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Phthalic Anhydride

Design Project

Anisha Sharma - 216 Prarthna Shetty – 217


Contents
1 INTRODUCTION ........................................................................................................................................ 3
1.1 OVERVIEW ........................................................................................................................................ 3
1.2 MARKET CONDITIONS ...................................................................................................................... 4
1.2.1 GLOBAL MARKET ...................................................................................................................... 4
1.2.2 INDIAN MARKET ....................................................................................................................... 4
2 CAPACITY.................................................................................................................................................. 6
2.1 END USER MARKET .......................................................................................................................... 6
2.1.1 AUTOMOBILE INDUSTRY .......................................................................................................... 6
2.1.2 PVC ........................................................................................................................................... 6
2.1.3 PAINT INDUSTRY ...................................................................................................................... 6
2.2 PROPOSED CAPACITY ....................................................................................................................... 6
3 TECHNOLOGY SELECTION ........................................................................................................................ 7
3.1 AVAILABLE TECHNOLOGIES.............................................................................................................. 7
3.2 TECHNOLOGY SELECTED .................................................................................................................. 9
VAPOUR PHASE FIXED BED CATALYTIC OXIDATION OF O-XYLENE .......................................................... 9
4 PROCESS DESCRIPTION .......................................................................................................................... 11
5 PREPARATION OF PROCESS FLOW DIAGRAM ........................................................................................ 13
5.1 BLOCK DIAGRAM ............................................................................................................................ 13
5.2 PFD ................................................................................................................................................. 14
6 MASS BALANCE ...................................................................................................................................... 15
8 ENERGY BALANCE .................................................................................................................................. 18
9 LINE SIZING............................................................................................................................................. 21
10 PNID ................................................................................................................................................... 24
....................................................................................................................................................................... 24
10.1 PNID EQUIPMENT LIST ................................................................................................................... 27
11 MSDS .................................................................................................................................................. 28
12 EQUIPMENT DESIGN .......................................................................................................................... 29
12.1 REACTOR DESIGN (PROCESS) ......................................................................................................... 29
12.1.1 ENGINEERING SPECIFICATION SHEET FOR THE REACTOR (R101) .......................................... 32
12.2 DISTILLATION COLUMN DESIGN .................................................................................................... 33
12.2.1 DIAMETER OF COLUMN ......................................................................................................... 35
12.2.2 PLATE LAYOUT........................................................................................................................ 36
12.2.3 PLATE PRESSURE DROP .......................................................................................................... 36

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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.

Applications of PA  The phthalate plasticizers application


dominated the global market and accounted
for 56.5% of the overall demand in 2012.
Growing demand from the phthalate
plasticizers market and strong demand from
Plasticizers Asia Pacific were the major growth drivers for
PA.
10%  Another important market for PA is
Unsaturated unsaturated polyester resins, which
15%
polyesters
accounted for 18.1% share of the total PA
57% volume consumed in 2012.
18%
Alkyd resins
 The growing demand of phthalate plasticizers
in the production of polyvinyl chloride (PVC)
and unsaturated polyester resins in the
Others
manufacturing of fiberglass-reinforced plastic
(FRP) are expected to drive the global PA
market in the next six years.

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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.

Worldwide consumption of PA  The global PA market is dominated by Asia


Pacific, which accounted for 55.2% of
global volumes consumed in 2012.
 Growth of PA in Asia Pacific is principally
driven by the extensive use of PVC
27%
applications from growing end user
Asia Pacific
industries such as automobile and
Europe
55% construction in the region. It is the largest
ROW
18% PA market, in terms of both production
and consumption.
 Asia Pacific was followed by Europe with
17.8% share in total volume consumption.

1.2.2 INDIAN MARKET


With an aggregate installed capacity of 3,46,310 TPA across India, major PA producers include:

MANUFACTURER CAPACITY (TPA)


IG Petrochemicals Ltd 1,16,110 + 50,000 expanded
Thirumalai Chemicals Ltd 1,45,000
Asian Paints Ltd 25,200
S.I. Group 10,000

 Apparent consumption of PA in INDIA was 2,68,806tons in 2012-2013.


 Capacity Utilization of the domestic industry is deemed to be around 75%.
 Mysore Petrochemicals Ltd with a capacity of 12,000-tpa shut down it’s plant as the
operation had been incurring cash losses.

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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.

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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.

2.1.3 PAINT INDUSTRY


The Indian paint industry is valued at Rs 26,000 crore with 71 per cent of it being decorative
paints and the remaining being industrial. In volume terms, the size of the industry is 3.1 million
tonnes with decorative paints being 2.4 million tonnes and industrial paints being 0.7 million
tonnes. The paint market is estimated to double to Rs 50,000 crore by 2016 with per capita
consumption increasing to over 4 kgs from 2.57 kgs. It is anticipated that this sector will post a
CAGR of around 15% during FY 2012 to FY 2015.

2.2 PROPOSED CAPACITY


PARAMETER VALUE (MT)
Production in India in FY 12-13 2,25,262
Consumption in India in FY 12-13 2,68,808
Gap 43,546
---Gap in PA demand for PVC industry 0.29*43546 = 12629
---Gap in PA demand for Paint industry 0.28*43546 = 12193
---Gap in PA demand for other apps 18724
Forecasted rise in PVC demand by 2016 49%
Forecasted rise in Paint demand by 2016 15% (CAGR)
Capacity Utilization 75%
Capacity calculation (43546/0.75)+(0.49*12629)+((1.15^3)*12193)
CALCULATED CAPACITY 82800
PROPOSED CAPACITY Assuming
 330 working days in a year
 10 mT/hr production
Capacity = 330*10*24 = 79200 mT/year

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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.

Advantages of fluidized bed over fixed bed

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.

3. More efficient condensation of phthalic anhydride- A substantially lower air:naphthalene


ratio makes possible the more efficient condensation of the reaction product because of
its greater partial pressure in the product gases. Operating the reactor at increased
pressure permits the condensation of 50% or moreof the product directly as liquid, the
balance being condensed as solid in switch condensers. The lower concentration of
oxygen in the product gases, compared with that obtained in fixed-bed plants, reduces
the hazard of fire and explosion down stream from the reactor.

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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.

6. Operation at increased pressure- The operation of fluidized-catalyst reactors at increased


pressure (1 to 2 atm. gauge) permits a substantial increase in the output of a particular
unit compared with its capacity at atmospheric pressure.

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:

Process Criteria Oxidation of O-xylene using a Oxidation of Naphthalene


fixed bed vapor-phase using fluidized bed vapor phase

Raw material Cost Lower Higher


(it is in an impure form)

Raw material availability More available Less available


(coal tar naphthalene)

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Safety: Less More
1. CO2 emission
2. Processing Higher (350 to 500) Lower (340 to 385)
Temperature

PA Yield Higher (Complete combustion) Lower

3.2 TECHNOLOGY SELECTED

VAPOUR PHASE FIXED BED CATALYTIC OXIDATION OF O-XYLENE


Basis for selection:

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.

3. Safety Health and Environment Compliance :


Potential emissions to the environment from the proposed phthalic anhydride plant have
been assessed in two categories:

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(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.

5. Valuable Intermediates and Co products:


A Large amount of steam is generated which can be reused for energy purposes. Maleic
anhydride produced can be sold.

6. Catalyst Recovery :
Not much loss of catalyst as it is a fixed bed process

7. Backward and Forward Integration :


Large quantity of Maleic Anhydride would need to be produced for forward integration.

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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 technology consists of 4 main phases:

 Oxidation (performed in reactor block),


 Recuperation of Phthalic Anhydride from reactor off-gases (performed in switch
condensing section) and
 Refining to commercial product (performed in distillation unit)
 Flaking and packing system

Any of Phthalic Anhydride production technologies include sub sections as:

 Steam system – energy recuperation


 Waste gases incineration
 Recovery of Maleic anhydride from off gases of switch condensers

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.

In the reactor, four reactions occur:

1. C8H10 + 3O2 C8H4O3 + 3H2O


2. C8H10 + 7.5O2 C4H2O3 + 4H2O + 4CO2
3. C8H10 + 10.5O2 8CO2+ 5H2O
4. C8H10 + 6.5O2 8CO+ 5H2O
The selectivity for the phthalic anhydride reaction is 70%, for the complete combustion of o-
xylene is 15%, for the incomplete combustion of o-xylene is 5%, for maleic anhydride is 9%, and
for the heavy impurity is 1%.

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.

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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.

INCINERATOR: The switch-condenser off-gas is treated by a scrubber-incinerator combination.


Scrubbers are employed to recover Maleic anhydride before sending the rest of the gases to the
incinerator for safe disposal. Another thermal incinerator treats all the waste streams from the
product purification section (Distillation towers) of the plant.

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.

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5 PREPARATION OF PROCESS FLOW DIAGRAM

5.1 BLOCK DIAGRAM

13
5.2 PFD

14
6 MASS BALANCE

Feed Streams:

1. C8H10 + 3O2 C8H4O3 + 3H2O


2. C8H10 + 7.5O2 C4H2O3 + 4H2O + 4CO2
3. C8H10 + 10.5O2 8CO2+ 5H2O
4. C8H10 + 6.5O2 8CO+ 5H2O

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%

Input Rate + Generation rate – Output Rate – Consumption Rate = Accumulation

CO2 , CO

AIR Maleic anhydride + Phthalic


O-XYLENE Anhydride + Water

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

C. Overall Mass Balance


Element Calculation Amount
(kmol/hr)
Phthalic 10200/148 68.92
Anhydride
O-xylene 68.92/0.7 98.46

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:

Reaction 1: 98.46*0.7 *3= 206.77 kmol/hr

Reaction 2 :98.46*0.1* 7.5= 73.845 kmol/hr

Reaction 3: 98.46*0.15*10.5 = 155.07 kmol/hr

Reaction 4: 98.46*0.05*6.5 = 32 kmol/hr

Total O2 consumed = 206.77+73.845+155.07+32 = 467.685kmol/hr

O2 unreacted = 1511.53- 467.685 = 1043.845kmol/hr

Stream_in Kmol/hr Kg/hr Stream_out Kmol/hr Kg/hr

O-xylene 98.46 10436.76


O2 1511.53 48368.96 CO 39.38 1102.64
N2 5686.24 159214.74 MA 9.846 964.908
PA 68.92 10200.16
O2 1043.845 33403.04
N2 5686.24 159214.72
CO2 157.534 6931.496
H2O 344.614 6203.052
TOTAL 218,020.44 TOTAL 218020.016

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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

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8 ENERGY BALANCE

Delta (Energy of system) = E in – E out

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

Latent Heat of Vaporization Lv of MP steam @ 215 C 1878.25 KJ/Kg


Mass of MP steam = E/Lv 20103.93 Kg/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

Condensate @ 215 deg C (MP Steam) Lv 1878.25 KJ/kg


Mass of MP steam = E/Lv 3609.955 kg/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

Dowtherm inlet 300 C


Dowtherm outlet 360 C
Cp of dowtherm 2.808 KJ/kgK
Mass of dowtherm = E/Cp*(T2-T1) 4551057.453 kg/hr

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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

Cp of BFW 1.16 KJ/kg K


BFW inlet 70 C
BFW outlet 165 C
Mass of BFW = E/Cp (T2-T1) 3,59,944 kg/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

Cp of diathermic oil 1.86 KJ/kg K


Mass of diathermic oil = E/ Cp*(60-45) 5,14,019.41 kg/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

HX 2.8991 6.4 2.8991 0.452984375 15 0.030199 30198.958 196.1377 7.721943


LINE SIZING

CA 57.66213333 2.9 57.66213333 19.88349425 20 0.994175 994174.71 112.5373 4.430594

CF 2.8991 1.65 60.56123333 36.70377778 25 1.468151 1468151.1 136.7573 5.384135


57.66213333

RO 9.278622222 0.8 60.56111556 75.70139444 30 2.52338 2523379.8 179.2902 7.058654


44.22631111
1.925415556
1.72307
0.26803
2.833377778
0.306288889

GC 9.278622222 0.7 60.56111556 86.51587937 30 2.883863 2883862.6 191.6693 7.546019


44.22631111
1.925415556
1.72307
0.26803
2.833377778
0.306288889

AC 9.278622222 0.55 60.56111556 110.1111192 30 3.670371 3670370.6 216.2321 8.513057


44.22631111
1.925415556
1.72307
0.26803
2.833377778
0.306288889

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)

To find volume of reactor

A catalytic, tubular, fixed-bed type reactor will be used which is operated continuously for 8000
hours/year.

Basis:

Total mass flow rate = 218020 kg/hr

Volumetric flow rate = Mass flow rate/ Density

= 218020/0.7022

= 310481.344 m3/hr

29
To find tubes required

Standard reactor tube diameter is accepted as 25 mm and tube length 3.5 m.

Catalyst particle diameter dp = 3 mm

Catalyst particle density = 1600 kg/m3

The hydrocarbon feed rate is limited by the catalyst activity to 340g/hr/tube.

Thus, number of tubes which are required to meet the design production requirements can be

calculated from:

79200000 kg/yr / 8000 hr/yr


N=
0.340 kg/hr/tube

= 26, 000 tubes

Since tubes are 25mm in diameter the cross section area of each tube is


= (25 10-3) 2 = 4.9 10-4m2
4

Steel tubing data and inner diameter of shell Nozzle

From heat transfer consideration, reactor is 1-1 heat exchanger in which the tubes are packed

with catalyst bed.

Stainless steel pipes are provided for process condition O.D = 30mm, I.D = 25mm,

thickness =5mm.

Surface area/m inside = 4.9 10-4 m2

Surface area/m outside = 7.07 10-4 m2

Tube arrangement: A standard 39.7 mm (1-9”) square pitch selected to allow easy cleaning

between the parallel rows of tubes.Packing efficiency of 99% is assumed.

Diameter of the reactor shell,

Dmin = √ [(4/π) * 26000 * 0.03972 ] / 99% = 6.87

=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

Dimensions and Manhole Provisions

Basis of 40 T/year Phthalic anhydride plant has considered the following dimensions:

Dowtherm Inlet ID = 600 mm

Dowtherm Outlet ID = 600 mm

Gas inlet ID = 1000 mm

Gas Outlet ID = 1000 mm

Manhole = 450 X 400 mm

On scaling up the dimensions to provide for the proposed capacity of 79,200 T/year,

Scale-up factor = A1/A2 = 1.9

(π/4) D12 = (π/4) D22

(D1/D2) = √ 1.9 = 1.4

Proposed dimensions of new reactor will be as follows:

31
Dowtherm Inlet ID = 840 mm

Dowtherm Outlet ID = 840 mm

Gas inlet ID = 1400 mm

Gas Outlet ID = 1400 mm

Manhole = 450 X 400 mm

Considering Length of shell to be increased by 30% of the tube length, and making provisions for

nozzles and manhole fittings:

Overall height of reactor H = 1.3 * 3500 = 4550 mm

= 4.5 m

12.1.1 ENGINEERING SPECIFICATION SHEET FOR THE REACTOR (R101)


Catalytic, tubular, fixed-bed
Vessel reactor Operation Continuous

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

Mechanical Design Heat Transfer


Material Low-alloy chromium steel Heat Duty 213 MW
Cylindrical walls with ellipsoidal
Construction ends Overall HT Coefficient 195 W/m2C
Support Cylindrical skirt
Foundation Concrete footing
Catalyst Vanadium Pentoxide

32
12.2 DISTILLATION COLUMN DESIGN

Feed composition:

MAN = (962.97/98)/((962.97/98)+(10200.16/148)) = 9.826/(9.826+68.92) = 0.124

PAN = (10200.16/148)/((962.97/98)+(10200.16/148)) = 68.92/(9.826+68.92) = 0.876

Top composition:

MAN = (953.38/98)/((953.38/98)+(10.2/148)) = 9.728/(9.728+0.0689) = 0.993

PAN = (10.2/148)/((953.38/98)+(10.2/148)) = 0.0689/(9.728+0.0689) = 0.007

Bottom composition:

MAN = (9.6/98)/((9.6/98)+(10190/148)) = 0.097/(0.097+68.85) = 0.0014

PAN = (10190/148)/((9.6/98)+(10190/148)) = 68.85/(0.097+68.85) = 0.9986

MAN is the more volatile component.

Distillation column is operated at a range of 177 deg C – 254 deg C and a pressure of 50 Kpa

Using the Antoine Equation:

33
To find alpha

From FenskeEquation :

N = log ((Xd/(1-Xd))*((1-Xb)/Xb))/log alpha - 1

= log ((0.993/7*10^-3)*(0.9986/0.0014))/log 7.57 - 1= 4.69

Minimum number of trays required = 5

From graph

Where,

Y = x*alpha/((alpha-1*x)+1)

From graph 1,

Y’ = 0.49

Rmin/Rmin+1 = xd-y’/xd-x’ =( 0.993-0.49)/(0.993-0.124) = 0.578

Rmin = 1.369

Ractual = Rmin*1.2 = 1.369*1.2 = 1.643

From graph 2,

34
Calculating y intercept for Ractual = 1.643

Yintercept = xd/(Ractual+1) = 0.993/(1.643+1) = 0.375

From graph total trays = 12

Feed tray location = 5th tray

Tray type = Sieve trays

MOC of column = SS 316

12.2.1 DIAMETER OF COLUMN


(Source : Richard and Coulson, Vol 2)

Average molecular weight of MAN and PAN in the feed = 0.124* 98 + 0.876*148 = 141.8 kg

PV = nRT

P = 0.493atm

R = 0.08206 atm m^3/kmol K

T = 250 deg C = 523 K

n/V = P/RT = 0.493/(0.08206*523) = 11.48* 10 ^-3 kmol/m^3

Vapour density = 11.48*10^-3 * avg molecular weight = 141.8 * 11.48 * 10 ^-3 = 1.627 kg/m^3

Total overhead load =G= D(R+1) = 963.58(2.643) = 2546.74 kg/hr

Q = G/ Vapour density = 2546.74/1.627 = 1565.29 m^3/hr = 0.435 m^3/sec

Q = Velocity*Area

Vapour velocity = (-0.171 l2+0.27l-0.047) * (rhol –rhov/rhov)^(1/2)

Where l = plate spacing

Assuming plate spacing to be 0.5 m

Vapour velocity = (-0.171*(0.5^2)+0.27*0.5-0.047)*(1181-0.3381/0.3381)^0.5 = (-0.04275+0.135-


0.047)*(59.09)

= 2.7 m/sec

Area = Q/V = 0.435/2.7 =0.16 m^2

Area = (3.14/4) * Diameter^2

Thus diameter = (4*0.16/3.14)^0.5 = 0.45 m

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

12.2.3 PLATE PRESSURE DROP


(Source : Richard & Coulson, vol 6)

Dry plate drop (hd) = 51*(uh/Co)^2*(rho v/rho l)

Orifice Coefficient Co = 0.85

Vapour velocity uh = 2.7 m/sec

hd = 51*(2.7/0.85)^2*(0.3381/1181) = 0.15 mm liquid

Residual head (hr) = 12.5*10^3/rho l

hr= 12.5*1000/1181 = 10.58 mm liquid

Weir liquid crest (how) = 750 *(liquid flow rate/(density of liquid*length of weir))^(2/3)

how = 750*((10200/3600)/(1181*0.38))^(2/3) = 25.61 mm liquid

hw = 12 mm

Total Plate drop (ht) = hd+hr+(how+hw) = 0.15+10.588+(25.61+12) = 48.3 mm liquid

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)

Tray efficiency = Eo = 0.52782 – 0.27511log10(αµ) + 0.044923[log10(αµ)]^2

Log µ = VISA*((1/T)-(1/VISB)) , where VISA and VISB are constants

µMAN at 250 deg C = 0.09703 cP

µPAN at 250 deg C = 0.0874 cP

µmixture = (0.124*((0.09703)^(1/3))+(0.876*(0.0874)^(1/3)))^3 = (0.0569+0.388)^3 = 0.0885 cP

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

12.2.5 HEIGHT OF THE COLUMN


Actual number of trays = N(calculated)/efficiency = 12/0.577= 21

Height of column = No of actual trays * tray spacing = 21* 0.5 = 10.5 m

Assuming 15 % for disengaging space at the top and holding space at the bottom,

New height = 0.15*10.5+10.5 = 12.075 m

H/D ratio = 12.075/0.45 = 26.8

12.2.6 NOZZLES
Feed inlet= 50 mm

Vapour discharge = 175 mm

Reflux inlet = 25 mm

Bottoms discharge = 50 mm

12.2.7 AREA OF CONDENSER


Inlet temperature of vapours = 177 deg C

Outlet temperature of distillate = 55 deg C

Inlet temperature of water = 20 deg C

Outlet temperature of water = 40 deg C

Mass of vapours entering the condenser = 969.783 Kg/hr

Average Cp = = (0.993*1.657+0.007*1.017) = 1.64 KJ/Kg

Total Overhead load = D(R+1) = 969.783(2.6) = 2521.44 kg/hr

37
From Clausius Clapeyron Equation, enthalpy of overhead load = 493 KJ/Kg

Qc = 969.783*1.64*(177-55) + 2521.44*493 = 1437104.103 KJ = 399195.58 W

dT1 = (177 – 40) = 137

dT2 = (55-20) = 35

dTlmtd = (dT1-dT2)/(ln(dT1/dT2)) = (137-35)/ln(137/35) = 102/1.36 = 75 deg C

U = 800 W/m2K (Table 12.1 Richard and Coulson, Vol 6)

Qc = UA dTlmtd

A = Qc/(U*dTlmtd) = 399195.58/(800*75) = 6.64 m2

12.2.8 AREA OF REBOILER


Inlet temperature of distillation bottoms = 254 deg C

Outlet temperature of vapours = 258 deg C

Inlet temperature of steam = 275 deg C

Outlet temperature of steam = 265 deg C

dT1 = (275 – 258) = 17

dT2 = (265-254) = 11

From Energy balance,

QR = 1455230.624 KJ/hr = 404230 W

dTlmtd = (dT1-dT2)/(ln(dT1/dT2)) = (17-11)/ln(17/11) = 6/0.435 = 13.78 deg C

U = 1000 W/m2K (Table 12.1 Richard and Coulson, Vol 6)

QR = UAdT

A = QR/(U*dTlmtd) = 404230/(1000*13.78) = 29.33 m2

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

Ortho-Xylene Feed Tank


Process objective: 10 days cover at maximum feed rate

Quantity 10436.76 kg/hr


Weight 10 days*24hrs/day*10436.76 kg/hr 2504822.4 kg
Volume 2504822.4/850 2946.84 m3

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

Phthalic Anhydride Product Tank


Process objective: 5 days supply at maximum product
rate

Quantity 10169.6 kg/hr


Weight 5 days*24hrs/day*10169.6 kg/hr 1220352 kg
Density 1210 kg/ m3
Volume 1220352/1210 1008.5 m3

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

Quantity 964.908 kg/hr


Weight 21 days*24hrs/day*964.908 kg/hr 486313.632 kg
Density 1100 kg/ m3
Volume 486313.632/1100 442.1 m3

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

Phthalic Anhydride Pretreatment Tank


Process objective: 24 hrs supply to the purification
section

Quantity 10200.16 kg/hr


Weight 24hrs/day*10200.16 kg/hr 244803.84 kg
Density 1210 kg/ m3
Volume 244803.84/1210 202.31 m3

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

Quantity 4551057.453 kg/hr


Weight 3 hrs/day*4551057.453 kg/hr 13653172.36 kg
Density 1056 kg/ m3
Volume 13653172.36/1056 12929.14 m3

Consider 2 tanks, volume of


1 = 12929.14/2 = 6464.57
m3

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

BFW Storage Tank


Process objective: 3 hrs supply

Quantity 359,944 kg/hr


Weight 3 hrs/day*359,944 kg/hr 1079832 kg
Density 980 kg/ m3
Volume 1079832/980 1101.86 m3

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

Quantity 514,019.41 kg/hr


Weight 3 hrs/day*514,019.41 kg/hr 1542058.23 kg
Density 911 kg/ m3
Volume 1542058.23/911 1692.7 m3

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

Flow rate 2631.73056 m3/hr


Specific heat of water 1 Kcal/hr
Inlet water temperature 35 C
Outlet water temperature 25 C
Ambient wet bulb
temperature 23 C
Delta T 10
(flow rate*density*specific heat*temperature
TR difference)/3024 8.702812698

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.

The principal factors are considered are:

a) Economic considerations: construction and operating costs.


b) The process requirements.
c) Convenience of operation.
d) Convenience of maintenance.
e) Safety.
f) Future expansion.

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:

SN Particular Area (m2)

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 :

Equipment D (m) L (m) Area (m2)

Reactor 7 7.35 161.6 m2

Switch Condensers(2) 10.694 5.1 171.25 m2

Gas Cooler 6 3.175 56.5 m2

Pre-treatment Tank 5.5 3 51.8 m2

Stripping Column 0.4 14 0.125 m2

Heater 7 3.5 80 m2

Miscellaneous Heat
Exchangers (8) 6.35 3.175 63.3 m2

Pumps (8 + spares) 1 6.32 m2

The ground area covered by the storage tanks in the main plant area is as follows :

Storage Area D (m) H (m) Area (m2)

Diatherm Oil Storage Tank 16.79 m 8.4 m 221.6 m2

BFW Storage Tank 14.55 m 7.27 m 167.2 m2

Dowtherm Storage Tank 26.25 m 13.12 m 544.3 m2

Maleic Anhydride Product Tank 8.52 m 8.52 m 57.3 m2

Phthalic Anhydride Product Tank 14.1 m 7.07 m 157.05 m2

Ortho-Xylene Feed Tank 20.20 m 10.1 m 322.35 m2

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.

14.1 SAFETY, HEALTH AND ENVIRONMENT COMPLIANCE STUDIES


All process design activities must be carried out with the design objective of ensuring the safe
operation of the plant within acceptable risk levels.

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.

Some of the techniques that are used are described below:

(i) Hazard and Operability (MZOP) Studies, sometimes simply referred to as

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:

Project Stage Details of Study


1. Feasibility Evaluation Identify major hazards and inherent process
risks (toxic, explosive).

2. Process Design Systematic quantitative analysis of hazards


and definition of measures to reduce them,
refer to the P&ID.

3. Engineering Design Formal examination of engineering drawings


(and the P&ID) with quantitative hazard
analysis to ensure the above measures have
been implemented.

4. Construction Systematic check that hardware (as


constructed) and operating instructions are as
intended in the design.

5. Operation Post start-up review of all departures from


design affect ing safety, operating difficulties,
equipment failures, etc., with associated
hazard implications. Plant modifications and
changes in operating procedures or conditions
are checked for their effect on plant safety.

53
15 FINANCIAL ANALYSIS

Basis for project cost estimate:

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

Project Cost Using 7/10 Rule

IGPL project Cost (2011) 340 Crs


Hence IGPL Plant &
Machinery Cost at 50% 170
Project Cost
Crs Capacity
IGPL (2011) 170 50000
Our Plant ? 79200

Factor for capacity [Cap(Our)/Cap (IGPL)]^7/10 1.38


Hence Cost of Our P&M IGPL Cost * Factor 234.6 Crs

Hence Cost of our plant in 2011 prices 469.20 Crs


2013 prices with 7%
Cost of our plant 537.20 Crs
inflation

Cost Break Up
% of Project Cost
Particulars
Cost (Crs)
Land & Site Development 3% 16.116

Building & Civil Works 5% 26.86

Plant & Machinery 50% 268.6


Know How & Engineering 16% 85.952
Expenes on technitians 1% 5.372
Misc. Fix Assets 3% 16.116
Preoperative Expenses 10% 53.72
Contingency 8% 42.976
Preliminary & Capital Issue Expenses 1% 5.372
Margin Money 3% 16.116
Total Cost 100% 537.20

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

Pre-operative Expenses 15.00 13.72 25.00

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

Depreciation Schedule in Crores Yr 1 Yr 2 Yr 3 Yr 4 Yr 5 Yr 6 Yr 7 Yr 8 Yr 9 Yr 10 Yr 11 Yr 12 Yr 13 Yr 14 Yr 15

Plant and Machinery


408.2 408.2 408.2 408.2 408.2 408.2
Gross 408.27 408.27 408.27 408.27 408.27 408.27 408.27 408.27 408.27 7 7 7 7 7 7
Depreciation for the year 81.65 65.32 52.26 41.81 33.45 26.76 21.41 17.12 13.70 10.96 8.77 7.01 5.61 4.49 3.59
364.4 373.2 380.2 385.8 390.3 393.9
Cumulative Depreciation 81.65 146.98 199.24 241.04 274.49 301.25 322.65 339.78 353.47 3 0 2 3 2 1
Net 326.62 261.29 209.04 167.23 133.78 107.03 85.62 68.50 54.80 43.84 35.07 28.06 22.44 17.96 14.36

Other Fixed Assets


Gross 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98 42.98
Depreciation for the year 12.89 9.02 6.32 4.42 3.10 2.17 1.52 1.06 0.74 0.52 0.36 0.25 0.18 0.12 0.09
Cumulative Depreciation 12.89 21.92 28.24 32.66 35.75 37.92 39.44 40.50 41.24 41.76 42.13 42.38 42.56 42.68 42.77
Net 30.08 21.06 14.74 10.32 7.22 5.06 3.54 2.48 1.73 1.21 0.85 0.59 0.42 0.29 0.20

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

ESTIMATED FINANCIAL REQUIREMENT


Project Cost Cr.s 537.20
Target D/E Ratio 2

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

Estimated Financial Outcomes

NPV Yr 6 -48.49581391
NPV Yr 7 per day 0.240077118
Hence Number of Days for breakeven 202.0009836

Payback Period ( In plant Days) 6 Years 202 Days


Internal Rate of Return (IRR) 12.14%

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:

Proposed Plant capacity 79200 TPA


O-xylene Fixed bed catalytic
Technology Selected
route
Project Cost Rs. 537.20 Crore
Plant & machinery Rs. 234.6 Crore
Breakeven point (in plant days) 6 Years 202 Days
Target D/E ratio 2
IRR 12.14%
Land Required (Approx.) 2 Acres

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

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