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CHAPTER 5

CHEMICAL DESIGN

5.1

PIPE REACTOR

5.1.1

Introduction

The reactor is the heart of most processes; developments in process technology


often centre on improvements in the design and operation of the reactor.
Subsequent stages in the chemical process are usually concerned with the
separation of various chemicals from the desired product, followed by the final
purification stages.
The treatment of reactor design in this section will be restricted to a discussion of
the selection of the appropriate reactor type for a particular process, and an outline
of the steps to be followed in the design of a reactor. The design of an industrial
chemical reactor must satisfy the following requirements:
1. The chemical factors: the kinetics of the reaction. The design must provide
sufficient residence time for the desired reaction to proceed to the required
degree of conversion.
2. The mass transfer factors: with heterogeneous reactions the reaction rate
may be controlled by the rates of diffusion of the reacting species; rather
than the chemical kinetics.
3. The heat transfer factors: the removal, or addition, of the heat of reaction.
4. The safety factors: the confinement of hazardous reactants and products,
and the control of the reaction and the process conditions.
The production of ammonium nitrate solution is carried out by a neutralization
process between nitric acid and ammonia in a pipe reactor. The pipe reactor or
turbular reactor is a length of pipe having a small diameter and containing no inside
stuffing.

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

CHEMICAL DESIGN FOR PIPE REACTOR

5.1.2.1 Chemical Reaction


Below is showed the main reaction between ammonia and nitric acid occurring in the
reactor to produce ammonium nitrate.

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

( )

where K is an equilibrium constant,


R is the gas constant
H is the heat of reaction.
Arrhenius, 1889 from Levenspiel (1999) proposed a similar expression for the rate
constant k

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

Where A is a constant referred to as the pre-exponential factor. Together, EA and A are


called the Arrhenius parameters. Equations (5.2) to (5.4) are all forms of the Arrhenius
equation. This equation is usefulness to represent experimental results for the
dependence of kA on T.
In this ammonium nitrate production, the equilibrium constant for the reaction can be
calculated as shown below.
Inlet temperature : 86.04 oC
Outlet temperature : 180 oC
Reaction temperature : 180 oC (453.15 K)
From HYSYS, the value of EA is 3.2744 x 10-2 and value for A is 1.327 are inserted in
the equation of 5.4.

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

5.1.2.3 Step Taken For Chemical Design of Reactor


Below are the steps taken to determine chemical design specification for designing this
pipe reactor:
1) Determination of specific reaction rate
2) Calculation of residence time by using Simpsons Rule equation.
3) Determination of working volume of reaction and size of reactor

Start

Determination of specific rate of reaction, interpretation of the rate

Determination of residence time by using Simpsons Rule

Determination of volume of reactor

End

Figure 5.1: Algorithm for chemical design of reactor


5.1.2.4 Analysis of the Reactor Inlet and Effluent
Analysis of the reactor inlet and effluent is important to determine the volume of the
reactor. It also will give more of the properties needed for the reactor design, the
mechanical strength needed for the reactor, also type of reactor suitable to be used.
From the Design Project 1 (DP1), the material balance for the reactor as below:
Table 5.1: Analysis data for reactor inlet and outlet

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

Total flowrate (kg/hr) = 3782.5 + 9165 + 1233


= 14180.5 kg/ hr
Density mixture (kg/m3) =

i i

Where is mass fraction and is density of each material


Density mixture (kg/m3) = 1235.76 kg/m3

14180.5
Flowrate in m3/hr =

( hkgr )

kg
1235.76 3
m

( )

=11.48 m3/hr

Initial Concentration for each component is:


Nitric Acid

: 12.67 kmol/m3

8
Ammonia,

: 19.35 kmol/m3

Water

: 5.96 kmol/m3

Ammonium nitrate : 0.000 kmol/m3


5.1.2.5

Determination Rate of Reaction

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

Where n and m are the order of kinetic reaction

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

5.1.2.6 Interpretation of the Reaction Rates


0.4
r=1.33 C 0.81
HN O C N H
3

Equation 5.7

C HNO3 =C HNO3 O C HNO3 O X HNO3


Equation 5.8

C NH3=C NH3 OC HNO3 O X HNO3


Equation 5.9

Substituting equation 5.8 and 5.9 into 5.7, therefore:

C HNO3 O C HNO 3O X HNO 3

C NH3 O C HNO3 O X HNO3

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

C HNO3 O C HNO3O X HNO3

C NH3 O C HNO3 O X HNO3

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

5.1.2.7 Calculation of Residence Time, of reactor


The values of reaction rates and graph of reaction rate versus conversion below is
calculated by using Microsoft excel.
Table 5.2: Data for Calculated Residence Time, s
XHNO3
0.00
0.05
0.10

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

CHNO3/rNH4NO3 versus Conversion, XHNO3


25.00000
20.00000
15.00000
CHNO3/rNH4NO3 10.00000
5.00000
0.00000
0

0.2 0.4 0.6 0.8

1.2

XHNO3

Figure 5.2: Graph of CHNO3/rNH4NO3 versus Conversion, XHNO


To evaluate the area under graph, Simpsons Rule is used.
0.99

=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=

29.14 145.45 kmol


hr

12.67
hr
3600 s

V =0.093 m

Height and radius of the vessel


Consider allowance for the reactor, therefore the volume for the pipe reactor is 0.0795
m3 .Volume of the cylinder, can be calculated from equation:
2

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.

Figure 5.3: Illustrate diagram for reactor sizing

5.1.2.9 Flow In and Out of the Reactor


Ammonia will be introduced into the pipe reactor along the horizontal lines. For nitric
acid, the reactant will flow into the pipe reactor at the right angles or from above of the
reactor. The product stream will flow directly into the separator for separation process.
The temperature and pressure at the feed are at 86 oC and 600kPa respectively while
for the outlet stream, the pressure and temperature are 180oC and 540kPa.

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Nitric
Acid
Product to
separator

Ammonia

Figure 5.4: Diagram for Pipe Reactor


5.2

GAS LIQUID SEPARATOR (V-101)

5.2.1

Chemical Design of Gas Liquid Separator

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

Figure 5.5: Stream Involve in 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.

Figure 5.6: A vertical gas liquid 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

Diameter and Length of Gas Liquid Separator

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

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Figure 5.7: Graph shown the value of Kv


From graph, Kv = 0.3ft/s = 0.3ft/s.1m/3.28ft = 0.09 m/s
Uvapor max = 0.09[(1225-2.7849)/2.7849]0.5
= 1.88543m/s
Minimum Cross sectional area for vapor, Av = Vmix/Uv =

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

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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.

Figure 5.8: Counter-current flow arrangement


Parallel flow also known as co-current flow. In parallel-flow heat exchangers, the two
fluids enter the exchanger at the same end, and travel in parallel to one another to the

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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.

Figure 5.9: Co-current or parallel flow arrangement


5.3.1.2 Types of Heat Exchanger
There are many types of heat exchanger in industry. The types chosen based on the
function of the heat exchanger itself. Heat exchangers are classified according to
transfer processes into indirect and direct contact types. For an indirect-contact heat
exchanger, the fluid streams remain separate and the heat transfers continuously
through an impervious dividing wall or into and out of the wall or into transient manner.
Direct-contact heat exchanger is when heat transfers continuously from the hot fluid to
the cold liquid through a dividing wall not direct mixing of the fluids.
Choosing the right heat exchanger requires knowledge of different type of heat
exchanger as well as well as the environment in which the heat exchanger will operate.
With sufficient knowledge of heat exchanger types and operating requirements, the best
selection can be made in optimizing the process. In selecting a suitable heat exchanger
for constructing the cooler, several exchanger types were considered. Below, in Table
3.1 are list of types and functions of each heat exchanger.
Table 5.3: Types and Functions of Heat Exchanger in Industry

21

No

Types

Functions

.
1.
Double

pipe

heat

The simplest type. Use for heating and

exchanger

cooling.

Shell and tube heat

Used for all application.

2.
exchanger
3.
Plate exchanger

Use for heating and cooling.

Plate-fin exchanger

Use for heating and cooling.

Spiral

Use for heating and cooling.

4.
5.
heat

exchanger
6.
Air cooled

Cooler and condenser.

Direct contact

Cooling and quenching.

Agitated vessels

Use for heating and cooling.

Fired heaters

Use for heating and cooling.

7.
8.
9.

5.3.1.3 Selections of Heat Exchanger


Typically in the manufacturing industry, several different types of heat exchangers are
used for just the one process or system to derive the final product. In order to select an
appropriate heat exchanger, one would firstly consider the design limitations for each
heat exchanger type. Although cost is often the first criterion evaluated, there are
several other important selection criteria which include:

High/ Low pressure limits


Thermal Performance
Temperature ranges
Product Mix (liquid/liquid, particulates or high-solids liquid)
Pressure Drops across the exchanger
Fluid flow capacity
Clean-ability, maintenance and repair
Materials required for construction
Ability and ease of future expansion

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.

5.3.1.5 Problem Identification

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

Corrosive fluid will be in tube side

Fouling

Fluid that has the greatest tendency to foul on heat transfer


surface will be allocated in the tube side.

Fluid

Very hot or very cold liquid is place in tube side to avoid the

temperatur

use of costlier material for shell. At moderate temperature,

hotter fluid is better passed through tubes. If placed on shell


side more insulation required not only to reduce the heat loss
but also the safety purpose.

Operating

High pressure stream should be place on tube side as high

pressure

pressure tube is cheaper than high pressure shell.

Fluid

flow Fluid which provides very low value of Reynolds number

rate

and

viscosity

should be placed on shell side as the dependency of shell side


heat transfer rate coefficient on Reynolds number is less as
compared to the same of tube side heat transfer coefficient.
(Sinnott R. K, 2005)

5.3.2

Chemical Design

The design procedure is as shown below:


1. Define the duty: heat transfer rate, fluids flow rate and temperature

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

5.3.2.2 Design of Shell and Tube Heat Exchanger

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

One shell and two tubes


Fixed and Tube
Horizontal
Horizontal
1
1
Mixture of Ammonium Nitrate,
Ammonia, Nitric Acid and water
1
1
Cooling water
1109.6

For Tube side, Q = Wmixture Cp t


= (12880/3600) x (2.9737) x (204.3-100)
= 1109.6 kJ/s
For Shell side, Wwater = Q/ (Cp x T)
= [1109.6/ (4.2 x (74-25))]
= 5.39 kg/s
= 19409.91 kg/hr
5.3.2.4 Overall Coefficient
From Table 12.1 ( R Sinnott, 2009), using typical overal coefficient for shell and tube
heat exchanger.
Hot fluid = Organic solvent
Cold fluid = water
Therefore the overall coefficient = 250 750 W/m2oC.
We take the maximum value of the overall coefficient of the heat exchanger,
Uo = 750 W/m2oC.
5.3.2.5 Heat Transfer Area

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

Where, T1 = Inlet shell side fluid temperature


T2 = Outlet shell side fluid temperature
t1 = Inlet tube side fluid temperature
t2 = Outlet tube side fluid temperature
From equation, Tlm = [(25-100)-(74-204.3)] / ln [(25-100)/(74-204.3)]
= 100.12 oC
True temperature difference is given by; Tm = Ft x Tlm
Where,
Ft = Temperature correction factor
R = (T1-T2)/(t2-t1) = (25-74)/(100-204.3) = 0.47
S = (t2-t1)/(T1-t1) = (100-204.3)/(25-204.3) = 0.58
From Figure 12.19 ( R Sinnott, 2009) the value of Ft = 0.91.
Tm = Ft x Tlm
= 0.91 x 100.12
= 91.11 oC
The heat transfer area of heat exchanger, Ao = Q/(Uo x Tm)
= (1109.6 x 1000) / (750 x 91.11)
= 16.24 m2

28

5.3.2.6 Tube Dimensions


From Table A.5-2 (C.J Geankoplis, 2003), we take standard pipe of:
Table 5.9: Tube dimension
Particulars
Tube length, L
Outer diameter, OD
Inside diameter, ID
Birmingham wire gage
(BWG)
Area of the tube, At = LOD

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.

Nt = Ao/At = (16.24/0.2992) = 54.28


Therefore, Nt = 58

Tube cross sectional area, Atc = (OD/2)2


= (0.01905/2)2
= 2.85 x 10-4 m2
Area per pass = 58 tubes x 2.85 x 10-4
= 0.0157 m2

29

Volumetric flow, Vt = Wmixture/mixture


= (12880/3600) / 1239
= 0.003 m3/s

Tube side velocity, Ut = Vt/Area per pass


= 0.003/0.0157
= 0.19 m/s

Reynolds number, Re = (UtID)/viscosity


= (1239 x 0.19 x 0.01483)/ (0.8414/1000)
= 4149.19

Prandtl number, Pr = (Cpx viscosity)/Kf


= [(2.9737 x 1000) x (0.8414/1000)]/ 70.74
= 0.04
L/ID = 5/ 0.01483 = 337.15

From Figure 12.23 (R Sinnott, 2009), heat transfer factor, jh = 0.032

30
Nusselt number, Nu = jh x Re x (Pr)0.33
= 0.032 x 4149.19 x 0.04
= 5.31

Tube heat transfer coefficient, ht = Nu x (Kf/ID)


= 5.31 x (70.74/0.01483)
= 25329.02 W/m2oC

From Figure 12.24 ( R Sinnott, 2009), jf = 0.06

Pressure drop on tube side, Pt = 2 x 8 x jh (L/ID) x (Ut2/)


= 2 x 8 x 0.06 (337.15) x (1239 x 0.192/0.8414)
= 17205.6 N/m2

5.3.2.7 Bundle and Shell Diameter Calculation

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

Figure 5.10: Triangular pitch


The bundle diameter, Db = OD (Nt / K1) 1/n
= 0.01905 (55/0.249)1/2.207
= 0.2198 m
= 219.8 mm
From Figure 12.12 ( R Sinnott, 2009), for bundle diameter of o.2198m, bundle
clearence is 10.05mm.
Shell diameter, Ds = 0.2198 + 0.01005 = 0.23m
Baffle spacing, IB = 5
Ds/5 = 0.23/5 = 0.046m
Shell cross flow area, As =[( Pt ODtube) x Ds x (Ds/5)] / Pt
= [(0.0238 0.01905) x 0.23 x 0.046] / 0.0238
= 0.0021m2
Equivalent triangular pitch arrangement diameter,
De = (1.10/OD) x (Pt2 0.917 x OD2)
= (1.10/0.01905) x (0.02382 0.917 x 0.019052)
= 0.0135m
Volumetric flow rate on the shell side,

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

Heat Exchanger Specification


Cooler, E-106
To cool down process line from

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)

Cold Fluid Properties


Flowrates (kg/hr)
Inlet temperature (C)
Outlet temperature (C)
Heat transfer area, A (m2)
Number of tubes, Nt
Tube inside diameter, di (m)
Tube outside diameter, do (m)
Length of tube, L (m)
Bundle diameter, Db (m)
Shell diameter, Ds (m)
Tube side heat transfer

19409.91
25.0
74.0
16.24
58
0.01483
0.01905
5.0
219.8
0.23
25329.02

coefficient, (W/ m2C)


Shell side heat transfer

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

AMMONIA RECOVERY COLUMN

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

Figure 5.11: Continuous distillation column


5.4.1.2 Distillation in Packed Column
The type of internal used in ARC is packing. Packed column is classified where trays of
various designs are used to hold up the liquid to provide better contract between vapour
and liquid, hence better separation. Packed columns are often used for distillation when
the separation is relatively easy and the required column diameter is not very large.
They are generally less expensive than plate columns when the column diameter is
relatively snall and have a lower pressure drop.
5.4.1.2.1 Comparing Trays and Packings
Almost every separation can be performed either with trays or with packings. These
factors only represent economic pros and cons, and each may be overridden. A couple
of trays-versus-packing comparisons have appeared in the recent literature. These
comparisons emphasize capacity, efficiency, and costs.
Factors favoring packed-column:
a) Small-diameter columns
When column diameter is less than 3ft, it is difficult to access the column from
inside in order to install and maintain the trays, Cartridge trays are often

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.

5.4.1.3 Distillation Column Design Steps


The design of a distillation column can be divided into the following steps:
1.
2.
3.
4.

Specify the degree of separation required: set product specifications.


Select the operating conditions: batch or continuous; operating pressure.
Select the type of contacting device: plates or packing.
Determine the stage and reflux requirements: the number of equilibrium stages.

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

Chemical Design Of Ammonia Recovery Column

5.4.2.1 Design Data


The Ammonia Recovery Column is shown in Figure 5.12 below:

Figure 5.12: T-101 Ammonia Recovery Column


The design data for ARC presented in Table 4.1 for feed, distillate, and bottom stream.
Table 5.12 Flow rate inlet and outlet ARC
Feed
Component

Ammonia (NH3)

Product

Feed inlet

Distillate

Bottom

Stream 15

Stream 16

Stream 18

Molar flow rate


(kgmol/hr)

Molar flow rate


(kgmol/hr)

Molar flow rate


(kgmol/hr)

75.0530

0.0075

145.4499

39

Ammonium Nitrate (NH4NO3)

145.4500

74.9850

0.0553

Water (H2O)

68.4480

0.0075

68.4448

Total

288.9510

75.0000

213.9500

5.4.2.2 Determination of Plate Number


The main components in the feed to the ARC are ammonia, ammonium nitrate, and
water as listed in the previous table. Since the feed is a mixture of those three
components, the ARC is then considered as a multicomponent distillation column. The
separation between the top and bottom products of multicomponent system is usually
specified by setting limits on two key components, between which it is desired to make
the separation. The light key (KLK) will be the component that it is desired to keep out of
the bottom product (high volatility), and the heavy key (KHK) is the component to be kept
out of the top product (low volatility).
For ARC, the key components chose are:
a)
b)

KHK = Water (H2O)


KLK = Ammonia (NH3)

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

Determination of Bubble and Dew Point Temperature

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

For multicomponent mixtures, the temperature that satisfies these equation, at a


given system pressure, must be found by iteration.
The vapour pressure can be determined by using the Antoines equation as follows:

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.

With related at equilibrium, constant K,

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

Dew point temperature (top column)

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.

Operating P = 450 kPa

Dew point T = 369.6 K

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

Bubble point temperature (bottom column)


By using goal seek in the excel program, the value of the bubble point temperature is
470.8 K with the constant operating pressure is 520 kPa.

Operating P = 150 kPa

Bubble point T = 470.8 K

Table 5.15: Bubble point temperature


Component
NH4NO3
NH3
H2O
Total
5.4.2.2.2

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

Determination of Relative Volatility,

The determination of relative volatility, of the components can be determined as the


ratio between K values of light key component to heavy key component.

K LK
K HK

Equation 5.16
where KLK

KHK =

Light key component, NH3


Heavy key component, H2O

The equilibrium vaporization constant K is defined for a compound by:

Ki

yi
xi

Equation 5.17

42
Where yi

mole fraction of component i in the vapour phase

xi

mole fraction of component i in the liquid phase


Table 5.16: Relative volatily for each component

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

Determination of Number of Stages Using Fenske Equation

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

light key concentrations

xHK

heavy key concentrations

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

the relative volatility of component i with respect to some


reference component, usually heavy key

Rmin =

the minimum reflux ratio

xi, d

concentration of component i in the distillate at minimum reflux

the root of the equation, from the following equation:

i xi, f

1 q

Equation 5.21
where,
xi,f

concentration of component i in the feed at minimum reflux

44
q

depends on the condition of the feed

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

By using goal seek, = 1.8694 when

Table 5.16: Relative volatility at feed


Component

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

Table 5.17: Relative volatility at distillate


Component

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 / ( )]

From the previous equation,

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 =

light key component at top flow

xd,HK =

heavy key component at top flow

xf,LK =

light key component at feed flow

xf,HK =

heavy key component at feed flow

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 molar average liquid viscosity, mNs/m2

average relative volatility of the light key

Figure 5.13: Distillation column efficiencies (OConnell, 1946).


5.4.2.2.6

Viscosity at Average Temperature

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

From feed composition:

(0.0292 0.5034) (0.2732 0.2597) (0.1635 0.2369)


3
Molar average viscosity =
aa
Eo

5.4.2.2.7

0.0415 mN/m2

36.7519 x 0.0415

1.5240

51 32.5 log (1.5240)

45.05 %

The Actual Number of Stages

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

Determination of Feed-Point Location

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

number of stages above the feed, including any partial condenser

Ns

number of stages below feed, including the reboiler

Xf,HK =

concentration of the heavy key in the feed

Xf,LK =

concentration of the light key in the feed

Xd,HK =

concentration of the heavy key in the top product

Xb,LK =

concentration of the light key in the bottom product

Therefore,

214 0.2369 0.0003 2


Nr
log


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

5.4.2.3 Equipment Sizing of Ammonia Recovery Column


The following table shows the mole fraction, molecular weight, and liquid density for
each component.
Table 5.19: Mole fraction, molecular weight, and liquid density for each component
Feed
Componen
t

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

Table 5.20: RMM and vapor density for each component

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

Sample of calculation at distillate:


The relative molecular mass (RMM) in distillate;

( x MW )

(0.0001 80.05) (0.9998 17.03) (0.0001 18.00)


17.0364kg / mol

(kg/m3)

NH4NO3

Component

(kgmol/hr

MW

616.07
997.99

50
Liquid density at distillate;

(1720 0.0001) (616.07 0.9998) (997.99 0.0001)


616.22kg / m 3
Vapor density at distillate;

RMM T STP POP

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

Feed, F = 3.93 kg/s

Distillate, D = 0.35 kg/s

Bottom, B = 3.58 kg/s

L above feed = 616.22 kg/m3

V above feed = 3.41 kg/m3

L below feed = 1488.74 kg/m3

V below feed = 7.99 kg/m3

Mass balance on top distillation column


Liquid mass flow rate, Lm = R x D

= 0.16 x 0.35
= 0.06 kg/s

Vapor mass flow rate, Vm = D + Lm

= 0.35 + 0.06
= 0.41 kg/s

Mass balance on bottom distillation column


Liquid mass flow rate, Ln = (R x D) + F

= 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

Calculation for Column Diameter

a) First trial: sieve tray column internal


Try tray spacing = 0.45 m
From Chemical Engineering, Volume 6;

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

From Chemical Engineering, Volume 6, Figure 4.4 below:


Top K1 =

0.078

Bottom K1

0.037

52

Figure 5.14: Flooding velocity, sieve plate


Correction for surface tension:
From HYSYS simulation;
Surface tension, top

0.032 N/m

Surface tension, bottom

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

From Chemical Engineering Design, Volume 6

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

Design for 80% flooding at maximum flow rate:


Top v

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

Maximum volumetric flow rate:


Top

Bottom

Net area required

Vm / V

0.41 / 3.41

0.119 m3/s

Vn / V

0.41 / 7.99

0.051 m3/s

Maximum volumetric flow rate


uv

54
Top
Bottom

0.119 / 0.92

0.13 m2

0.051 / 0.82

0.062 m2

As first trial take downcomer as 19% of total:


Column cross-sectional area
Top

Bottom

Net area / 0.81

0.13 / 0.81

0.16 m2

Net area / 0.81

0.062 / 0.81

0.076 m2

Column diameter
Top

=
=

Bottom

=
=

Column cross section area 4

0.160 4

0.452 m

Column cross section area 4

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

Figure 5.15: Intalox Structured Packing (Koch-Glitsch)


Intalox structured packing is a unique family of patented distillation devices that offer
better efficiency and capacity than other metal-sheet structured packings. Intalox
structured packing delivers superior performance in these and other applications:
i.
ii.
iii.
iv.
v.
vi.
vii.
viii.

FCC main fractionators


Aromatic distillations
Alcohol distillations
Amine scrubbers and regenerators
Amine distillations
Glycol distillations
Flavor/fragrance fractionators
Refrigerant distillations

The characteristic of Intalox Structured Packing is as follows:


Table 5.22: Characteristic of Intalox Structured Packing
Surface area (ft2/ft3)
Voidage, (%)
Packing factor, Pf (ft-1)

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

Flood prediction by GPDC interpolation and Kister & Gill correlation


Table 5.24: Flow parameter and capacity parameter at flooding
Top
Bottom
X or Flv
0.010
0.719
Co
1.89
0.65
Cs,fl (ft/s)
0.452
0.149
Flow parameter, Flv is taken from the previous calculation; calculated using equation;

FLV

G
L

Equation 5.27
Pressure drop at flooding is calculated using equation;

PFl 0.115F p

0.7

PFl 0.115( 20) 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

Velocity, us, area, At, and diameter, Dt are calculated using;

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.

Table 5.26: Diameter calculation at maximum pressure drop


-1

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

off to the nearest standard pipe size 18 in (1.5 ft).


5.4.2.3.2 Determination of Packed Height
Table 5.27: Determination of packed height
dp(in)
Dt (ft)
12 Dt/dp
Area (ft2)
HETP (ft)
n (stages)
Total packed height (ft)
Height

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

www.cheresoures.com with refers to the packing size used in the tower;


tabulate in Table 4.18. For distillation process, HETP is equal to 1.5 ft (0.46
m) for packing size of 1.0 in. The total packed height is 30 ft; equivalent to
9.144 m. Height to diameter (H/D) ratio is 20 which is satisfactory the range
given that is H/D ratio must be kept below 20 to 30.
Table 5.28: HETP with respect to process and packing size
SETUP

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)

Table 5.29: Chemical Design Specification Sheet

60
CHEMICAL DESIGN SPECIFICATION SHEET
Identification:
Item: Distillation Column (Recovery Column)
Item Code: T-101
No. Required: 1

By: Siti Hajar binti Abd Kadir

Function: To separate ammonia to be recycled back to the feed stream


Operating Condition
0

Operating Temperature : 204.3 C


Operating Pressure: 503.33 kPa
Operation: Continuous
Column Specification
Design type

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

Column Cross Sectional

1.77 m2

20

Area

0.16

Top: 12

Reflux Ratio

Top: 0.12 m3/s

Bottom: 8

CFS (vapor flow rate)

Bottom: 0.05 m3/s

H/D ratio

20

Number of Stages

Stream Flow rate (kg/s)


Feed flowrate

3.93

Distillate flowrate

0.35

Bottom flowrate

3.58

1T Intalox Structured Packing Design


Surface area

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

Top: 1.18 m/s


Bottom: 0.39 m/s

Maximum pressure drop criteria

61
Pressure drop

83.3 mm H2O/m

Superficial velocity

Top: 1.90 m/s


Bottom: 0.63 m/s

5.5

DISTILLATION COLUMN 2, T-102

5.5.1

Introduction

Generally, the function of distillation is to separate components based on difference of


its boiling point by vaporization, a liquid mixture of miscible and volatile substances into
individual components or some into groups of components. Distillation employs heat to
generate vapors and cooling to effect partial or total condensation as needed. In
reboiled absorbers, partial stripping of the lighter components is performed in the lower
part of the equipment.
The feasibility of separation of mixtures by distillation, absorption, or stripping depends
on the fact that the compositions of vapor and liquid phases are different from each
other at equilibrium (Ulrich, 1984). When a liquid mixture of two volatile materials is
heated, the vapor that comes off will have a higher concentration of the more volatile
(i.e., lower boiling point) material than the liquid from which it was evolved. The greater
relative volatility, the mixture is easier to separate.
Vapour flows up the column and liquid counter-currently down the column. In other
words, the more volatile component is discharge at the top in vapour phase and the
less volatile is release at the bottom as liquid (Duncan and Reimer, 1998). This means
that the top product has low boiling point compared to the bottom product.
The purpose of this distillation column is to separate the components mixture to get the
desired product of ammonium nitrate. A distillation column design can be divided into
chemical and mechanical designs.
5.5.2

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.

Specify the degree of separation required: set product specification.


Select the operating conditions: batch or continuous; operating pressure.
Select the type of contacting device: plate or packing.
Determine the stage and reflux requirements.
Size the column: diameter, number of real stages.
Design the column internals: plates, packing supports.
Mechanical design: vessel and internal fittings.

Figure 5.17: Schematic Diagram for Distillation Column


For this design, the base column is heated by using condensing steam. The operation
of partial condensation of rising vapour and partial vaporization of the reflux is repeated
on each tray. On ideal tray the vapour rising from it will be in equilibrium with the liquid
leaving, though in practice a smaller degree of enrichment will occur. Continuous
fractionating column will be used in this design.
The purpose of this distillation column is to separate the components mixture
(ammonium nitrate, water, ammonia and nitric acid) to get the desired product of
ammonium nitrate in the bottom stream. The complete composition of the inlet and
outlet streams for the distillation column is shown in Table 5.30.

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.

There are no chemical reactions in the distillation column.

ii.

A cylindrical vertical vessel is suitable for this separation because of


large production and will be the cheapest shape.

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.

Neglecting friction loss in the pipes.

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

5.5.2.1 Bubble and Dew Point Temperature


To estimate the stage and condenser and reboiler temperature, procedures are required
for calculating dew and bubble points (Ulrich, 1984). By definition, a saturated liquid is
at its bubble points (any rise in temperature will cause a bubble of vapour to form), and
a saturated vapour is at its dew point (any drop in temperature will causes a drop in
liquid form). It can be calculated in term of equilibrium constant, K. Table below show
the constant of Antoine equation for each component (HYSYS).
Bubble point :

yi

kixi

= 1.0

Dew point

xi

yi/ki

= 1.0

Using Antoine equation to find vapour pressure (P0) (Hysys)

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

Table 5.34: Bubble point Calculation, Bottom (PT = 530 kPa)


T
Component
NH4NO2
H2O

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

Table 5.35: Dew Point Calculation, Top (PT= 400 kPa)


T
Component
NH4NO2
H2O

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

Table 5.36: Bubble-Point calculation, feed (liquid feed) (PT=530 kPa)


T
Component
NH4NO2
H2O

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)

5.5.2.2 Relative Volatility

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

light key component

KHK

heavy key component

LK

water, H2O

HK

ammonium nitrate, NH4NO2

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

5.5.2.3 Average volatility

LK , AVG = T B

Equation

5.35

LK , AVG = 400.086724 14.0374561


= 74.9413092
5.5.2.4 Number of Stages
Number of stages to this distillation column is calculate using Frenske equation in
continuous fractional distillation is an equation used for calculating the minimum
number of theoretical plates required for the separation of a binary feed stream by a
fractionation column that is being operated at total reflux (Duncan and Reimer, 1998).

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 m=2.3638 stages 3 stages


Normally after using Frenskes equation, the value of Nm is given by the equation below
to get the number of theoretical stages NT.

N T =2(N m )

Equation 5.37
= 2(3)
=6

5.5.2.5 Plate Efficiency


Feed composition, mole fraction:
Ammonium nitrate

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,

the average liquid viscosity, mNs/m2

average volatility of the light key

Average Liquid Viscosity


From HYSYS Simulation and calculation,
1. For distillate,

0.1445 mNs/m2

2. For bottom,

0.7783 mNs/m2

Average liquid viscosity =

0.1445 + 0.7783
2

0.4614 mNs/m2

From the previous calculation, relative volatility of light key is:

a=

74.9410392

Therefore, overall column efficiency,

74.9413092 0.4614 0.25

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

5.5.2.6 Feed Point


Estimation of the feed point location can be calculated using Kirkbride equation (1944):

[( )( )( ) ]

[ ]

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

Number of stages above the feed, including any partial

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

Where actual number of stages is 30


Nr + Ns
=
30

24.3524 N + N
s
s
Ns
Nr

Feed point

30

=
=
=

1.1833
28.8267
2 from bottom

5.5.2.7 Physical properties


5.5.2.7.1

Calculation for Density and Relative Molar Mass (RMM)


Table 5.38: Properties component
Molecular
Componen
t

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

Calculation for Relative Molar Mass (RMM)

RMM =

Component mole fraction MW

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

RMM Bottom Product =

0.8438(80.052) + 0.1562(18.015)

RMM Top Product

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

Total pressure drop, Pa, (N/m2)

ht

Total plate pressure drop, mm liquid

Pt =9.81 103 ht L
Top pressure, 5.132 atm

= 520 kPa

Bottom pressure, 3.9477 atm = 400 kPa


5.5.2.7.4

Calculation for density

a. Bottom product
Liquid density, L,w

xB,i i

0.8438(1725) + 0.1562(1000)

1611.755 kg/m3

Vapour density, V,w

VMW TSTP P OP

70.3618 kg /kmol 273.15


5.132

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

Vapour density, V,T

VMW TSTP P OP

18.0274 kg/kmol 273.15


3.9477

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

Table 5.40: Summary of density


Density (kg/m3)

Top

Bottom

Liquid

1000.145

1611.755

Vapour

2.0949

2.0949

5.5.2.8 Column Sizing


5.5.2.8.1

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

uv =( 0.171l +0.27 l t 0.047 )

( L V )
V

1 /2

Equation 5.42

uv = Maximum allowable vapour velocity, based on the gross (total)


column cross-sectional area, m/s

l t = Plate spacing (range 0.5 -1.0)


Where:

In order to use the given equation, the plate spacing has to be specified. Plate spacing
0.55 m is chosen.
Thus,

2
t

uv =( 0.171l +0.27 l t 0.047 )

( 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

Where Vw is the vapour flow rate (kg/s).


So,

V w=

234.1308 kmol /hr RMM (kg/kmol)


3600 s
234.1308 kmol / hr 70.3618(kg /kmol)
3600 s

= 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

Flooding velocity can be estimated from the correlation by Fair (1961):

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).

This will be revised as necessary. Therefore, the selected plate spacing is

satisfactory since the column diameter is 1.5 m.


From Figure 11.34: Flooding Velocity, Sieve Plate (Coulson and Ricardson, 2009)
Bottom Ki

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

0.8439 m/s (0.85)

0.7173 m/s

Top

5.5.2.8.4

Uf

2.4009 m/s (0.85)

2.0408 m/s

Maximum Volumetric Flow Rate

Maximum volumetric flow rate

Bottom

Top

234.1308 (18.0274)
1

2.0949
3600
0.5597 m3/s

Net Area, An

Net area required

Bottom

0.5205 m3/s

=
5.5.2.8.5

234.1308 (70.3618)
1

8.7916
3600

volumetric flow rate


flooding velocity

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

As first trial, take down corner area as 12% of total.

Column cross-sectional area:

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

5.5.2.9 Liquid Flow Pattern

Maximum volumetric liquid rate

L w RMM bottom
3600 L
406.5023 kg/ s 70.3618 kg /kmol
3
3600 s 1611.755 kg /m

4.9294 10-3 m3/s

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

plate by vapour flow

others
Sieve Plate
(Perforated

Simplest type

through the holes in the

Highest capacity rating

plate
Low flow rate of liquid

Good operating range

Plate)

Liquid is returned on the

will weep through the


holes, reducing the plate
efficiency

Bubble Cap
Plate

Traditional and oldest

Expensive

Risers ensures that level

Highest pressure drop

of liquid maintained on

Lowest capacity rating

tray at all vapour flow rate


Operate efficiently at low
vapour rates

Valve plate
(Floating Cap
Plate)

Operates efficiently at lower

Expensive than sieve

flow rate than sieve plates


Valve closing at low vapour
rates

plates

Pressure drop higher


than sieve 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

Provisional Plate Design

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

Number of holes per plate,

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

Height = (no.stages-1)(tray spacing)+(tray spacing2)+(no.stages-1)(thickness of plate)


Height =

(30 1)(0.55 m)+(0.55 m 2)+(30 1)(0.005 m)

17.195 m

18.9145 m (including 10% safety)

Approximate = 19 m

Table 5.42: Summary


Item
Column Diameter Dc

Value
1.5 m

No. of Plates

30

Plate Spacing

0.55 m

No. of stages below feed

Plate thickness

5 mm

Total Column Height, Ht

19 m

Down Corner Area, Ad


Column Area, Ac
Net Area, An
Active Area, Aa
Hole Area, Ah
Number of Holes

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

Weir Liquid Crest

Check weeping (Enough vapour to prevent liquid flow through hole)

LW (RMM )
3600 S

Maximum liquid rate =

406.5023 (70.3618 )
3600 S

Minimum liquid rate

7.9451 kg/s

0.7 7.9451 kg/s (at 70% turn-down ratio)

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

how +hw =( 15.694+50 ) mm liquid


= 65.694 mm liquid
From the figure 11.37: Weep-point correlation (Eduljee, 1959), we can find K 2 (a
constant, dependent on the depth of clear liquid on the plate)
When

how +hw =65.694 mm liquid


K2 = 30.4

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

Actual minimum vapour velocity

minimum vapour rate


Ah

0.7 (0.52051 m / s)
0.08
=

Actual minimum vapour velocity

4.5545 m/s

Uh

So, minimum operating rate will be below the weep point.

5.5.2.15

Plate Pressure Drop

5.5.2.15.1 Dry Plate Drop


The pressure drop through the dry plate can be estimated using expression derived for
flow through orifices:
2

[ ]

U
hd =51 h
Co

v
L

Equation 5.48
Uh
Co
Uh

=
=
=

Velocity through the holes


Orifice coefficient

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

Therefore, dry plate drop:


2

6.506375 8.7916
hd =51
0.812
1611.755
=17.86097 mm liquid

5.5.2.15.2

Residual Head

Residual head can be calculated using Hunt et al (1955) equation:

hr =

12.5 103
L

hr =

12.5 10
1611.755

Equation 5.49

= 7.75552 mm liquid

5.5.2.15.3

Total Plate Pressure Drop

ht =hd + ( h w + how ) + hr

ht =17.86097+ ( 50+15.694 )+ 7.75552


ht =91.31049 mm liquid

5.5.2.15.4

Downcomer Liquid Back-up

Downcomer pressure loss:

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.

Area under apron,

A ap=hap (I w )
= 4010-3 m (1.14 m)
= 0.0456 m2 0.05 m2
Where

A ap is the clearance area under downcomer.

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

= Head loss in down comer, mm

c
Lw
Am

= Liquid flow rate in down, kg/s


= Either the down comer area Ad or the
clearance

area

under

A ap :whichever is the smaller

down

comer,

hdc =166

7.9451
1611.755 0.05

= 1.6135
= 2 mm
Back-up in the down comer, (hb),

hbc =h w + how + hht +h dc

Equation 5.51

hbc =50+15.694+ 91.31049+2


= 159.00449 mm liquid or 0.159 m
For safe design the clear liquid back-up should not exceed half the plate spacing it, to
avoid flooding. Therefore,
hb

<

1/2 (plate spacing + weir height)

0.159m

<

1/2 (plate spacing + weir height)

0.159m

<

1/2 (0.55 + 0.05) m

0.159m

<

0.3 m

So, tray spacing is acceptable (to avoid flooding)

5.5.2.15.5

Downcomer Residence Time

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

0.2121 0.159 1611.755


7.9451

= 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

value is below 0.1, so column diameter which is proposed earlier is acceptable.

5.5.2.15.7

Perforated Area

From (Coulson & Richardsons, 2009)

At=

Iw
Dc

Equation 5.54

1.14 m
1.5 m
= 0.76

Therefore,

99

Angle subtended at plate edge by unperforated strips,

5.5.2.15.8

(180 99)

81

Mean Length, Unperforated Edge Strips

( Dc 0.05)

81
180

(1.50.05)

81
180

1.1745m

5.5.2.15.9

Area of Unperforated Edge Strips

(5010-3) m (1.1745) m

0.058725 m2

5.5.2.15.10

Area of Calming Zones

2 0.05 (Iw 2 50 10-3) m2

2 0.05 (1.41 2 50 10-3) m2

0.113 m2

5.5.2.15.11
Ap

=
=
=

Total Area Available for Perforation, Ap


Active area (Area of unperforated edge + Area of calming zones)
1.342946 m2 (0.058725 + 0.113)m2
1.171221 m2

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,)

satisfactory , range normally within 2.5


Ip
=3.34( 4.0)
dh

5.5.2.15.12

Trial Layout

50 mm

1.14 m

50 mm

Figure 5.19: Trial layout

1.5 m

5.5.3

Summary of Chemical Design of T-102


Table 5.43: Summary of chemical design
Item

Value

Column diameter, Dc

1.5 m

Plate spacing, ts

0.55 m

Downcomer area, Ad

0.2121 m2

Downcomer Material

Stainless steel, type 304

Plate material

Stainless steel, type 304

Plate Thickness t

0.005 m

Column Area, Ac

1.7671 m2

Net Area, An

1.5551 m2

Perforated plate area, Ap

1.1712 m2

Active area, Aa

1.3429 m2

Total hole area, Ah

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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http://www.fanagalo.co.za/tech/tech_grade_304.htm
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High

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tray.

Source:

http://www.distillationgroup.com/questions/question008.htm
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