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COMPRESSOR (K-102)
MIXER (M-101)
1
TABLE OF CONTENTS
CHAPTER 1: R-106 PROCESS DESIGN...........................................................3
CHAPTER 2: R-106 SPECIFICATION SHEET .............................................14
CHAPTER 3: R-106 MECHANICAL DESIGN ...............................................15
CHAPTER 4: R-106 OPERATING PROCEDURE .........................................36
CHAPTER 5: R-106 EQUIPMENT COSTING ...............................................39
CHAPTER 6: K-102 COMPRESSOR DESIGN...............................................40
CHAPTER 7: M-101 MIXER DESIN................................................................43
2
CHAPTER 1: PROCESS DESIGN
1.1 INTRODUCTION
The reaction stage is the heart of a chemical manufacturing process. In the reactor the raw
materials are brought together under conditions that promote the production of the desired
product and/or by-product as well (Sinnott, 2005). Chemical engineers are responsible to
design reactors in order to maximize net present value for the given reaction. Designers
ensure that the reaction proceeds with the highest efficiency towards the desired output
product, producing the highest yield of product while requiring the least amount of money
to purchase and operate. This section will further discuss on the detail design of oxidative
dehydrogenation reactor to convert 4-vinylcyclohexane into styrene monomer. Following
figure shows the particular reaction with addition of by-product produce such as water and
ethylbenzene in the present of excess oxygen.
US patent 4165441 entitle process for production of styrene by DOW chemical suggest the
reaction carried out at atmospheric pressure with operating temperature of 380C and
operating pressure of 101.3 kPa in the present of tin/antimony oxide catalyst. The reaction
takes place in gaseous phase and highly exothermic. The following paragraph explains on
reactor design methodology.
3
1.2 METHODOLOGY OF DESIGN
In general, the design methodology for the major equipment is classified into 2 major
sections; the process design and mechanical design. The overall design is carried out in
series of stages as follow:
4
models.
From above comparison on the properties of packed bed and fluidized bed reactor, it is
found that packed bed reactor is more convenient to be used as heterogeneous phase exist.
The inlet reactant is in gas phase in contact with the solid catalyst. Following paragraph
describe further justification of using fixed bed reactor for oxidative dehydrogenation
reaction.
1) Flow arrangement
With the reaction highly exothermic, single flow will prone to create reactor hot spot due
to the uneven heat release. To overcome this, a multi-tubular reactor is used. It is a
modified multiple packed-bed units, where the multiple beds are catalyst-filled tubes
arranged in parallel with conduction fluid flowing outside the tubes. Reactor temperature
can be maintain with the increase of cooling surface area.
5
2) Lower capital and operating cost
Operating pressure required for the process is at 101.3 kPa. For operating pressure, the
required volume for packed bed catalytic reactor is smaller compared to fluidized bed
reactor. Therefore, lower capital cost is required.
The catalyst is packed in the tubes when it is at contact with the reactant in fixed bed
catalytic reactor which results in low possibility of catalyst loss. Gasification process that
take place in fluidized bed reactor increase the possibility of catalyst particles carry over
along with fines.
6
Component Mass Fraction Flow Rate (kg/h) Flow Rate (kgmole/h)
1,3-butadiene 0.000000 0.00000 0.00000
I-Butene 0.000000 0.00000 0.00000
1-butene 0.000000 0.00000 0.00000
Cis-2-butene 0.000000 0.00000 0.00000
Trans-2-butene 0.000000 0.00000 0.00000
N-butane 0.000000 0.00000 0.00000
Isobutane 0.000000 0.00000 0.00000
Vinylcyclohexene 0.024999 12114 111.98
Oxygen 0.144088 69821 2181.9
Styrene 0.122555 59386 570.19
Nitrogen 0.645283 312690 11162
Hydrogen 0.000038 18.633 9.2424
Benzene 0.000048 23.176 0.29672
Water 0.046757 22657 1257.7
Carbon dioxide 0.014206 6883.6 156.41
Ethylbenzene 0.002025 981.23 9.2424
Reaction takes
Main reaction
Side reaction
All reaction are highly exothermic reaction since the heat of reactions shows negative sign.
1.6 CATALYST
7
In the production process of styrene from 4-vinylclclohexene (VCH) comprising
contacting feed stream in a gas phase with catalyst comprising tin, antimony and oxygen
under sufficient condition. The catalyst has a half-life of 1000 hours. (US Patent 4165441).
i. Temperature Optimisation
The reaction can be performed under a low degree of pressure, under reduced pressure or
at normal conditions. Thus, based on economic justification operation at atmospheric
pressure is desirable. In this design, the pressure of 1.013 bar (101.3 kPa) is used where it
is at atmospheric condition to make sure no outside air enter the reactor in case of leakage.
For packed bed or homogenous reactors, the gas hourly space velocity (GHSV) is a way of
rapidly sizing reactors. Space velocity is defined as the ratio of the volumetric feed flow
rate to the reaction volume or the ratio of mass feed flow rate to the catalyst mass. The
volumetric feed-gas flow rate is calculated at a standard temperature and pressure. Thus,
the space velocity is defined by:
8
In this design, the reaction takes place in gas phase. According to the patent, GHSV for the
reaction is in the range of 5000 h-1 to 1000 h-1. Thus for the calculation 1000 h-1 is
considered where it means that 1000 reactor volume of 4-vinylcyclohexene at standard
condition is converted in one hour.
s = 0.04462 kg.mol/m3
Thus,
9
=
=
s = 0.03232 kg.mol/m3
Ab = 225.36 m2
v. Bed Diameter.
4'(
) = *
,
Thus,
D = 4.068 m
10
Normal sizing is round off to the nearest feet. 4.068 m = 13.26 ft. is round off to
13.50 ft. thus actual bed diameter is 4.115 m.
Thus,
Lb = 6.3246 m
Thus,
Vb = 84.12 m3
Tube material selection must be made in accordance to the suitability to the process.
Carbon steel IS: 3609 -1966 1% Cr Mo is selected due to good corrosion resistance and
mechanical properties. With the catalyst inside the tubes, the reactor volume must be equal
to the inside volume of the tubes. By specifying the tube diameter and length of a single
tube, the volume per tube can calculated. Preliminarily, tubes of 2 1/2 in. carbon steel IS:
3609 -1966 1% Cr Mo, with 14.68 m length are selected. This is a large size for heat
exchanger tubing but a large size is desirable for good catalyst distribution and minimal
wall effects. The properties of the pipe are stated as below (Values obtained from
Timmerhaus (2003) Table D-13):
11
Table 2.1: Tube Specification
Lb,eff = 9m
Thus,
Volume of one tube = 0.02781 m2
: =
(
.!"
!5
Thus,
Nt = 3009 tubes
12
1.10 PRESSURE DROP ON TUBE SIDE
There are 2 major sources of pressure loss on the tube side which are the friction loss in the
tubes and the losses due to the sudden contraction, expansion and flow reversals
experienced by the fluid while flowing through the tube arrangement. For fluid flow
through fixed-bed, the most popular method of calculating pressure drop in a packed
porous bed is the Erguns equation. According to Fogler (2001),
2?; - A
= (1 )/
; ;
B(1 ) 150(1 )J
?; = [ + 1.75B]
DE ; )F G )F
"77 . 89
B=
!5 7
13
CHAPTER 2: SPECIFICATION SHEET
14
CHAPTER 3: MECHANICAL DESIGN
15
3.2 REACTOR SHELL DESIGN
Based on the patent 4165441, process for the production of styrene, suggested the
oxidative dehydrogenation of 4-vinylcyclohexe to styrene can be performed under a low
degree of pressure, under reduced pressure or at normal conditions. In this design, reactor
operating pressure is set at 1.013 kPa. In calculating the design pressure, maximum
working pressure (MWP) has to be considered. The maximum working pressure is the
maximum gauge pressure expected in the equipment under any condition. It should not be
exceeded under any conditions to avoid damage to the equipment. MWP for the column is
taken as 5% above the operating pressure, to take care of valve hysteresis, noise and
overpressure.
Design pressure is taken as more than the maximum working pressure. Design pressure is
the differential pressure between the outside atmospheric pressure and PMWP, to give the
column maximum allowance for operation. Factor of 1.05 is added to the differential
pressure which resemble 5% safety factor.
Prior to find the value of allowable stress for the material of construction which is
temperature dependent, it is vital to determination the appropriate design temperature.
Design temperature is determined from the process design temperature.
Generally, the following heuristics are applied in order to determine the design
temperature:
1. For unheated part consider the highest temperature of the stored material.
16
2. For part that is heated by means of steam, hot water, and oil consider the highest
temperature of the heating media, or 10C higher than the maximum temperature
that any part of body is likely to attain during course of operation.
3. For vessel where direct internal or external heating is employed by means of fire,
flue gas or electricity or for severe exothermic reactions that takes place:
a. Consider the highest temperature of the inside material plus minimum of
20C if vessel is shielded.
b. Consider the highest temperature of the inside material plus minimum of
50C if vessel is not shielded.
c. For highly exothermic reactions, same condition as above applies.
For the oxidative dehydrogenation reactor, first heuristic is applied. Factor of 1.05 is to
consider the safety limit for column operation.
Pressure vessels are usually constructed from plain carbon steels, low and high alloy steels,
other alloys, clad plate, and reinforced plastics (Sinnott, 2005). Several issues need to be
considered for material selection such as corrosion, compatibility of the material toward
process environment and the cost. In this design Carbon-Steel is selected for oxidative
dehydrogenation reactor because the reaction taking place at both moderate temperature
and pressure as well as it involve non-corrosive gases component.
A minimum wall thickness required to ensure that the column is sufficiently rigid to
withstand the design pressure for the reaction is given in the equation below.
17
Where Di = Internal Diameter
f = Design stress = 85 N/mm2
PD = Design absolute pressure = 0.159 N/mm2
J = Welding efficiency = 1.0
c = Corrosion allowance
For carbon and alloy steel, where severe corrosion is not expected, a minimum corrosion
allowance of 2 mm should be taken into account (Sinnott, 2005). From reactor process
sizing, the internal reactor diameter, Di = 4.115 m.
Thus, t= 5.85 mm
However, the minimum practical wall thickness is also a function of column diameter. The
1.5 and e 0.25
ei
ef
condition above is only valid if:
f
The ends of a cylindrical process vessel are to be closed by heads of various shapes.
According to (Sinnott, 2005), the principal types used are:
The selection for a particular type of head depends on the factors such as process
temperature and pressure, nature of the materials to be handled and products produced,
18
position of the vessel, nature of the support and above all the economy. Standard
torispherical heads (dished ends) are the most commonly used end closure for vessels up to
operating pressures of 15 bar and it has less stress concentration as compared to flat plate.
The minimum thickness required can be calculated using equation below.
r 6%
=
2 s + (6% 0.2)
1 r
6% = (3 + * )
4 t
Thus, CS = 1.77
Substituting all the values above into thickness equation gives,
t = 6.436 mm
Flanged joints are used for connecting pipes and instruments to vessels, for manhole
covers, and for removable vessel heads when ease of access is required. Flanges may also
be used on the vessel body, when it is necessary to divide the vessel into sections for
transport or maintenance (Sinnott, 2005).
19
Several different types of flange are used for various applications. The principal types used
in the process industries are:
1. Welding-neck flanges.
2. Slip-on flanges, hub and plate types.
3. Lap-joint flanges.
4. Screwed flanges.
5. Blank, or blind, flanges.
In this design, welding-neck flanges are suitable to be used because it can withstand
extreme service condition such as temperature, shear and vibration loads. It have a long
tapered hub between the flange ring and the welded joint. This gradual transition of the
section reduces the discontinuity stresses between the flange and branch, and increases the
strength of the flange assembly.
Gaskets are used to make a leak-tight joint between two surfaces. It is made from soft
semi-plastic material which will deform and flow under load to fill the surface
irregularities between the flange faces, at the same time retains sufficient elasticity to take
up the changes in the flange alignment that occur under load. Selection of gasket material
depends on the process condition such as pressure, temperature and corrosive action of
chemicals that may contact the gasket, the gasket location and type of gasket construction
as well on the type of flange and flange face. The data for gasket calculation is listed
below:
20
Table 3.1: Gasket material (Based on a similar table in BS 5500: 1991)
Minimum Minimum
Gasket Gasket
design Sketches Gasket
Material Factor
seating stress Width
Asbestos with a
suitable binder 2.75 25.5 N/mm2 10 mm
(1.6 mm thick)
u e "
= *
R e (" + 1@
Thus;
u
1.069
R
Assume gasket inside diameter 5 mm larger the reactor outside diameter. Thus:
R )u 2 <5 mm@
Where, DO = Reactor outside diameter = 4.127 m
Thus;
di = 4137 mm
21
u
1.069
R
Thus;
do = 4422.5 mm
Thus;
N = 142.75 mm
The minimum width of the gasket is 10 mm. The calculated value can be used as
gasket width.
Thus;
b = 21.12 mm
Thus;
G = 4279.75 mm
The bolts hold the flange faces together, resisting the forces acting on a flanged joint.
Table below shows the suitable bolt material used for the design and its characteristic.
22
i. Bolt loads, W
Thus;
WM1 = H + Hg = 2158113.34 N + 85200.03 N = 2243313.37 N = 2.24 MN
Since Wm2 is greater than Wm1, it controls the load. Further calculation will base on
Wm2.
23
ii. Minimum bolting area, Abf
y_
'(3
(
Make sure the gasket material is strong enough for bolting. If the left hand term
(LHS) of equation below is less than the right hand term (RHS), the material
selected is strong enough for bolting.
< 2
'(3 T
,B:QE{Q|
24
, / e
yA
4
W1 = 2127 kN
W2 = 160 kN
c. Gasket load, W3
yG ,B<25)e
Thus;
W3 = 90 kN
6
A =
2
A + G
/ =
2
6B
G =
2
25
B = Shell outside diameter = Do = 4127
mm
C = Bolt circle diameter = 4300 mm
Thus;
a1 = 86.50 mm
a2 = 53.38 mm
a3 = 20.25 mm
T
'(3 (
2
yT
6}
3 = *
26
St = Allowable stress of flange material = 10 000
MN/m2
B = Shell outside diameter = Do = 4127
mm
Thus;
Cf = 9.35 mm
Pipe diameter for both inlet and outlet of oxidative dehydrogenation reactor can be
determine using correlation below (Richardson's, 1994).
)uFR_{_ 226 B p.n hp.Gn
Thus;
D inlet nozzle = 1134.1 mm
D outlet nozzle = 1372.5 mm
Thus;
e inlet nozzle = 3.85 mm
27
e outlet nozzle = 3.85 mm
For cylindrical vessel with domed ends, and uniform wall thickness, the approximate
weight can be estimated using following equation:
Thus;
Wv = 67 727 N
28
Total weight of fluid in reactor comprises of the weight of fluid, catalyst and the heating
medium molten salts. On the tube side, the volume of fluid and catalyst are calculated
whilst at the shell side the weight of molten salts is taken into consideration.
i. Weight of fluid , Wf
y3 3 D
4
Thus;
Wc = 1188312.8 N
yR R D
,); z~
29
Where, Wi = weight of insulating material
i = insulation density (mineral wool) = 130 kg/m3
V = insulation volume
= pi = 3.142
Do = reactor outside diameter = 4.127 m
t = insulation thickness = 0.1 m
Hv = Reactor height = 10 m
Thus;
V = 12.965 m2
Wi = 16534.26 N
i. Wind pressure , Pw
0.05(! )/
Thus;
30
Pw = 1280 N/m2
)R
=
4
)R
$ =
2
31
H = circumferential stress
P = Operating pressure = 0.15 N/mm2
Di = Inner diameter = 4115 mm
t = wall thickness = 5.85 mm
Thus;
L = 26.378 N/mm2
H = 52.756 N/mm2
()u k )R k )
,
64
&
)R
( = ( + )
& 2
32
N (
W is compressive, thus the value will be a negative.
As assume that there is no torsional shear stress, the principal stresses will be Z and h.
The radial stress is negligible,
R
2
= 0.075 N/mm2
If the resultant axial stress, z due to the combined loading is negative, the reactor may fail
due to elastic instability (buckling). The condition for this not to take place is the
maximum compression stress, c must be more than the critical buckling stress, c max.
r,_Q = + ((h~2)
r = 2 10k (/); )
33
Thus;
The maximum compression stress is 4.679 N/mm2 which is lower than 28.35 N/mm2. It is
well below the critical buckling stress. Thus, design is satisfactory.
<z~ z @/
2
y
=
,() + )
Thus;
ws = 16.35 N/mm2
34
3.10.3 Resultant skirt stresses
<
79 @ (
<8" 779. @ (
Thus;
<
79 @ s sin
<8" 779. @ 0.125 sin
)
35
CHAPTER 4: OPERATING PROCEDURE
This procedure provides operating instruction for the R-106 s ystem, inclusive
of operation instructions for system start-up and shutdown.
36
4.6 Procedures
4.6.1 Reactor Pre-Start up Procedures
No. Procedures Checklist
Ensure that ample inventory is available at each unit operation.
1
Note that reactor will be last unit operation to start up.
Verify Vessel Readiness for start-up, i.e., all maintenance and
I&E works completed, the reactor is clean and rinse with process
2
water if necessary, man way closed, all blinds are removed and
proper gasket are installed.
3 Line up molten salt into the shell-side of R-106.
4 Line up all transmitters and stroke all control valves.
5 Close, plug and cap all bleeders.
Place the reactor temperature indicator (TI) and pressure
6
indicator (PI) in service.
Purge reactor with high pressure N2 until the vent of O2 is
7
lower than 6%.
Pressure up the reactor with high-pressure nitrogen to 400kPa
8
and perform leak check on all flanges.
10 Pressure up the reactor to 800kPa and check flanges for leaks.
37
4.6.3 Hot Hold and Shut Down of Reactor
No. Procedures Steps Checklist
8 Open both man ways of the reactor and inspect the cleanliness
inside the reactor. Access the need of washing.
12 If reactor is not clean, then close the man ways and perform
washing with process water.
38
CHAPTER 5: COSTING
The costing for reactor is based on the cost correlation method of reactors (Douglas,
1988).
&
!87 87, $ = [101.9)A.p z p.q/(r )]
280
Thus,
USD 1 = RM 3.24
39
CHAPTER 6: K-102 COMPRESSOR DESIGN
AIR COMPRESSOR
6.1 Introduction
Compressor is used to transfer and compress gases from one process unit to another to
carry out chemical reactions, separation and to liquefy gases. In this styrene
production plant, K-102 is located in between a packed bed reactor, R-106 and a heat
exchanger, E-105. The original purpose is to compress product gas coming out of
reactor to an increased pressure before flowing in it into a heat exchanger. The type of
this compressor will be a multistage centrifugal compressor.
Vs
6F 6F,RS|2 41.12
VD"
= = = = 1.253
6~ 6F,RS|2 41.12 Vs Vs
8.3144
VD" VD"
Polytropic Efficiency, Ep
= 78.303 %
40
Polytropic temperature exponent, m
1 1.253 1
= = 0.258
(1.253)(0.78303)
/ _ 500 p./nq
= A = 380 = 573.68
A 101.3
Polytropic exponent, n
1 1
= = = 1.3478
1 " 1 0.258
= 10 725.70 Vs V" hA
where
A = 380 = 653
A = 101.3 V
/ = 500 V
6" 779599 8, = 1.000
Shaft Power
= 98 yV ()
41
484600 VD 1 V"
10725.70 Vs V" hA
31.35 VD
= 165 795 030.9 Vs hA
Vs 1 1 "9
42
CHAPTER 7: M-101 MIXERDESIGN
7.1 Introduction
Mixer M-101 is a two phase mixer which mixes two inlet streams which are vinyl
cyclohexene, VCH stream and air stream containing oxygen. This mixer will mix
these streams and will have one product stream. This mixing is required prior VCH-
Styrene conversion reaction. The illustration of Mixer, M-101 can be described as
follows:-
The following table shows the conditions of stream entering and leaving the mixer M-
101
Table 7.1- Properties of Streams Entering and Leaving M-101
Stream
In Out
Conditions A 26 27
Phase Vapour Vapour Vapour
Temperature [C] 339.7 339.7 339.6
Pressure [kPa] 101.3 101.3 101.3
Molar Flow [kgmole/h] 1.413 x 104 711.3 1.484 x 104
Mass Flow [kg/h] 4.076 x 105 7.693 x 104 4.846 x 105
Molar Enthalphy
9477 1.308 x 105 1.529 x 104
[kJ/kgmole]
Molar Enthropy
173.3 -30.62 165.1
[kJ/kgmole-C]
8 7
Heat Flow [kJ/h] 1.339 x 10 9.306 x 10 2.270 x 108
43
7.2 Process Design
The minimum size of charge for the mixer is equal to the volume of the outlet strean
abd the time of mixing is assumed to be 5 seconds.
Table Error! No text of specified style in document.-1: Operating Data for M-101
!"
79 8D "99
D 9"
26.67 "G 7 hA 5 7 = 133.355 "G
The mixing is in continuous flow process for 330 days in a year for the production of
styrene. The length and diameter of the vessel which represents the volume of the
1036.55 m3 can be calculated by using trial and error method. The diameter and length
of the mixer is assumed to be following the equation below:-
= , / - = , / (5) = 5, G
= 133.355 "G
G = 8.49 "G
= 2.04 "
Therefore the diameter and length of the vessel are at 4.16 m and 10.21 m
respectively. The mechanical data of the vessel are tabulated in the following table.
44
Mechanical Data Value
Pressure Operating 101.3 kPa
Design 106.365 kPa
Temperature Operating 339.7 oC
Design 349.7 oC
The operating temperature and pressure are taken from the mixing temperature and
pressure. The design temperature is 10oC higher than operating temperature. The
design pressure is 1.05 of operating pressure.
45