9 K
Table 5.18: Viscosity for each component
47
Component
VIS A
VIS B
NH4NO3
NH3
H2O
0.7109
-0.1391
-0.8678
0.4628
-0.2470
-1.1067
mN
m2
0.0292
0.2732
0.1635
Mole fraction
0.5034
0.2597
0.2369
(avg)=
Molar viscosity
0.0147
0.0709
0.0387
0.0415
5.4.2.2.7
0.0415 mN/m2
36.7519 x 0.0415
1.5240
45.05 %
The actual number of stages, N is the number is stages required for the column. This
stage can be determined by:
NT
Eo
Equation 5.25
10 1
0.4505
N 19.98
N 20
5.4.2.2.8
stages
48
Feed point location is calculated using equation by Kirkbride (1944):
N
log r
Ns
B x f , HK
0.206 log
D x f , LK
x b , LK
x
d , HK
Equation 5.26
where
Nr
Ns
Xf,HK =
Xf,LK =
Xd,HK =
Xb,LK =
Therefore,
0.206 log
Ns
75 0.2597 0.0001
Nr
1.80
Ns
N r 1.80 N s
From the previous calculation, the number of stages excluding reboiler is 20. Hence,
N r N s 20
N s 20 N r
N s 20 1.8 N s
N s 7.14
Ns 8
; feed enters at stage number 8.
49
Distillate
Bottom
(kgmol/hr
xf
xd
145.4500
0.5034
0.0075
NH3
75.0530
0.2597
74.9850
H2O
68.4480
0.2369
0.0075
Total
288.9510
1.0000
75.0000
(kgmol/hr
xb
0.000
1
0.999
8
0.000
1
1.000
0
145.4499
0.0553
68.4448
213.9500
0.679
80.0
1720.0
8
0.000
5
17.0
3
0.319
3
18.0
9
1.000
NH4NO3
NH3
H2O
RMM
Top
0.0080
17.0266
0.0018
Bottom
54.4205
0.0044
5.7584
V(kg/m3)
Top
Bottom
0.0016
7.2258
3.4057
0.0006
0.0004
0.7646
( x MW )
(kg/m3)
NH4NO3
Component
(kgmol/hr
MW
616.07
997.99
50
Liquid density at distillate;
V STP
TOP PSTP
0.008
273K
4.5bar 17.0266
273K
4.5bar
3
3
274.192 K 1bar
22.4kg / m 274.192 K 1bar 22.4kg / m
0.0018
273K
4.5bar
3
22.4kg / m 274.192 K 1bar
3.41kg / m 3
All calculated data is tabulate in Table 5.21.
Table 5.21: Liquid and vapor density at distillate and bottom
Reflux ratio, R = 0.16
= 0.16 x 0.35
= 0.06 kg/s
= 0.35 + 0.06
= 0.41 kg/s
= 0.06 + 3.93
51
= 3.99 kg/s
Vapor mass flow rate, Vn = Ln - B
= 3.99 3.58
= 0.41 kg/s
5.4.2.3.1
V
L
Lm
Vm
Top liquid-vapor flow factor, FLV =
0.06
0.41
3.41
616.22
=
=
0.01
Ln
Vn
Bottom liquid-vapor flow factor, FLV
V
L
3.99
7.99
0.41 1488.74
=
=
0.719
0.078
Bottom K1
0.037
52
0.032 N/m
0.700 N/m
2
Top K (correction)
0.02 K1
2
=
=
0.032
0.02 0.01
0.086
2
Bottom K (correction)
=
=
0.02 K1
0 .7
0.02
0.719
0.075
53
K1
Top flooding velocity, uf
L V
V
0.086
616.22 3.41
3.41
=
=
1.15 m/s
K1
Bottom flooding velocity, uf
L V
V
0.075
1488.74 7.99
7.99
=
=
1.03 m/s
Bottom v
0.80 x uf
0.80 x 1.15
0.92 m/s
0.80 x uf
0.80 x 1.03
0.82 m/s
Bottom
Vm / V
0.41 / 3.41
0.119 m3/s
Vn / V
0.41 / 7.99
0.051 m3/s
54
Top
Bottom
0.119 / 0.92
0.13 m2
0.051 / 0.82
0.062 m2
Bottom
0.13 / 0.81
0.16 m2
0.062 / 0.81
0.076 m2
Column diameter
Top
=
=
Bottom
=
=
0.160 4
0.452 m
0.076 4
0.312 m
Since the column diameter is smaller than 0.6m, packing should be considered
because plates would be difficult to install and expensive. For the design of packed
distillation columns, it is simpler to treat the separation as a staged process and use the
concept of the height of an equivalent equilibrium stage to convert the number of ideal
55
stages required to a height of packing. The method for estimating the number of ideal
stages from the previous calculation can then be applied to packed column.
b) Second trial: 1T Intalox sheet metal structured packing column internal
96
95
20
56
Since the data available for packing is in English unit, thus the packing distillation
column is calculated by using English unit, instead of SI unit. The properties from
calculation and HYSYS simulation are as follows:
Table 5.23: Properties from calculation and HYSYS
L (lb/s)
G (lb/s)
L/G
(cSt)
(cP)
(dyne/cm)
L (lb/ft3)
G(lb/ft3)
Vl (ft3/s)
Vg (ft3/s)
Top
0.12
0.90
0.1379
0.2592
0.1635
31.658
38.47
0.21
0.0032
4.2075
Bottom
8.79
0.90
9.8177
0.6159
0.7014
699.93
92.94
0.50
0.0946
1.7942
FLV
G
L
Equation 5.27
Pressure drop at flooding is calculated using equation;
PFl 0.115F p
0.7
PFl 0.9363in.H 2 O / ft
Capacity parameter, Co is determined from Figure 5.16:
57
FLOW PARAMETER
Figure 5.16: GPDC for structured packing only
The capacity parameter is then inserted into the following equation to calculate Cs;
C o C s F p0.5 0.05
Equation 5.28
Therefore,
Cs
Co
F 0.05
0.5
p
Packed column are usually design to 70-80 % margin from flooding velocity. This
practice provides sufficient margin to allow the uncertainties associated with the flood
point concept and prediction to avoid the flood point. For the calculation purpose, the
column will be designed for 75% of flood. Cs design = 0.75Cs,fl. The derating factor is
0.85.
Table 5.25: Diameter calculation due to flooding
Cs nonderated
derating factor
Top
0.339
0.85
Bottom
0.112
0.85
58
Cs derated
G/(L-G)
sqrt [G/(L-G)]
Us (ft/s)
CFS (vapor flow rate, (ft3/s)
At (ft2)
Dt (ft)
Dt (m)
0.288
0.006
0.075
3.865
4.208
1.089
1.177
0.359
0.095
0.005
0.073
1.292
1.794
1.388
1.330
0.405
G
L G
Cs us
Equation 5.29
AT
CFS
us
Equation 5.30
Diameter calculation due to maximum pressure drop criterion;
DT
4 AT
Equation 5.31
Maximum pressure drops, P (in. H2O/ft) recommended for packed column
for atmospheric and low-to-medium pressure is between 0.5 and 1.0.
Fp (ft )
(cSt)
Pmax (in H2O/ft)
Co
Cs, max
G/(L-G)
sqrt [G/(L-G)]
Us, max (ft/s)
Top
20
0.2592
1.000
1.94
0.464
0.006
0.075
6.224
Bottom
20
0.6159
1.000
0.66
0.151
0.005
0.073
2.058
59
CFS (ft3/s)
4.208
2
0.676
At (ft )
0.928
Dt (ft)
0.283
Dt (m)
The diameter is taken from the largest one, which
1.794
0.872
1.054
0.321
is 1.177 ft, and then round
of
equivalent
theoretical
plate
Top
1.00
1.50
18
1.77
1.50
12
18
Bottom
1.00
1.50
18
1.77
1.50
8
12
(HETP)
is
determined
from
Method
Distillation
Vacuum Distillation
Absorption/Stripping
HETP expressed
Packing
as ft (meters)
Size (in)
1.0
1.5
2.0
1.5 (0.46)
2.2 (0.67)
3.0 (0.91)
1.0
2.0 (0.67)
1.5
2.0
All Sizes
2.7 (0.82)
3.5 (1.06)
6.0 (1.83)
60
CHEMICAL DESIGN SPECIFICATION SHEET
Identification:
Item: Distillation Column (Recovery Column)
Item Code: T-101
No. Required: 1
Vertical
Feed location
Stage 8
Material of
Stainless steel
HETP
0.4572 m
construction
1T Intalox
Column Diameter
0.4572 m
Packing
Structured
Column Height
9.144 m
Packing
1.77 m2
20
Area
0.16
Top: 12
Reflux Ratio
Bottom: 8
H/D ratio
20
Number of Stages
3.93
Distillate flowrate
0.35
Bottom flowrate
3.58
315 m2/m3
Voidage
95 %
Size
2.54 cm
Packing factor
66 m-1
Flooding criteria
Flooding %
75
Pressure drop
78.3 mm H2O/m
Derating factor
0.85
Superficial velocity
61
Pressure drop
83.3 mm H2O/m
Superficial velocity
5.5
5.5.1
Introduction
Chemical Design
62
There are several steps that can be followed in designing the distillation column, (Sinnot
and Towler, 2009):
1.
2.
3.
4.
5.
6.
7.
63
Table 5.30: Summary of inlet and outlet composition
Component
Feed
Molar Flow
Mole
Rate
Fraction
(Kmol/hr)
NH4NO2
HNO3
NH3
H2O
Total
145.4513
0.0008
0.0485
68.4480
213.9486
Assumption:
Product
0.6798
0.0000
0.0002
0.3199
1.0000
Top
Molar Flow
Bottom
Molar Flow
Mole
Mole
Rate
Fraction
Rate
Fraction
(Kmol/hr)
0.0085
0.0008
0.0485
41.5193
41.5771
0.0002
0.0000
0.0012
0.9986
1.0000
(Kmol/hr)
145.4428
0.0000
0.0000
26.9287
172.3715
0.8438
0.0000
0.0000
0.1562
1.0000
If the presence of the other components does not significantly affect the
volatility of the key components, the keys can be treated as a pseudo-binary. Thus, for
this distillation column, pseudo-binary system will be used. Since the nitric acid and
ammonia content are too small which is less than 1%, all calculation will be based on
binary system calculations. Since the calculation is based on pseudo-binary system, the
mole faction will have to be recalculated. The new mole fraction is shown in table
below:
Table 5.31: Binary mol fraction and mol flow rate of inlet and outlet composition
Feed
Componen
t
Product
Molar
Mole
Flow
Fraction
Rate
145.4513
68.4480
213.8993
Molar
Mole
Flow
Fraction
Rate
(Kmol/hr)
NH4NO2
H2O
Total
Top
0.6800
0.3200
1.0000
(Kmol/hr)
0.0085
41.5193
41.5278
Bottom
Molar
Mole
Flow
Fraction
Rate
0.0002
0.9998
1.0000
(Kmol/hr)
145.4428
26.9287
172.3715
0.8438
0.1562
1.0000
Besides that, there are a few other assumptions can be made for this distillation column
design (Couper, 2005):
i.
ii.
iii.
The position of the interface can be controlled with or without the use of
instruments, by use of a siphon take off for the heavy liquid
iv.
64
Table 5.32: Temperature and pressure at feed, top and bottom distillation column
Feed
100
530
Temperature (c)
Pressure (kPa)
Top
141.1
400
Bottom
227.7
520
yi
kixi
= 1.0
Dew point
xi
yi/ki
= 1.0
ln P0= A
B
+ D ln ( T ) + E T F
T +C
Equation 5.32
K=
P0
PT
Equation 5.33
65
Compone
-2.711E+1
1.697E-17
0
6.593E+1 -7.228E+3
-7.177
0
1.632E+2 -1.008E+4
-2.277E+1
0
5.966E+1 -4.262E+3
-6.905
Table 5.33: Antoine Constant
4.031E-6
2.729E-5
1.002E-5
2
2
2
nt
NH4NO2
H2O
HNO3
NH3
2.199E+2 -2.316E+4
Xb
0.8438
0.1562
221.8597438 C
ln P
P(kPa)
5.14315E+00 171.2549828
7.78488E+00 2403.984301
495.0097438 K
K
K*Xb
0.329336505 0.277894143
4.623046733
0.7221199
TOTAL 1.000014043
Yb
0.0002
0.9998
143.6425413 C
ln P
P(kPa)
8.66005E-01
1
5.99168E+00 400.0867244
416.7925413 K
K
K*Yb
0.0025
0.0000005
1.000216811 1.000016768
TOTAL 1.000017268
199.1414003 C
X
ln P
0.68 4.10523E+00
0.32 7.33114E+00
P(kPa)
60.65658132
1527.125937
472.2914003 K
K
K*X
0.11444638 0.077823538
2.881369692 0.922038301
TOTAL 0.99986184
Temperature dew point and bubble point are calculated by using goal and seek
(Microsoft Excel)
66
It is in need to identify the light and heavy key to determine average relative volatility.
Water is needed to recover much at distillate; therefore it is a light key Average relative
volatility, a can be determined by knowing top and bottom column temperature.
K LK
K HK
Equation 5.34
Where;
KLK
KHK
LK
water, H2O
HK
And
For this case, the light component is water and heavy component is ammonium nitrate.
Table 5.37: The relative volatility for component
Feed
Top
Bottom
Component
NH4NO2
H2O
NH4NO2
H2O
NH4NO2
H2O
X
0.68
0.32
0.0002
0.9998
0.8438
0.1562
K
0.11444638
2.88136969
0.0025
1.00021681
0.32933651
4.62304673
Sample calculation:
At the top
KHK
0.0025
KLK
1.00021681
,T
At the bottom
1.00021681
0.0025
400.086724
1
25.176591
1
400.086724
1
14.0374561
67
KHK
0.32933651
KLK
4.62304673
,B
4.62304673
0.32933651
14.0374561
LK , AVG = T B
Equation
5.35
x HK
x LK b
x LK
x HK d
log
N m=
Equation 5.36
0.9998 0.8438
][
]
0.0002 0.1562
log 74.9413092
log [
N m=
N T =2(N m )
Equation 5.37
= 2(3)
=6
0.68
Water
0.32
The overall column efficiency is correlated with the product of the relative volatility of the
light key component and the molar average viscosity of the feed, estimated at the
average column temperatures. The Cornells correlation is mainly based on data
obtained with hydrocarbon system, but also includes some values for water-alcohol
mixtures as well. The method only considered the viscosity and volatility of each
component and does not take into account the plate design parameters.
0.25
0.5
Eo =
Equation
5.38
Where,
0.1445 mNs/m2
2. For bottom,
0.7783 mNs/m2
0.1445 + 0.7783
2
0.4614 mNs/m2
a=
74.9410392
0.5
E O=
= 20.62 %
= 0.2062
To get the real number of stages, the efficiency of the process must be considered and
the efficiency is calculated based on the equation by OConnells (J. Douglous, 1988)
N=
NT
EO
6
0.2062
= 29.09 30 stages
[( )( )( ) ]
[ ]
N
B
log r =0.206 log
Ns
D
x f , HK
x f , LK
x b , LK
x d ,HK
Equation 5.39
Where,
Nr
Ns
xf,HK
xf,LK
xd,HK
xb,LK
B
D
=
=
=
=
=
=
=
condenser
Number of stages below the feed, including the reboiler
Concentration of the heavy key in the feed
Concentration of the light key in the feed
Concentration of the heavy key in the top product
Concentration of the light key in the bottom product
Molar flow of bottom product
Molar flow of top product
[( )( )( ) ]
[ ]
N
B
log r =0.206 log
Ns
D
log
x f , HK
x f , LK
[ ]
x b , LK
x d ,HK
[(
Nr
172.3715
=0.206 log
Ns
41.5278
Equation 5.40
0.68 0.1562
0.32 0.0002
)( )(
)]
2
[ ]
Nr
=24.3524
Ns
24.3524 N + N
s
s
Ns
Nr
Feed point
30
=
=
=
1.1833
28.8267
2 from bottom
Ammonium Nitrate
Water
5.5.2.7.2
NH4NO2
H2O
Total
Weight
(MW)
80.052
18.015
98.067
Liquid
Feed,x
Top, xD
xW
0.6800
0.3200
1.0000
0.0002
0.9998
1.0000
RMM =
RMM feed
0.6800(80.052) + 0.3200(18.015)
60.2002 kg/kmol
=
=
0.0002(80.052) + 0.9998(18.015)
18.0274 kg/kmol
0.8438(80.052) + 0.1562(18.015)
Bottom,
0.8438
0.1562
1.0000
Density
(kg/m3)
1725
1000
=
5.5.2.7.3
70.3618 kg/kmol
Pressure Drop
The pressure drop over the plate is an important design consideration. There are two
main sources of pressure loss:
1. Vapour flow through the holes (an orifice loss)
2. Static head of liquid on the plate
It is convenient to express the pressure drops in term of milimetres of liquid. In pressure
units:
Pt =9.81 103 ht L
Equation 5.41
Pt
ht
Pt =9.81 103 ht L
Top pressure, 5.132 atm
= 520 kPa
a. Bottom product
Liquid density, L,w
xB,i i
0.8438(1725) + 0.1562(1000)
1611.755 kg/m3
VMW TSTP P OP
K
atm
3
500.85
1
22.4 m /lmol
STP
OP
STP
8.7916 kg/m3
xB,i i
0.0002(1725) + 0.9998(1000)
1000.145 kg/m3
b. Top product
Liquid density, L,T
VMW TSTP P OP
K
atm
3
414.25
1
22.4 m /lmol
STP
OP
STP
2.0949 kg/m3
5.5.2.7.5
Summary
Table 5.39: Summary vapour and liquid flow
Vapour and Liquid Flow
F
213.9486 kmol/hr
41.5771 kmol/hr
172.3715 kmol/hr
Enriching Section
Ln
192.5537 kmol/hr
Vn
234.1308 kmol/hr
Stripping Section
Lm(Lw)
406.5023 kmol/hr
Vm(Vw)
234.1308 kmol/hr
Top
Bottom
Liquid
1000.145
1611.755
Vapour
2.0949
2.0949
Column Diameter
The principal factor that determines the column diameter is the vapour flow rate. The
vapour velocity must be below that which caused excessive liquid entrainment or a
high-pressure drop. The equation given below, which is based on the well-known
Souders and Brown equation (Duncan and Reimer, 1998), can be used to estimate the
maximum allowable superficial vapour velocity, and hence the column area and
diameter.
2
t
( L V )
V
1 /2
Equation 5.42
In order to use the given equation, the plate spacing has to be specified. Plate spacing
0.55 m is chosen.
Thus,
2
t
( L V )
V
1 /2
( 1611.7552.0949 )
uv =( 0.171(0.55) +0.27 (0.55)0.047 )
2.0949
2
= 0.0497725 27.7195
= 1.37966 m/s
With the value gained, the column diameter can be calculated using:
Dc =
4V w
v uv
V w=
= 4.576075 kg/s
Therefore,
Dc=
4 4.576075 kg/ s
2.0949 kg /m3 1.37966 m/ s
Dc = 1.419814 m
1 /2
Approximate to 1.5 m.
5.5.2.8.2
Column Area
The column area can be calculated from the calculation of internal diameter
A c=
D 2c
4
1.5
A c =
A c =1.767146 m2
5.5.2.8.3
Column Diameter
U f =Ki
L V
V
Equation 5.43
Where,
Uf
Ki
=
=
Flooding vapour velocity, m/s, based on the net column cross-sectional area.
A constant obtain from (Coulson and Richardson, 2009)
The liquid-vapour flow factor, Fv (Coulson and Richardson, 2009) is given by:
F LV =
LW
VW
LW
VW
V
L
= Liquid mass flow rate, kg/s
= Vapour mass flow rate, kg/s
Equation 5.44
Where:
F LV , bottom=
406.5023 8.7916
234.1308 1611.755
= 0.1282
F LV , bottom=
192.5537 2.0949
234.1308 1000.145
= 0.03764
Take plate spacing as 0.55 m. (Plate spacing is the important for determined the overall
height of column. Plates spacing from 0.15 m to 1 m are normally used. The spacing
chosen depends on the column diameter and operating conditions. For columns above
1 m diameter, plate spacing 0.3 to 0.6 m will normally be used (Sinnot and Towler,
2009).
0.0625
Top Ki
1.1 10-1
Hence:
U f =Ki
L V
V
Equation 5.45
Bottom
U f =0.0625
1611.7558.7916
8.7916
= 0.8439 m/s
Top
U f =1.1 101
1000.1452.0949
2.0949
= 0.4009 m/s
For design, a value of 80 to 85 percent of the flooding velocity should be used.
Bottom
Uf
0.7173 m/s
Top
5.5.2.8.4
Uf
2.0408 m/s
Bottom
Top
234.1308 (18.0274)
1
2.0949
3600
0.5597 m3/s
Net Area, An
Bottom
0.5205 m3/s
=
5.5.2.8.5
234.1308 (70.3618)
1
8.7916
3600
m
( 3/s )
0.52051
0.7173( m/ s)
Top
V m( RMM )
1
v
3600
0.7257 m2
m
0.5597( 3/ s)
2.0408(m/s)
0.2743 m2
Bottom
Top
0.7257
0.88
0.8247 m2
0.2743
0.88
0.3117 m2
Column Diameter
Bottom
Top
0.9612 m
=
=
4 0.7257
4 0.2743
0.59097 m
L w RMM bottom
3600 L
406.5023 kg/ s 70.3618 kg /kmol
3
3600 s 1611.755 kg /m
The choice of plate type will depend on the liquid flow rate and column diameter.
Table 5.41: Advantages and disadvantages of different type of plates (Sinnot and
Towler, 2009)
Type of plate
Advantages
The cheapest among the
Disadvantages
others
Sieve Plate
(Perforated
Simplest type
plate
Low flow rate of liquid
Plate)
Bubble Cap
Plate
Expensive
of liquid maintained on
Valve plate
(Floating Cap
Plate)
plates
In this project, a sieve plate has been selected due to various factors such as cost,
capacity, operating range, efficiency and pressure drop.
Figure 5.18: Normal operation of sieve plate (Sinnot and Towler, 2009)
5.5.2.10
Column diameter, Dc
Column area, Ac
Down corner area, Ad
Net area, An
Active area, Aa
Hole area, Ah
5.5.2.11
=
=
=
=
=
=
=
=
=
=
=
1.5 m
1.767146 m2
0.12 1.767146 m2 (at 12%)
0.2121 m2
Ac- Ad
1.767146 m2 0.2121 m2
1.5551 m2
Ac- 2Ad
1.767146 m2 2(0.2121 m2)
1.342946 m2
0.08 m2 (take 6% of Aa as second trial after 10%)
Weir Length
Ad
0.2121
100 =
100 =12
Ac
1.767146
From figure 11.39: Relation Between Downcomer Area And Weir Length (Coulson and
Richardson, 2009)
Iw
=
Dc
0.76
Iw =
0.76 1.5 m
=
Weir height, hw
Hole diameter, dh
Plate thickness
1.14 m
=
=
=
50mm
5mm
5mm
Take
Area of 1 hole,
Alh
d 2h
4
0.005
Equation 5.46
1.963
105 m
N h=
Ah
Alh
Equation 5.47
0.08
5
1.963 10
4075 holes
The column height will be calculated based on the equation given below. The equation
determines the height of the column without taking the skirt or any support into
consideration. It is determined based on the condition inside the column.
5.5.2.12
Column Height
17.195 m
Approximate = 19 m
Value
1.5 m
No. of Plates
30
Plate Spacing
0.55 m
Plate thickness
5 mm
19 m
0.2121 m2
1.767146 m2
1.5551 m2
1.342946 m2
0.08 m2
4074
Weir Length
1.14 m
Weir Height
0.05 m(standard)
5.5.2.13
LW (RMM )
3600 S
406.5023 (70.3618 )
3600 S
7.9451 kg/s
5.5615 kg/s
The height of the liquid crest over the weir can be estimated using the Francis weir
formula. For a segmental down corner this can be written as:
how =750
Lw
l (l w )
2 /3
( )
Where,
lw
Lw
= Weir length
= Liquid flow rate, kg/s
l = Liquid density
Maximum ,h ow =750
7.9451 kg /s
1611.75 kg /m3 1.14 m
2 /3
=19.906 mm liquid
5.5615 kg /s
Minimum , how =750
1611.75 kg /m3 1.14 m
= 15.694 mm liquid
At minimum rate, clear liquid depth,
2/ 3
5.5.2.14
Weeping Point
Liquid flow through sieve-plate perforations occurs when the gas pressure drop through
the perforations is not sufficient to create bubble surface and support the static head of
froth above the perforations. Weeping can be harmful in that liquid tends to short-circuit
the primary contacting zones. Minimum vapour velocity through the holes based on the
holes area can be calculated using Eduljee (1959) equation:
K 20.9(25.4d h)
U h (min)=
Uh
dh
K2
=
=
=
Minimum vapour velocity through the holes based on the holes area
Hole diameter, mm
A constant, dependent on the depth of clear liquid on the plate.
Obtain from figure 11.37: Weep-point Correlation (Coulson &
Richardson, 2005)
K 20.9(25.4d h)
U h (min)=
Where,
1 /2
8.7916
30.40.9 (25.45)
4.06757 m/s
0.7 (0.52051 m / s)
0.08
=
4.5545 m/s
Uh
5.5.2.15
[ ]
U
hd =51 h
Co
v
L
Equation 5.48
Uh
Co
Uh
=
=
=
Where,
volumetric flowrate
hole area , A h
Uh
0.52051m 3 /s
2
0.08 m
6.506375 m/s
When:
plate thickness 5 mm
=
=1
hole diameter 5 mm
And:
2
Ah
0.08 m
=
100
A a 1.342946 m2
=6%
So, orifice coefficient value can be obtained from figure 11.42: Discharge Coefficient
Sieve Plates (Coulson & Richardson, 2009)
Co
0.81
6.506375 8.7916
hd =51
0.812
1611.755
=17.86097 mm liquid
5.5.2.15.2
Residual Head
hr =
12.5 103
L
hr =
12.5 10
1611.755
Equation 5.49
= 7.75552 mm liquid
5.5.2.15.3
ht =hd + ( h w + how ) + hr
5.5.2.15.4
hap=hw 10 mm
hap=50 mm10 mm
= 40 mm
Where
hap
is the height of the bottom edge of the apron above the plate.
A ap=hap (I w )
= 4010-3 m (1.14 m)
= 0.0456 m2 0.05 m2
Where
As this is less that Ad= 0.965 m2, this equation can be used to calculate the head loss in
downcomer.
hdc =166
[ ]
Lw
L Am
Equation 5.50
Where,
hd
c
Lw
Am
area
under
down
comer,
hdc =166
7.9451
1611.755 0.05
= 1.6135
= 2 mm
Back-up in the down comer, (hb),
Equation 5.51
<
0.159m
<
0.159m
<
0.159m
<
0.3 m
5.5.2.15.5
Sufficient residence time must be allowed in the downcomer for the entrained vapour to
disengange from the liquid stream; to prevent heavily aerated liquid being carried
under the downcomer. At time of at least 3 seconds is recommended. (Couper, 2005)
Check residence time
t r=
A d hb L
Lw
Equation 5.52
= 6.84128 s
3 s (satisfactory)
5.5.2.15.6
Check Entrainment
Entrainment can be estimated from the correlation given by Fair (1961). The
percentage flooding is given by:
flooding=
U n actual velocity
(based on net area)
Uf
Equation
5.53
U n=
Uf
An
0.5205
1.5551
0.3347 m/s
flooding=
0.3347
100
0.7173
= 46.66 %
From figure 11.36: Entrainment Correlation for Sieve Plates (Coulson & Richardsons,
Chemical Engineering Design, 2009)
Fractional entrainment,
= 0.03
5.5.2.15.7
Perforated Area
At=
Iw
Dc
Equation 5.54
1.14 m
1.5 m
= 0.76
Therefore,
99
5.5.2.15.8
(180 99)
81
( Dc 0.05)
81
180
(1.50.05)
81
180
1.1745m
5.5.2.15.9
(5010-3) m (1.1745) m
0.058725 m2
5.5.2.15.10
0.113 m2
5.5.2.15.11
Ap
=
=
=
Ah
0.08 m2
=
A p 1.171221 m2
= 0.0683
From figure 11.41: Relation between hole area and pitch (Coulson & Richardsons,
Chemical Engineering Design, 2009,)
5.5.2.15.12
Trial Layout
50 mm
1.14 m
50 mm
1.5 m
5.5.3
Value
Column diameter, Dc
1.5 m
Plate spacing, ts
0.55 m
Downcomer area, Ad
0.2121 m2
Downcomer Material
Plate material
Plate Thickness t
0.005 m
Column Area, Ac
1.7671 m2
Net Area, An
1.5551 m2
1.1712 m2
Active area, Aa
1.3429 m2
0.08 m2
Weir length
1.14 m
Weir height
0.005 m
Hole diameter
0.005 m
Number of holes
4075
Flooding %
47 %
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