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Design Project
1
12.2.4 OVERALL COLUMN EFFICIENCY .............................................................................................. 37
12.2.5 HEIGHT OF THE COLUMN....................................................................................................... 37
12.2.6 NOZZLES ................................................................................................................................. 37
12.2.7 AREA OF CONDENSER ............................................................................................................ 37
12.2.8 AREA OF REBOILER ................................................................................................................. 38
12.2.9 ENGINEERING SPECIFICATION SHEET FOR DISTILLATION COLUMN (T-101).......................... 41
13. OSBL SPECIFICATIONS ........................................................................................................................ 42
13 PLANT LAYOUT ................................................................................................................................... 46
14 SAFETY, HEALTH AND ENVIRONMENT ............................................................................................... 50
14.1 SAFETY, HEALTH AND ENVIRONMENT COMPLIANCE STUDIES...................................................... 51
15 FINANCIAL ANALYSIS .......................................................................................................................... 54
16 CONCLUSION & RECOMMENDATIONS .............................................................................................. 57
17 REFERENCES ....................................................................................................................................... 58
2
1 INTRODUCTION
1.1 OVERVIEW
Phthalic Anhydride (PA) is a principal commercial form of phthalic acid, discovered in 1836. It is
an important chemical intermediate and its biggest application, accounting for just over half of
production, is in the manufacture of phthalate plasticizers, the main product being dioctyl
phthalate (DOP) which is used as a plasticizer in polyvinyl chloride (PVC). Hence, the consumption
of PA is mainly dependent on the growth of flexible PVC, which is sensitive to general economic
conditions as it is consumed in the construction and automobile industries.
3
1.2 MARKET CONDITIONS
1.2.1 GLOBAL MARKET
The Phthalic Anhydride market was valued at USD 6.46 billion in 2012 and is expected to reach
USD 9.58 billion by 2019, growing at a CAGR of 5.8% from 2013 to 2019. In terms of volumes,
global consumption was over 4.3 million tons in 2012 and is expected to grow at a CAGR of 3.6%
from 2013 to 2019.
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1.2.2.1 IMPORTS
Phthalic Anhydride is imported into India from a number of countries, and primarily from
Republic of Korea, Israel, Iran, Taiwan, China and Russia. The imports of Phthalic Anhydride have
shown an increasing trend in absolute terms as well as compared to the domestic production.
Imports have increased to 43420 MT in 2012-13 from 38894 MT in 2011-12. Further domestic
production has increased to 225262 MT in 2012-13 from 215124 MT in 2011-12. Domestic
production has therefore, increased by 5%.
1.2.2.2 EXPORTS
The domestic sales have increased to 196115 MT in 2012-13 from 177730 MT in the preceding
year. The exports have slightly decreased to 26324 MT in 2012-13 from 40254 MT in the
preceding year.
The major export destinations are: Egypt, Saudi Arabia, UAE, Kuwait, Iran, China and Thailand.
5
2 CAPACITY
2.1 END USER MARKET
2.1.1 AUTOMOBILE INDUSTRY
The Indian automobile industry produced a total 1.69 million vehicles including passenger
vehicles, commercial vehicles, three wheelers and two wheelers in August 2013 as against 1.56
million in August 2012, registering a growth of 8.18 percent over the same month last year.
The overall automobile exports grew by 2.03 per cent during April-August 2013. Furthermore, the
production of passenger vehicles in India was recorded at 3.23 million in 2012-13 and is expected
to grow at a compound annual growth rate (CAGR) of 13 per cent during 2012-2021.
2.1.2 PVC
According to industry sources in India, the country’s PVC demand is currently pegged at 2.08
million mt/year. The consumption of PVC in India is expected to increase to 3.1 million mt/year
by 2016-17.
6
3 TECHNOLOGY SELECTION
3.1 AVAILABLE TECHNOLOGIES
The available process technology for PA manufacture can be categorized via either Naphthalene
or O-xylene as feed under: Vapour phase (fixed and fluid bed) and liquid phase. Fluidized bed
processes mainly use naphthalene and their yield is lower than that of fixed bed processes,
especially if they employ o-xylene.
NAPHTHALENE ROUTE
Naphthalene route was adopted by the older Phthalic anhydride plants using process like
Sherwin-williams/badger fluidized bed process.
Fluidized-bed vs Fixed-bed.
Phthalic anhydride has been manufactured by the oxidation of naphthalene in fixed-bed reactors
for more than forty years. However, it is widely known that such reactors have inherent defects
which make impossible the desired control of reaction conditions. The advent of the fluidized-bed
reactor has made possible not only a much closer approach to these ideal reaction conditions but
also several other important advantages which favourably influence the economics of the
process.
1. Greater Safety- prevents explosions and so permits operation well inside the explosive
range of air:naphthalene ratios.
2. More precise control of reaction conditions-The high thermal conductivity and good
heat-exchange characteristics of this fluidized-catalyst bed permits an exact control of
reaction temperature without the formation of hot spots. Temperatures varying only by
one or two deg F can be held throughout a fluidized bed containing up to 30 tons of
catalyst or more. Pressure, temperature, air:naphthalene ratios and contact time can each
be varied, independently and quickly, so permitting a rapid and exact adjustment of
operating conditions to meetparticular requirements.
7
4. Liquid naphthalene feed- mixture of air and naphthalene vapour involving the use of a
separate evaporator. This can give trouble. With a fluidized-catalyst reactor liquid
naphthalene is pumped-directly into the reactor.
5. Catalyst charging- The tedious operation of charging catalyst pellets into the tubes of the
fixed bed reactor is avoided. On the fluidized bed plant catalyst can be moved
pneumatically from the reactor to the catalyst storage vessel or in the opposite direction,
even whilst the plant is operating.
7. High purity product- The precise control of reaction conditions in a fluidized catalyst
reactor results in the formation of a crude product of high purity. The redistillation
process is thereby considerably simplified, and a final sales product of a high standard of
purity is obtained.
O-XYLENE ROUTE
O-xylene is used as the raw material in Phthalic anhydride plants all over the world now.
The consideration for process selection was on the basis of the following criteria:
8
Safety: Less More
1. CO2 emission
2. Processing Higher (350 to 500) Lower (340 to 385)
Temperature
1. Raw Materials :
O-Xylene is readily available in large quantities for the manufacture of Phthalic Anhydride.
Reliance Industries Limited is India’s largest manufacturer of Orthoxylene with a capacity
of 150 KTA, and figures amongst the top 5 Orthoxylene producers in the world.
Orthoxylene is produced at Reliance Jamnagar Complex as a co-product from the
Paraxylene Plant.
Contemporary processes are based on O-Xylene and all plants in India employ this route,
as naphthalene is expensive and not easily available.The major outlet for naphthalene is
now in the production of naphthalene sulfonates as a result of whose expanding NSF
markets and feedslate shifts, it’s use in the consumption for phthalicanhydride has been
reduced.
Thus, O-xylene is the preferred raw material since it is higher yielding as all carbon atoms
appear in the product), because of availability (naphthalene sources are becoming rarer)
and cost (naphthalene is only available at a competitive cost in an impure form which is
less suitable).
2. Utilities :
Basic utilities required would be water, power, air and process water. Applied utilities
include dowtherm as a heat transfer fluid, hot oil and cooling water.
9
(a) airborne emissions;
(b) waterborne emissions;
Airborne emissions will contain low concentrations of PAN and other organics but these
will be satisfactorily dispersed by a stack. Waterborne emissions will be minimal but
available treatment facilities will be utilised where required.
The main process hazard which may occur during normal operation of phthalic anhydride
plants is the risk of PAN dust clouds forming from minor process breaches. PAN dust
clouds are both toxic (at concentrations below 1%) and explosive (at concentrations of
1.5-10.5%). Air quality monitoring will be utilised to identify process breaches producing
dust clouds before they become hazardous. Appropriate breathing equipment (dust
masks, respirators, etc.) will always be available.
Also, the Toxicological Profile for Naphthalene and strict environmental regulations are
limiting the use of Naphthalenes.
4. Simplicity of Process :
In recent years, the fixed-bed vapour-phase process has proven to be superior to the
alternatives and all plants built in the last ten years have used this process. Fluidized bed
processes mainly use naphthalene and their yield is lower than that of fixed bed
processes, especially if they employ o-xylene. Fluidised bed processes have proved
difficult to maintain and have suffered from erosion problems and excessive catalyst
losses. The construction costs of liquid-phase processes have proven prohibitive.
6. Catalyst Recovery :
Not much loss of catalyst as it is a fixed bed process
10
4 PROCESS DESCRIPTION
Phthalic Anhydride (PA) today is produced from two main sources:
1. Production from o-xylene (Vapour phase: fixed, fluidized bed; Liquid phase)
2. Production from naphthalene(Fixed, Fluidized beds)
Both main technologies involve specific catalyst for selective oxidation of raw material to
product.
The raw o-xylene is pre-heated and mixed with a compressed air stream. Excess air is employed
to ensure that the mixture is below the lower explosive limit of 1.5 mole percent o-xylene.Then, it
enters a fixed-bed reactor where the crude product is obtained. Here, steam is generated which
is used as a utility in the plant.
CATALYST: Many variations of the Vanadium oxide catalyst are possible. We have decided to
employ a catalyst which consists of 3.75 wt% Vanadium oxide and 21.25 wt% potassium
pyrosulphate on a titanium dioxide carrier (75 wt%). To activate the catalyst, about 65% of the
vanadium is converted to the tetravalent state by heating in air containing SO2.
11
PREHEATER AND REACTOR SECTION: The o-xylene preheated to 140-150 deg C and air, filtered,
compressed and preheated to 160 deg C, is introduced into the multi-tube reactor. The
temperature is kept at 380 deg C by dowtherm circulation. A heat exchanger system installed on
the coolant fluid circuit is used to produce high pressure steam. The catalyst is a mixture of
vanadium and titanium oxides deposited on an inert, non-porous support. The gaseous reactor
effluent is first cooled with the production of low-pressure steam and the residual gases scrubbed
with water and then discharged to the atmosphere.
CONDENSATION AND RECOVERY: The recovery of phthalic anhydride is done using a set of
switch condensers. The condensed stream obtained is sent to switch condensers which are a
complex set of condensers in which phthalic anhydride is first desublimated using cooled
diathermic oil and then melted at 130 deg C and sent to a storage tank. The following fractions
leave as the off gases:
O-Xylene, Oxygen, Nitrogen, Water, Carbon Dioxide, Carbon Monoxide, Phthalic Anhydride,
Maleic Anhydride and Heavy Impurity.
DISTILLATION COLUMNS: The distillation columns consist of a stripping and a rectifying column.
The stream enters the stripping column first. Here,the rest of the maleic anhydride comes out
from the top as stream 5. 99% of the phthalic anhydride and all of the heavy impurity goes to
Stream 6 as per purity requirements.
Finally, stream enters the Rectifying column. Here, 99.9% of the phthalic anhydride, and any
remaining maleic anhydride go to Stream 7, and all of the heavy impurity goes to Stream 8.
WASTE WATER STREAMS: Sources of waste water are steam boiler blowdown and scrubber.
HEAT TRANSFER CIRCUITS: The process employs two heat-transfer systems: (1) a dowtherm
system which removes heat from the reactor. This is important because the reactor reactions are
highly exothermic and heat need to continuously be removed to minimize by-product formation
and conserve the catalyst. (2) an organic fluid (diathermic oil) system that heats and cools the
switch condenser.
12
5 PREPARATION OF PROCESS FLOW DIAGRAM
13
5.2 PFD
14
6 MASS BALANCE
Feed Streams:
Assumptions:
Reaction 1 has a selectivity of 70%, Reaction 2 has 10% ,Reaction 3 has 15% and Reaction 4
has 5%
Air : O-xylene ratio = 20:1 by weight
PAN is being manufactured in excess of 2%
CO2 , CO
A. Molecular Weights:
Phthalic Anhydride – 148
Maleic Anhydride – 98
O-xylene – 106
B. Considering loss of 2 %, PA to be produced = 10,200 kg/hr
15
required
MA 98.46*0.1 9.846
produced
CO2 (98.46*0.1*4)+(98.46*0.15*8) 157.534
produced
H2O (68.92*3)+(98.46*0.1*4)+(98.46*0.15*5)+(98.46*0.05*5) 344.614
produced
CO 98.46*0.05*8 39.38
produced
Air 98.46*106*20 (208735.2/29)
= 7197.77
O2 7197.77*0.21 1511.53
N2 7197.77*0.79 5686.24
Oxygen Balance:
16
INDIVIDUAL MASS BALANCE:
Streams 1 2 3 4 5 6 7 8
(kg/hr)
O-xylene 10436. - - - - - - -
76
O2 48368. 33403. 33403. - - - - -
96 04 04
N2 159214 159214 159214 - - - - -
.72 .72 .72
CO2 - 6931.4 6931.4 - - - - -
96 96
H2O - 6203.0 6196.8 6.203 6.203 - - -
52 5
MAN - 964.90 1.93 962.97 953.38 9.6 9.5 0.1
8 8
PAN - 10200. - 10200. 10.2 10190 10169. <0.2
16 16 6
CO - 1102.6 1102.6 - - - - -
4 4
RESIDUE - 25.4 - 25.4 - 25.4 <0.5 25
17
8 ENERGY BALANCE
AIR PRE-HEATER:
Mass of air 208735.2 kg/hr
Cp 1.005 KJ/kgK
Tinlet 25 C
Toutlet 205 C
-7
E = m*Cp*(T2-T1) 3.7 X 10 KJ/hr
O-XYLENE VAPOURIZER
Mass of O-xylene 10436.76 kg/hr
Cp 1.71 KJ/kgK
Tinlet 25 C
Toutlet 205 C
Heat of Vaporization of O-xylene @ 144 C 341.88 KJ/Kg
E = m*Cp*(T2-T1) + m*Lv 6780399.584 KJ/hr
REACTOR
Mass of o-xylene 10436.76 kg/hr
Mass of oxygen 48368.96 kg/hr
Mass of nitrogen 159214.72 kg/hr
Mass of PAN 10,200.16 kg/hr
Mass of CO2 6931.496 kg/hr
Cp O-xylene @ 370 deg C 3.83 KJ/KgK
Cp Oxygen @ 370 deg C 1.017 KJ/KgK
Cp Nitrogen @ 370 deg C 1.086 KJ/KgK
Reactor inlet temp 370 C
Reactor outlet temp 205 C
Heat of formation of phthalic anhydride Hf 7500 KJ/Kg
Heat of combustion Hc 99545.45 KJ/Kg
E= mCp(T2-T1) + Heat liberated 766762159.7 KJ/hr
18
DOWTHERM COOLER:
Mass of dowtherm 4551057.453 kg/hr
Mass of BFW 359944 kg/hr
Enthalpy of superheated steam 3071 KJ/kg
Boiling point of water at 6000 kPa 276 C
Cp of dowtherm 2.808 KJ/kgK
Cp of BFW 1.041 KJ/kgK
Cp of HP steam 1.28 KJ/kgK
m*Cp(dowtherm)*(360-300) = m*Cp(BFW) *(276-165) +m(steam)*latent heat+ m(steam)*Cp*(315-276)
Mass of HP steam 232357.853 kg/hr
GAS COOLER:
Reaction gases @ 370C and 170KPa 218020.016 kg/hr
Cooled gases @ 205C 218020.44 kg/hr
Cp of oxygen @ 370C 1.017 KJ/kg K
BFW (from 70C to 165C and @6000 kPa) Cp 1.16 KJ/kg K
Cp of PAN @ 370 deg C 1.017 KJ/kg K
Cp of MAN @ 370 deg C 1.657 KJ/kg K
Cp of CO2 @ 370 deg C 1.102 KJ/kg K
Cp of CO @ 370 deg C 1.1 KJ/kg K
Cp of O2 @ 370 deg C 1.017 KJ/kg K
Cp of N2 @ 370 deg C 1.086 KJ/kg K
Cp of H2O (gas) @ 370 deg C 2.047 KJ/kg K
E = m(indiv)*Cp(indiv)*(370-205) 39665926.23 KJ/hr
SWITCH CONDENSER:
Cp of N2 @ 136 deg C 1.044 KJ/kg K
Cp of O2 @ 136 deg C 0.941 KJ/kg K
Cp of CO2 @ 136 deg C 0.939 KJ/kg K
Cp of CO @ 136 deg C 1.048 KJ/kg K
Cp of PAN @ 136 deg C 1.017 KJ/kg K
Cp of MAN @ 136 deg C 1.657 KJ/kg K
Cp of H20 @ 136 deg C 1.901 KJ/kg K
Switch Condenser inlet 136 C
Switch Condenser outlet 70 C
E = m*Cp(inlet gases)*(136-70) 217290.026 KJ/hr
19
DISTILLATION COLUMN - 1
Column feed inlet 250 C
Column Top Temperature 177 C
Column Bottom Temperature 254 C
Outlet temperature of MAN 55 C
Feed 11169.341 kg/hr
Distillate 969.783 kg/hr
Bottoms 10199.6 kg/hr
Assuming reflux ratio of 1.6
Total Overhead load = D(R+1) = 969.783(2.6) 2521.44 kg/hr
Feed composition:
MAN = (962.97/98)/((962.97/98)+(10200.16/148)) 0.124
PAN = (10200.16/148)/((962.97/98)+(10200.16/148)) 0.875
Cp avg = (0.124*1.657+0.875*1.017) 1.09 KJ/kg
Top composition:
MAN = (953.38/98)/((953.38/98)+(10.2/148)) 0.993
PAN = (10.2/148)/((953.38/98)+(10.2/148)) 0.007
Cp avg = (0.993*1.657+0.007*1.017) 1.64 KJ/Kg
Bottom composition:
MAN = (9.6/98)/((9.6/98)+(10190/148)) 0.0014
PAN = (10190/148)/((9.6/98)+(10190/148)) 0.9986
Cp = (0.0014*1.657+0.9986*1.017) 1.017 KJ/kg
Qc = 969.783*1.64*(177-55) + 2521.44*493 1437104.103 KJ
Qf = 11169.341*(1.09)*250 3043645.423 KJ
Qbp = 10199.6*1.017*254 2634740.273 KJ
Qtp = 969.783*1.64*177 281508.6092 KJ
Qb = Qc+Qbp+Qtp-Qf+Ql
Assuming Ql = 0.1Qb
Qb 1455230.624 KJ
Cooling water required = 1437104.103/(4.179*20) 17194.35 kg/hr
Steam required = 1455230.624/ 2257
1.984*10 73348.3645 kg/hr
20
9
Notation Mass Flow rate Avg Density Total Mass flow Volumetric Flow rate Fluid velocity Area Area (mm2) Diameter Diameter
3 3 2
(kg/sec) (kg/m ) rate (m /sec) (assumed)(m/s) (m ) (mm) (in)
CX 2.8991 880 2.8991 0.003294432 15 0.00022 219.62879 16.72668 0.658529
21
22
23
10 PNID
24
25
26
10.1 PNID EQUIPMENT LIST
Equipment No. Description
C101 Air compressor
D101 Heat transfer dowtherm drum
D102 Cold diathermic oil receiver
D103 Hot diathermic oil receiver
D104 Stripping column reflux accumulator
D105 Heater reflux accumulator
E101 O-xylene vaporiser
E102 Air preheater
E103 Dowtherm cooler
E104 Gas cooler
E105 After cooler
E106 & E107 Switch condenser
E108 Stripping column preheater
E109 Stripping column reboiler
E110 Heater reboiler
E111 Stripping column condenser
E112 Heater condenser
E113 Vapour sublime
E114 Diathermic oil cooler
E115 Diathermic oil heater
E116 MAN condenser
G101 O-xylene feed pump
G102 Dowtherm pump
G103 Cold diathermic oil pump
G104 Hot diathermic oil pump
G105 Crude PAN transfer pump
G106 Stripping bottoms pump
G107 Rectification bottoms pump
G108 Stripping column reflux pump
G109 Rectification reflux pump
G110 PAN product pump
G111 MAN product pump
M101 Air filter
R101 PAN reactor
T101 Stripping column
T102 Rectification column
Tk101/102 O-xylene tanks
Tk201 Crude PAN tank
Tk301/302 Product PAN tank
Tk303 Product MAN tank
27
11 MSDS
28
12 EQUIPMENT DESIGN
12.1 REACTOR DESIGN (PROCESS)
GAS
DOWTHERM
INLET OUTLET
GAS
INLET
DOWTHERM
OUTLET
MANHOLE
(450 X 400 mm)
A catalytic, tubular, fixed-bed type reactor will be used which is operated continuously for 8000
hours/year.
Basis:
= 218020/0.7022
= 310481.344 m3/hr
29
To find tubes required
Thus, number of tubes which are required to meet the design production requirements can be
calculated from:
Since tubes are 25mm in diameter the cross section area of each tube is
= (25 10-3) 2 = 4.9 10-4m2
4
From heat transfer consideration, reactor is 1-1 heat exchanger in which the tubes are packed
Stainless steel pipes are provided for process condition O.D = 30mm, I.D = 25mm,
thickness =5mm.
Tube arrangement: A standard 39.7 mm (1-9”) square pitch selected to allow easy cleaning
=7m
30
Effect of number of baffles on overall heat transfer coefficient and average coolant velocity can
be estimated with the help of the table mentioned below. According to the proposed plant
overall HT coefficient, 3 baffles are sufficient to provide adequate heat transfer. However, 5
baffles are preferred in order to maximize the heat transfer rate and allow an additional 600 mm
per pass which reduces the average velocity and minimises pressure drop.
Number of Shell Baffles Overall Heat Transfer Average Coolant Velocity (m/s)
Coefficient (W/m2/C)
0 172 0.1
1 182 0.2
3 191 0.4
5 195 0.6
7 198 0.8
9 200 1.0
Basis of 40 T/year Phthalic anhydride plant has considered the following dimensions:
On scaling up the dimensions to provide for the proposed capacity of 79,200 T/year,
31
Dowtherm Inlet ID = 840 mm
Considering Length of shell to be increased by 30% of the tube length, and making provisions for
= 4.5 m
Shell Tubes
Orientation - Vertical
Fluid Dowtherm Hydrocarbon vapour and air
Flow rate (kg/hr) 4551057.453 kg/hr 218020 kg/hr
Composition Pure 10.5% phthalic anhydride
Number 1
Dimensions 4550 X 7000 ID mm 3.5 m X 25 mm ID
Inlet Temperature 371 C 205 C
Outlet Temperature 385 C 370 C
32
12.2 DISTILLATION COLUMN DESIGN
Feed composition:
Top composition:
Bottom composition:
Distillation column is operated at a range of 177 deg C – 254 deg C and a pressure of 50 Kpa
33
To find alpha
From FenskeEquation :
From graph
Where,
Y = x*alpha/((alpha-1*x)+1)
From graph 1,
Y’ = 0.49
Rmin = 1.369
From graph 2,
34
Calculating y intercept for Ractual = 1.643
Average molecular weight of MAN and PAN in the feed = 0.124* 98 + 0.876*148 = 141.8 kg
PV = nRT
P = 0.493atm
Vapour density = 11.48*10^-3 * avg molecular weight = 141.8 * 11.48 * 10 ^-3 = 1.627 kg/m^3
Q = Velocity*Area
= 2.7 m/sec
35
12.2.2 PLATE LAYOUT
Column diameter 0.45 m
Column area 0.16 m2
0.88*column
Net area area = 0.141 m2
0.88*0.16 =
(1-
Active area 2*0.12)*Column 0.03 m2
area
Hole area 0.1*Active Area 0.003 m2
Weir Length 0.38 m
Assume
Wier Height 12 mm
Hole diameter 5 mm
Plate Thickness 5 mm
Weir liquid crest (how) = 750 *(liquid flow rate/(density of liquid*length of weir))^(2/3)
hw = 12 mm
Total plate pressure drop over the column = 9.81*10^-3*ht*rho liq= 9.81*10^-3*48.3*1181 = 560
Pa
Total pressure drop over the column = 560*21 = 11760 Pa = 11.76 KPa
36
12.2.4 OVERALL COLUMN EFFICIENCY
(Source : Physical Property Data Bank Appendix C, Richard and Coulson Vol 6)
Eo = 0.52782-0.27511log10(7.57*0.0885)+0.044923[log10(7.57*0.0885)]^2 = 0.52782 – ( -
0.04785) + 1.359*10^-3 = 0.577
Assuming 15 % for disengaging space at the top and holding space at the bottom,
12.2.6 NOZZLES
Feed inlet= 50 mm
Reflux inlet = 25 mm
Bottoms discharge = 50 mm
37
From Clausius Clapeyron Equation, enthalpy of overhead load = 493 KJ/Kg
dT2 = (55-20) = 35
Qc = UA dTlmtd
dT2 = (265-254) = 11
QR = UAdT
38
39
40
12.2.9 ENGINEERING SPECIFICATION SHEET FOR DISTILLATION COLUMN (T-101)
Distillation Column Data Sheet
Equipment Number: T-101 Item Number:
Function: Separation of Maleic Anhydride and Phthalic Anhydride
Operation: Continuous Date: 15.3.14
Design Data
Number of Plates 21
Feed Point location 5
Height of column 12.075 m
Diameter of column 0.45 m
Column Area 0.16 m2
Plate spacing 0.5 m
Hole Area 0.003 m2
Active Area 0.03 m2
Minimum Reflux Ratio 1.369
Actual Reflux Ratio 1.643
Weir Length 0.38 m
Hole diameter 5 mm
H/D ratio 26.8
Type of Trays Sieve
MOC SS-316
Operating Conditions
Feed temperature 250 deg C
Top temperature 177 deg C
Bottom temperature 254 deg C
Pressure 50 Kpa
Density of Liquid 1181 kg/m3
Density of Vapour 0.3381 kg/m3
Vapour discharge
Reflux entry
Feed entry
Steam inlet
Bottoms exit
41
13. OSBL SPECIFICATIONS
Tank Dimensions :
Assume H/D ratio 0.5
Assuming 10% extra
volume
Volume (pi/4)*D^2*(0.5D)= 2946.84+(0.1*2946.84)
D 20.20 m
H 10.1 m
Tank Dimensions :
Assume H/D ratio 0.5
Assuming 10% extra
volume
Volume (pi/4)*D^2*(0.5D)= 1008.5+(0.1*1008.5)
D 14.1 m
H 7.07 m
42
Maleic Anhydride Product Tank
Process objective: 21 days supply
Tank Dimensions :
Assume H/D ratio 1
Assuming 10% extra
volume
Volume (pi/4)*D^2*(D)= 442.1+(0.1*442.1)
D 8.52 m
H 8.52 m
Tank Dimensions :
Assume H/D ratio 1
Assuming 10% extra
volume
Volume (pi/4)*D^2*(D)= 202.31+(0.1*202.31)
D 6.56 m
H 6.56 m
43
Dowtherm Storage Tank
Process objective: 3 hrs supply
Tank Dimensions :
Assume H/D ratio 0.5
Assuming 10% extra
volume
Volume (pi/4)*D^2*(0.5*D)= 6464.57+(0.1*6464.57)
D 26.25 m
H 13.12 m
Tank Dimensions :
Assume H/D ratio 0.5
Assuming 10% extra
volume
Volume (pi/4)*D^2*(0.5*D)= 1101.86+(0.1*1101.86)
D 14.55 m
H 7.27 m
44
Diatherm Oil Storage Tank
Process objective: 3 hrs supply
Tank Dimensions :
Assume H/D ratio 0.5
Assuming 10% extra
volume
Volume (pi/4)*D^2*(0.5*D)= 1692.7+(0.1*1692.7)
D 16.79 m
H 8.39 m
Cooling Tower
Process objective: 24 hrs supply
45
13 PLANT LAYOUT
46
The economic construction and efficient operation of a process unit will depend on how well the
plant and equipment specified on the process flow sheet is laid out.
Personnel and service buildings should almost never be downwind. The control room is also to
the north of the plant to protect it in the event of an emergency. The small overall size of the
plant allows the control room to be located away from the centre of the main processing
equipment. In the event of an emergency, the plant can be viewed (line of sight) from both the
office buildings and the control room.
Storage facilities will be located reasonably close to both the feed point and the product
discharge point which minimises piping and pumping costs. The loading station can be accessed
easily via the main entrance. Clearance around the storage areas is low but should be sufficient in
emergency situations.
The process equipment is split into two areas: reaction and purification. This separates the
potentially hazardous reactor from other equipment. In the event of an accident, the prevailing
winds should carry vapours away from other equipment.
Market conditions suggest that future expansion will be very limited. If necessary, there is
sufficient space for the de-bottlenecking of major items of equipment (for example, a second
reactor could be added).
Medical facilities and other essential services will be shared with other industries on the site.
Senior management, secretarial, personnel and accounting staff will also be housed in the same
building, away from the process operations. The small size of the phthalic anhydride plant
precludes the need for non-operational staff to be on site.
47
Plant Boundary particulars are estimated as follows:
1 Plant Area
1. Main Plant 534.4
2. Raw Material Storage 332.35
3. Instrumentation and Lab 400.00
4. Utility 933.1
5. Product Storage 214.35
6. Fire Safety Station 600.00
7. Roads 1225.00
8. Empty Space (Garden, Drainage) 1369.00
TOTAL 5608.2 m2
2 Administration
1. Admin Office 300.00
2. Technical Support Offices/Canteen 400.00
3. Car Park 196.00
4. Warehouse 200.00
5. Control Room 100.00
6. Roads 900.00
7. Garden 400.00
TOTAL 2496 m2
TOTAL AREA 8104.2 m2
Plant Boundary Length 70 m
Plant Boundary Breadth 120 m
48
The main plant area has been calculated after considering the following equipments :
Heater 7 3.5 80 m2
Miscellaneous Heat
Exchangers (8) 6.35 3.175 63.3 m2
The ground area covered by the storage tanks in the main plant area is as follows :
49
14 SAFETY, HEALTH AND ENVIRONMENT
The most serious process hazard is the potential for phthalic anhydride dust clouds to form
following process breaches. The condensers will be the primary point of risk but other
equipment, including the storage tanks (if proper heating is not maintained) and the reactor are
also possible sources. At low concentrations (less than 1%), PAN dust is a serious health risk. At
higher levels (1.5-10.5%), PAN dust is a major explosion hazard. A level of 10,000 ppm (1 %) PAN
in the atmosphere is immediately dangerous to life, but a lower concentration also poses a health
risk and is an eye, nose and skin irritant.
Respirators will always be available from the control room for use in susceptible areas,i.e.
dust and mist respirators at less than 10 ppm, air purifiers at less than 50 ppm, and
positive-pressure respirators with face masks for emergency conditions up to 2000 ppm.
Health and safety standards require a minimum of 3 ppm PAN and 0.05 ppm MAN for safe
working environments before acute or chronic effects are detectable. These standards will
be met through appropriate process design and operating precautions.
Phthalic anhydride dust is explosive at concentrations of 1.5-10.5% in air. As there is always the
possibility of process leaks (even at very low probabilities), all sources of ignition and non-
intrinsically safe equipment will be excluded from the site, except within the main buildings.
High-risk zones will be identified and equipped with air quality monitors to detect dust
before it reaches a hazardous level.
The three areas of highest risk are the condensers, reactor and storage vessels. The areas
where these items are located are separated from other items of equipment to prevent
an explosion in one area triggering an explosion in another.
A fire station, manned by specially trained process operators, will be located near the
process equipment in order to access and contain any fires before they become difficult
to manage.
Protective equipment will be made available to all employees and a mandatory policy for
the use of safety glasses and hard hats will be implemented.
Dust respirators and filters will be available in the control room at all times.
Monitoring programs will be established to ensure that the time-weighted average daily
exposure of workers to PAN or MAN is below the acceptable safety limits. Similar
regulations will apply to visitors.
AIRBORNE EMISSIONS
Normal operating conditions will produce only two significant discharges to the environment
which are :
50
non-condensable reaction by-products that remain with the air as it is rejected from the
process to the environment;
heavy residue from the bottoms of the rectification column.
The reaction by-products are mostly light organic vapours. A scrubbing unit will be installed in
order to reduce the concentrations of contaminants to less than 25 ppm PAN and 10 ppm maleic
anhydride prior to discharge to the atmosphere. A 50 m stack should disperse these
concentrations to acceptable levels. The total amount of PAN vented to the atmosphere will be
less than 1 kg/hr. The bottoms will be transferred to another local chemical manufacturer for
reprocessing to recover valuable components and, therefore, will not contribute to daily
emissions.
WATERBORNE EMISSIONS
Water is not part of the phthalic anhydride process and will not come into direct contact with any
process stream in the system. Air coolers will be used to satisfy most of the process cooling
requirements so that cooling water usage will be minimal.
Steam requirements will be essentially met by the process itself using the heat generated by the
PAN reaction.
Process contaminants that might enter the steam system through exchanger leaks or other
process disturbances will be scrubbed at the shared utilities plant, so that condensate can be
recycled to reduce energy consumption and chemical treatment costs.
SOLID WASTE
Due to the small volumes of waste to be processed, the incinerator will only be operated on a
batch basis, and a small sump will be installed to collect residue during normal operation. This
would allow incinerator operation to be scheduled only when wind conditions were suitable (e.g.
not calm days). It would also reduce the risk of incinerator failure as it would allow a routine
cleaning and maintenance program to be established.
To achieve this aim, safety and plant operation must be considered at several stages in the
preliminary design work and it is necessary to perform a detailed and complete safety analysis.
This study should identify aspects of the design that may cause operational or safety problems,
and also any modifications necessary to the equipment design (or the control scheme) which will
minimize the effects of changes in the plant operating conditions.
The following activities are carried out in order to achieve these aims.
51
(a) A safety review of all equipment designs, e.g. design to appropriate standards and observation
of design code recommendations. However, mistakes do occur and a second opinion and review
by a group of experts can help to uncover some errors.
(b) Loss Prevention Studies. Loss prevention is the general name given to the activities that help
provide anticipatory safety measures for the prevention of accidents.
Operability Studies, provide a systematic and critical examination of the operability of a process.
They indicate potential hazards due to deviations from the intended design conditions. The
techniques can be applied to existing p lants, and should be standard procedure at the process
design stage of new plants.
(ii) Failure Analysis, The overall reliability of a chemical plant can be calculated from the reliability
of individual components, additional consideration is then given to parts of low reliability, e.g.
duplication of equipment.
(iii) Hazard Analysis (HAZAN)is a technique for the quantitative assessment of a hazard, after it
has been identified by an operability study, or similar technique. HAZAN is used to compare risks
to life per hour of exposure. Attention is concentrated on those risks which exceed a given
acceptable value, e.g. 3 deaths per 10 5 people per year.
(c) Quantitative Safety Analysis Techniques need to be applied to particular and appropriate
situations.
(i) Quantitative Risk Assessment (QRA) investigates the risk involved in an incident and the
consequences, decisions are then made based on comparisons with various acceptance criteria.
All QRA is based on the construction of logic diagrams (either fault trees or event trees) showing
how the various causes of an incident are related. Failure data is used to quantify the logic trees.
(ii) Consequence Modelling evaluates the consequences of an incident on people, property and
land (Le. the environment). The problem that is specific to a chemical plant is that an incident
may result in either the release of a toxic or flammable material, or an uncontrollable release of
energy. The effects may be both long-term and distant from the plant site. This approach is quite
complex and it is essential to appreciate the limitations of the methods, models, and data that
are being used.
(iii) Evaluation of Human Factors: Human error can never be totally eliminated and therefore
available models and methods must be used to evaluate the probability of human error and to
assess the consequences.
52
The following summary describes the relevant SHE compliance studies required during the
various stages of a Phthalic Anhydride plant:
53
15 FINANCIAL ANALYSIS
The cost of a complete plant can be estimated using the 'seventh-tenth rule' which states that: 'the ratio
of the costs of two plants producing the same product is proportional to the ratio of their capacities raised
to the power of 0.7'. This statement can be written as:
(C1/C2) = (Q1/Q2)0.7
Cost Break Up
% of Project Cost
Particulars
Cost (Crs)
Land & Site Development 3% 16.116
54
Profit & Loss
Year 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
Income
1041.0 1113.8 1191.8 1275.2 1364.5
Sales (in Cr) 463.32 533.89 648.29 693.67 742.23 794.19 849.78 909.26 972.91 1 9 6 9 6 1460.08
EXPENDITURE
Raw Material 222.39 256.27 311.18 332.96 356.27 381.21 407.89 436.45 467.00 499.69 534.67 572.09 612.14 654.99 700.84
Power & Fuel 60.23 69.41 84.28 90.18 96.49 103.24 110.47 118.20 126.48 135.33 144.81 154.94 165.79 177.39 189.81
Employee Cost 9.27 10.68 12.97 13.87 14.84 15.88 17.00 18.19 19.46 20.82 22.28 23.84 25.51 27.29 29.20
Other Manufacturing
Expenses 13.90 16.02 19.45 20.81 22.27 23.83 25.49 27.28 29.19 31.23 33.42 35.76 38.26 40.94 43.80
Selling & Administration
Expenses 23.17 26.69 32.41 34.68 37.11 39.71 42.49 45.46 48.65 52.05 55.69 59.59 63.76 68.23 73.00
Miscellaneous Expenses 9.27 10.68 12.97 13.87 14.84 15.88 17.00 18.19 19.46 20.82 22.28 23.84 25.51 27.29 29.20
FIXED COST
1065.8
Total Expenditure 338.22 389.74 473.25 506.38 541.83 579.76 620.34 663.76 710.22 759.94 813.14 870.06 930.96 996.13 6
Operating Profit 125.10 144.15 175.04 187.29 200.40 214.43 229.44 245.50 262.69 281.07 300.75 321.80 344.33 368.43 394.22
EBIDTA 110.10 130.43 150.04 187.29 200.40 214.43 229.44 245.50 262.69 281.07 300.75 321.80 344.33 368.43 394.22
Depreciation 94.55 74.35 58.58 46.23 36.54 28.92 22.92 18.19 14.44 11.48 9.13 7.27 5.79 4.61 3.68
EBIT 15.55 56.08 91.46 141.06 163.86 185.51 206.52 227.31 248.24 269.59 291.62 314.53 338.54 363.82 390.54
Interest 32.22 32.22 30.87 29.52 28.17 26.37 24.57 21.87 19.17 16.47 13.77 11.07 8.37 5.67 2.97
EBT - 23.86 60.59 111.54 135.69 159.14 181.95 205.44 229.07 253.12 277.85 303.46 330.17 358.15 387.57
Tax - 7.87 20.00 36.81 44.78 52.52 60.04 67.80 75.59 83.53 91.69 100.14 108.96 118.19 127.90
Profit After Tax - 15.99 40.60 74.73 90.91 106.62 121.91 137.65 153.48 169.59 186.16 203.32 221.21 239.96 259.67
Depriciation Table
Total 94.55 74.35 58.58 46.23 36.54 28.92 22.92 18.19 14.44 11.48 9.13 7.27 5.79 4.61 3.68
Debt Schedule
year 1 year 2 year 3 year 4 year 5 year 6 year 7 year 8 year 9 year 10 year 11 year 12 year 13 year 14 year 15
Debt Outstanding 358 358 358 343 328 313 293 273 243 213 183 143 103 63 23
Interest Repayable (@9%) 32.22 32.22 32.22 30.87 29.52 28.17 26.37 24.57 21.87 19.17 16.47 12.87 9.27 5.67 2.07
Debt Repaid 0 0 15 15 15 20 20 30 30 30 40 40 40 40 40
Total Paid 32.22 32.22 47.22 45.87 44.52 48.17 46.37 54.57 51.87 49.17 56.47 52.87 49.27 45.67 42.07
Hence
Debt Required 358
Equity 179.0666667
Cash Flow Table
Discounting at 9%
Year 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
Cash OutFlow
Intial Investment 537.2
Cash Inflows
Profit After Tax 15.99 40.60 74.73 90.91 106.62 121.91 137.65 153.48 169.59 186.16 203.32 221.21 239.96 259.67
Depriciation 94.55 74.35 58.58 46.23 36.54 28.92 22.92 18.19 14.44 11.48 9.13 7.27 5.79 4.61 3.68
Total Cash Inflow 94.55 90.34 99.17 120.96 127.45 135.54 144.83 155.83 167.92 181.07 195.29 210.59 227.00 244.57 263.35
Discounted Cash Flow -537.2 86.74 76.03 76.58 85.69 82.84 80.82 79.23 78.21 77.32 76.49 75.68 74.87 74.04 73.19 72.30
NPV Yr 6 -48.49581391
NPV Yr 7 per day 0.240077118
Hence Number of Days for breakeven 202.0009836
Particulars Yr1 Yr2 Yr3 Yr4 Yr5 Yr6 Yr7 Yr8 Yr9 Yr10 Yr11 Yr12 Yr13 Yr14 Yr15
ROI - 3% 8% 14% 17% 20% 23% 26% 29% 32% 35% 38% 41% 45% 48%
ROE - 9% 23% 42% 51% 60% 68% 77% 86% 95% 104% 114% 124% 134% 145%
PAT Margin - 3% 6% 11% 12% 13% 14% 15% 16% 16% 17% 17% 17% 18% 18%
16 CONCLUSION & RECOMMENDATIONS
Phthalic Anhydride is an important chemical intermediate. Its biggest application, accounting for
just over half of production, is in the manufacture of phthalate plasticizers, the main product
being dioctyl phthalate (DOP) which is used as a plasticizer in polyvinyl chloride (PVC). Hence, the
consumption of PA is mainly dependent on the growth of flexible PVC, which is sensitive to
general economic conditions as it is consumed in the construction and automobile industries.
The following table provides a summary of the major parameters found from our study:
It can be seen from the study that the cost of setting up a Phthalic Anhydride plant is financially
viable with an internal rate of return (IRR) of 20.80%, and more so because it is highly profitable
given its recent increasing demand on a year-on-year basis.
The improvements in PA industry mainly have been with respect to Air to o-xylene ratio, catalyst
modifications and energy saving devises. The performance of the new plants using the above
improved technologies need to be studied with respect to technical, economical and safety
angles. If found suitable, attempts should be made to study if the old plants can take advantage
of these new processes.
Technologies exist for recovery of off-gases to convert to useful by-products. They need to be
explored for application in existing units thereby avoid pollution and improve the plant
economics. This has become all the more attractive in view of the capacity expansions by most of
the units.
The plant proposed in this study can be set up at Jamnagar, Gujarat largely because of the
presence of petrochemical plants of Reliance Industries Ltd that is one of the dominant
manufacturers of O-xylene in India. Also, the proximity to Gulf of Kutch and location on the west
coast of India supported by world-class logistics and port facilities provides the Company with
freight advantages.
17 REFERENCES
1. Kirk-Othmer, Encyclopedia of Chemical Technology, 5th Edition, John Wiley & Sons, Inc.
2. Phthalic Acid and derivatives, Ullmann’sEncyclopedia of Industrial Chemistry, 5th Edition,
VCH
3. Perry, R.M., Green, D.W', Moloney, J.O. (1984) "Perry Chemical Engineers Hand Book" 6th
Edition McGraw Hill Book Co.
4. Detailed country statistics, charts, and maps compiled from multiple sources. Available
from: < http://www.indexmundi.com/ >.
5. Trusted market intelligence for the global chemical, energy and fertilizer industries.
Available from:
<http://www.icis.com/v2/chemicals/9076143/phthalic+anhydride/process.html>.
6. Ray, Sneesby. Chemical Engineering Design Project, a case study approach, 2 nd Edition,
Gordon and Breach Science Publishers
7. Mall, ID. Petrochemical Process Technology, Macmillan India Ltd
8. Phthalic Anhydride, McKettaEncyclopedia of Chemical Processes and Design, Vol. 34,
Marcel Dekker, New York (1990)
9. ICI, Safety Data Sheet, Phthalic Anhydride (1996)
10. Mahajani, V.V; Mokashi, S.M; Chemical Project Economics, Macmillan India Ltd.
11. Coulson, J.M. and Richardson, J.F., Chemical Engineering Volume 6
58