Group 2

PRODUCTION OF 40,000 TPA OF PHTHALIC
ANHYDRIDE FROM OXIDATION OF O-XYLENE
Session 2015-2019
Supervised by
Engr. Muhammad Rashed Javed
Engr Rabia Sabir
Group Members
Talha Imtiaz UW-15-Ch.E-BSc-001

Mohsin Ali Shah UW-15-Ch.E-BSc-037
Gul Muhammad UW-15-Ch.E-BSc-023
Jasim Khan UW-15-Ch.E-BSc-024
Department of Chemical Engineering,
Wah Engineering College,

University of Wah, Wah Cantt.
PRODUCTION OF 40,000 TPA OF PHTHALIC
ANHYDRIDE FROM OXIDATION OF O-XYLENE
This report is submitted to the Department of Chemical Engineering, Wah Engineering

College, University of Wah for the partial fulfilments of the requirement for the
Bachelor of Science
In
Chemical Engineering
Internal Examiner:
Name: _______________
Sign: ________________
External Examiner:
Name: _______________
Sign: ________________
Department of Chemical Engineering,

Wah Engineering College,
University of Wah, Wah Cantt.
i
Dedicated to our beloved parents and respected teachers whose
tremendous support and cooperation led us to this wonderful
accomplishment.
ii
ACKNOWLEDGEMENT
All praise to Almighty ALLAH, who provided us with the strength to complete this project report. All
respects are for His HOLY PROPHET (Peace Be Upon Him), whose teachings are true source of
knowledge & guidance for whole mankind.
Before anybody else we thank our parents who have always been a source of moral support. We are
indebted to our project advisor Engr. Rashed Javed for his worthy discussions, encouragement,
technical discussions, inspiring guidance, remarkable suggestions, keen interest, constructive criticism
& friendly discussions which enabled us to complete this report.
We are thankful to the Chairperson of our Department Prof. Dr. K.S Baig for providing facilities and
guidance. We are also thankful to project coordinator Engr Rabia Sabir and other teachers for their
keen and sincere efforts and suggestions that proved to be very helpful in achieving our goal.
iii
ABSTRACT
Phthalic Anhydride is the intermediate in the manufacturing of plastics. It is also used to produce
unsaturated polyester resins and alkyd resins. Alkyd resins made with Phthalic Anhydride are widely
used in the paints and coating industry. Phthalic Anhydride are also used in the pharmaceutical and
manufacturing of dyes, pigments, detergents, herbicides and insecticides fire retardant and poly ester
resins crosslinking agent
The goal of this project is to design an economically feasible and environmentally friendly process for
the production of 40,000 Ton per annum of Phthalic Anhydride via oxidation of o-xylene. In designing
the process we perform detailed calculations material & energy balance including design of major
equipment, cost analysis, instrumentation & process control, hazard & operability study and
environmental study
iv
Table of Contents
Chapter # 1 Introduction….....................................................................................................................1
1 Phthalic Anhydride: ....................................................................................................................... 1
1.1 Physical and Thermodynamic Properties: ............................................................................... 1
1.2 Chemical Reactions: ................................................................................................................ 2
1.3 Uses and Industrial Applications: ........................................................................................... 3
1.3.1 Plasticizers: ...................................................................................................................... 3
1.3.2 Unsaturated polyester resins: ........................................................................................... 4
1.3.3 Alkyd Resins: ................................................................................................................... 4
1.3.4 Pharmaceuticals: .............................................................................................................. 4
1.3.5 Other uses: ....................................................................................................................... 4
1.4 Production and Consumption in Pakistan: .............................................................................. 4
1.5 Production and Consumption in world: .................................................................................. 4
1.6 Future Trends: ......................................................................................................................... 5
1.7 Market Assessment: ................................................................................................................ 5
1.8 Handling: ................................................................................................................................. 6
1.9 Storage:.................................................................................................................................... 6
1.10 Transportation:..................................................................................................................... 6
Chapter # 2: Manufacturing Process…………………………………………………………………..7
2 Production method: ........................................................................................................................ 7
2.1 Production from naphthalene: ................................................................................................. 7
2.2 Production of O-xylene: .......................................................................................................... 7
2.3 Raw materials: ......................................................................................................................... 7
2.3.1 O-xylene:.......................................................................................................................... 7
2.3.2 Naphthalene: .................................................................................................................... 8
2.4 Comparison of Naphthalene & O-xylene Process: ................................................................. 8
2.5 Selection of BASF process: .................................................................................................... 9
2.6 Capacity Selection: .................................................................................................................. 9
2.7 Process description of selected process:.................................................................................. 9
2.8 Selection of Catalyst: ............................................................................................................ 10
2.9 Choice of a reactor: ............................................................................................................... 11
Chapter # 3: Material Balance………………………………………………………………………..14
v
3 Material Balance: ......................................................................................................................... 14
3.1 Material Balance Around Mixing Point: ............................................................................... 15
3.2 Material Balance Around Reactor (R-401): .......................................................................... 15
3.3 Material Balance around Flash Drum (F-501): ..................................................................... 18
3.4 Material Balance Around Distillation Tower (D-601): ......................................................... 22
Chapter # 4: Energy Balance………………………………………………………………………….27
4 Energy Balance: ........................................................................................................................... 27
4.1 Energy Balance around Air heater (E-201): .......................................................................... 27
4.2 Energy Balance O-Xylene Vaporizer (E-202): ..................................................................... 28
4.3 Energy Balance around Reactor (R-401): ............................................................................. 30
4.4 Energy Balance around Dowtherm A Cooler (E-205): ......................................................... 32
4.5 Energy Balance on Product Gas Cooler (E-203): ................................................................. 33
4.6 Energy Balance on Product Gas Cooler (E-204): ................................................................. 35
4.7 Energy Balance Around Distillation Column (D-601): ........................................................ 36
Chapter # 5: Equipment Design………………………………………………………………………38
5 Air Preheater design (E-201): ...................................................................................................... 38
5.1 Vaporizer Design: ................................................................................................................. 42
5.2 Reactor Design: ..................................................................................................................... 50
5.3 Gas Cooler Design (E-203): .................................................................................................. 57
5.4 Vapor liquid separator design ............................................................................................... 67
5.5 Dowtherm A Cooler Design (E-205): ................................................................................... 72
5.6 Distillation Column Design: ................................................................................................. 78
Chapter # 6: Mechanical Design……………………………………………………………………..94
6 Mechanical Design of Heat Exchanger: ...................................................................................... 94
Chapter # 7: Pumps and Compressor Calculations…………………………………………………..99
7 Pumps:.......................................................................................................................................... 99
7.1 Pump Types ........................................................................................................................... 99
7.1.1 Centrifugal Pumps ......................................................................................................... 99
7.1.2 Reciprocating Pumps ..................................................................................................... 99
7.1.3 Helical Rotor Pumps ...................................................................................................... 99
7.2 Selection Criteria of Pumps................................................................................................... 99
7.3 Pump Sizing Calculation Steps ............................................................................................. 99
vi
7.4 O- Xylene Pump (P-301): ................................................................................................... 100
7.5 Compressors ........................................................................................................................ 104
7.6 Positive Displacement Compressor ..................................................................................... 104
7.7 Dynamic compressor ........................................................................................................... 104
7.8 Compressor Sizing Calculation Steps ................................................................................. 104
7.9 Air Compressor (C-101) : ................................................................................................... 105
Chapter # 8: Cost Estimation………………………………………………………………………..109
8 Cost of Packed Bed Tubular Reactor: ........................................................................................ 109
8.1 Cost of Flash Separator : ..................................................................................................... 109
8.2 Cost of Air-Preheater : ........................................................................................................ 110
8.3 Cost of Gas Cooler (E-203):................................................................................................ 110
8.4 Cost of O-Xylene Vaporizer: .............................................................................................. 111
8.5 Cost of Dowtherm A Cooler: .............................................................................................. 111
8.6 Cost of Pump (P-301):......................................................................................................... 112
8.7 Cost of Pump (P-302):......................................................................................................... 112
8.8 Cost of Compressor: ............................................................................................................ 113
8.9 Cost of Distillation Column ................................................................................................ 113
8.10 Cost of Plates: .................................................................................................................. 114
8.11 Total Cost of Equipment In 2018: ................................................................................... 114
8.12 Direct Cost: ...................................................................................................................... 114
8.13 Indirect Cost: ................................................................................................................... 115
8.14 Variable Cost: .................................................................................................................. 115
8.15 Utilities: ........................................................................................................................... 116
8.16 Fixed Cost:....................................................................................................................... 116
8.17 Overhead Charges: .......................................................................................................... 117
8.18 Profitability Analysis: ...................................................................................................... 117
8.19 Total Income: ................................................................................................................... 118
Chapter # 9: Instrumentation and Control…………………………………………………………..119
9 Introduction ................................................................................................................................ 119
9.1 Importance of Process Control: ........................................................................................... 119
9.2 Process Control Terms: ....................................................................................................... 120
9.3 Hardware elements of control system: ................................................................................ 120
9.4 Classification of control systems: ....................................................................................... 120
vii
9.5 Control Scheme of Reactor: ................................................................................................ 121
Chapter # 10: HAZOP Study………………………………………………………………………..124
10 HAZOP: ..................................................................................................................................... 124
10.1 Perform a HAZOP ........................................................................................................... 124
10.2 Why HAZOP Carry out? ................................................................................................. 124
10.3 Guide words ..................................................................................................................... 124
10.4 HAZOP Study on Distillation Column............................................................................ 126
Chapter # 11: Environmental Study……………………………………..………………………….129
11 Introduction ................................................................................................................................ 129
11.1 Environmental Release: ................................................................................................... 129
11.2 Transport:......................................................................................................................... 129
11.3 Transformation /Persistence: ........................................................................................... 129
11.4 Health effects: .................................................................................................................. 130
11.5 Acute Effects: .................................................................................................................. 131
11.6 Sub chronic/Chronic Effects:........................................................................................... 131
11.7 Environmental effects: ..................................................................................................... 131
11.8 Personal Protection: ......................................................................................................... 132
12 References: ................................................................................................................................. 133

13 Appendix:……………………………………………………………………………………….135
viii
List of Figures
Figure 1.1: Phthalic Anhydride ............................................................................................................. 1

Figure 1.2: Structure ............................................................................................................................. 1
Figure 1.3: Industrial Applications ....................................................................................................... 3
Figure 1.4: Production in World ........................................................................................................... 5
Figure 3.1: Mixing Point..................................................................................................................... 15
Figure 3.2: Reactor (R-401) ................................................................................................................ 16
Figure 3.3: Flash Separator (F-501) .................................................................................................... 18
Figure 3.4: Distillation Column (D-601) ............................................................................................ 22
Figure 4.1: Air Preheater (E-201) ....................................................................................................... 27
Figure 4.2: O-Xylene Vaporizer (E-202) ............................................................................................ 28
Figure 4.3: Reactor (R-401) ................................................................................................................ 30
Figure 4.4: Dowtherm A Cooler (E-205)............................................................................................ 32
Figure 4.5: Product Gas Cooler (E-203) ............................................................................................. 33
Figure 4.6: Product Gas Cooler (E-204) ............................................................................................. 35
Figure 5.1: Vertical Separator ............................................................................................................. 68
Figure 5.2: Dowtherm A Cooler ......................................................................................................... 72
Figure 5.3: Maccabe Thiele Method…………………………………………………………………85
Figure 7.1: O-Xylene Pump .............................................................................................................. 100
Figure 7.8: Air Compressor (C-101)................................................................................................ 105
Figure 9.1: Control Loop on Reactor ............................................................................................... 135
Figure A.1: Relation Between Downcomer Area and Weir Lenth…………………………………135
Figure A.2: Weep Point Corelation…………………………………………………………………135
Figure A.3: Discharge Coefficient Sieve Plate……………………………………………………..136
Figure A.4: Maximum Allowable Stress…………………………………………………………...136
Figure B.1: Selection of Pump .......................................................................................................... 137
Figure B.2: Rule of thumbs for locating the process equipment ...................................................... 137
Figure B.3: Estimate Frictional pressure losses ED and ES ............................................................. 137
Figure B.4: Efficiency of Pump ........................................................................................................ 138
Figure B.5: Efficiency of Electric motor .......................................................................................... 138
Figure B.6: Stanadard Sizes .............................................................................................................. 139
Figure B.7: Selection of Compressor………………………………………………………………139
Figure B.8: Compressibility Factor………………………………………………………………..139
Figure B.9: Hydraullic Efficiency Graph………………………………………………………….140
Figure C.1: Cost of Equipment…………………………………….………………………………141
Figure C.2: Cost of Equipment…………………………………………………………………….141
Figure D.1: Heat Exchanger Tube Data…………………………………………………………...142
Figure D.2: Tube Sheet Layout……………………………………………………………………142
Figure D.3: Overall Design Coefficient…………………………………………………………...143
Figure D.4: Tube Side Return Pressure Losses…………………………………………………….143
ix
List of Tables
Table 1.1: Thermodynamic and Physical Properties ............................................................................ 2
Table 2.1: Comparison between two processes .................................................................................... 8
Table 2.2: Fractional Conversion of O-Xylene .................................................................................. 10
Table 2.3: Stream Table ...................................................................................................................... 13
Table 3.1: Inlet and Outlet Stream of Mixing Point ........................................................................... 15
Table 3.2: Inlet and Outlet Stream Of Reactor ................................................................................... 16
Table 3.3: Inlet and Outlet Stream of Flash Separator ........................................................................ 19
Table 3.4: Antoine Coefficient............................................................................................................ 19
Table 3.5: Flash Calculations .............................................................................................................. 20
Table 3.6: Antoine Coefficient............................................................................................................ 22
Table 3.7: Flash Calculations .............................................................................................................. 23
Table 3.8: Inlet and Outlet Stream of Distillation Column ................................................................. 24
Table 3.9: Molar Flow rate ................................................................................................................. 25
Table 3.10: Mass Flow rate ................................................................................................................. 26
Table 4.1: Heat Capacity..................................................................................................................... 29
Table 4.2: Heat Capacity..................................................................................................................... 30
Table 4.3: Heat of Formation .............................................................................................................. 31
Table 8.1: Total Cost of Equipment .................................................................................................. 114
Table 8.2: Direct Cost ....................................................................................................................... 114
Table 8.3: Indirect Cost ..................................................................................................................... 115
Table 8.4: Fixed Cost ........................................................................................................................ 116
Table 10.1: HAZOP Terminology .................................................................................................... 125
Table 10.2: HAZOP Study on Distillation Column .......................................................................... 126
x
Chapter # 1 Introduction
Chapter # 1
Introduction
1 Phthalic Anhydride:
Phthalic anhydride is the organic compound with the formula C6H4(CO)2O. It is the anhydride of
phthalic acid. Phthalic anhydride is a principal commercial form of phthalic acid. It was the first
anhydride of a dicarboxylic acid to be used commercially. Its IUPAC name is 2-benzofuran-1,3-dione
[1].Figure 1.1 shows the structure of phthalic anhydride and figure 1.2 shows the solid form of phthalic
anhydride
Figure 1.1: Structure Figure 1.2: Phthalic Anhydride
Phthalic anhydride obtained from catalytic oxidation of ortho-xylene and naphthalene .It was first
reported in 1836 by Augusta Laurent. Until World War II, Phthalic anhydride was manufactured
primarily by liquid phase oxidation of suitable feed stocks. The first method was oxidation of
naphthalene by sulfuric acid in the presence of mercury salts to form anhydride. This process was
patented in 1896. After World War 1, A process to make phthalic anhydride by oxidation of
naphthalene in the independently in Germany, with US patents being granted in 1930 and 1934.
Naphthalene from coal tar continued to be the feed stock of twice in both the United States and
Germany until the late 1950, when a storage of naphthalene coupled with availability of xylene from
a burgeoning petro chemical industry forced many companies to use O-xylene. Air oxidation of 90%
pure O-xylene to phthalic anhydride was commercialized in 1946.An advantage of O-xylene is the
theoretical yield to phthalic anhydride of 1.395 kg/kg. With naphthalene, two of the ten carbon atoms
are lost to carbon oxide formation and at most a 1.157 kg/kg yield is possible. Although both are
suitable feed stock, O-xylene is overwhelmingly favored. Coal tar naphthalene is used in some cases
e-g where it is readily available from coke operation in steel mills. Naphthalene can be produced by
hydro de-alkylation of substituted naphthalene’s from refinery operations but no refinery produced
naphthalene is used as feed stock. Alkyl naphthalene can be converted directly to phthalic anhydride
but at low yield [2]
1.1 Physical and Thermodynamic Properties:

In the production of PA xylene is used as a basic feed stock Maleic anhydride is produced as a
byproduct. The table below enlist the important physical, Chemical and thermodynamic properties of
PA, MA and xylene [2]
1
Table 1.1: Thermodynamic and Physical Properties
Properties Phthalic Anhydride Maleic Xylene

Anhydride
Molecular weight 148.12 98.06 106
Boiling point (oC) 284.5 202 144oC
Melting point 131 52.8 -24oC
Vapor pressure mmHg 1.2 0.2 7
Flash point (oC) 152 102 25
Heat of fusion (kJ/mol) 22.93 32.16 17.11
Heat of vaporization 65.3 54.8 24.70
(kJ/mol)
Specific gravity at 4 (oC) 1.213 1.46 0.86
Triple point (oC) 131 200 286.3
Heat of sublimation at 88.7 85.4 60.8
131oC (kJ/mol)
Heat of formation at -460 -470 59.14
25(oC) (kJ/mol)
Heat of combustion at -3259 -1389.5 -
25(oC) (kJ/mol)
Density g/cm3 1.215 1.48 0.88
Viscosity (cp) 1.19 0.61 1.104
Surface Tension (N/m) 0.0355 0.1101
Auto-Ignition (oC) 494 417 363
Appearance White Crystalline White Crystal Clear, Colorless
Solid liquid
Odor Irritating Odor Irritating Sweet
Decomposition:
Phthalic anhydride hydrolyzes rapidly in the presence of water forming phthalic acid. Half-life for
phthalic anhydride was 30.5 seconds at pH 7.24. At pH 6.8 the half-life of phthalic anhydride in water
was prolonged to 61 seconds.[2][3]
1.2 Chemical Reactions:

Phthalic anhydride is a versatile intermediate in organic chemistry, in part because it is bifunctional
and cheaply available.
Hydrolysis
Hydrolysis by hot water forms ortho-phthalic acid. Hydrolysis of anhydrides is not typically a
reversible process. Phthalic acid is however easily dehydrated to form phthalic anhydride. Above 180
°C, phthalic anhydride re-forms.
2
C6H4(CO)2O + H2O C6H4(CO2H)2

Phthalic Anhydride Water Phthalic Acid
Ammonolysis:
When phthalic anhydride is heated with aqueous ammonia gives 95–97% yield of phthalimide
Synthesis of Phenolphthalein:
Phenolphthalein can be synthesized by the condensation of phthalic anhydride with two equivalents of
phenol under acidic conditions.[4]
1.3 Uses and Industrial Applications:

Phthalic anhydride has a wide range of uses and application in chemical industry. Some of the uses of
phthalic anhydride are given below.
Uses of Phthalic Anhydride

Other uses
10%
Polymer resins
17%
Plasticizers
56%
Alkyl resins
17%
Plasticizers Alkyl resins Polymer resins Other uses
Figure 1.3: Industrial Applications
1.3.1 Plasticizers:
The primary use of phthalic anhydride is a chemical intermediate in the production of plastics from
vinyl chloride (CH2=CHCL). Phthalic esters, which function as plasticizers, are derived from phthalic
anhydride like dioctylphthalate (DOP), di-iso-decyl phthalate (DIP), n-butyl benzyl phthalate.
Phthalate plasticizers are used for the production of the flexible and softer PVC products. Such as
3
cables, pipes, leather cloth, shoes film for packaging etc. .The alcoholysis reaction the basis of the
manufacture of phthalate esters. In the 2010s, approximately 8.5×109 kg of these esters were produced
annually, and the scale of production was increasing each year, all from phthalic anhydride
C8H4O3 + ROH C6H4(CO2H)CO2R
1.3.2 Unsaturated polyester resins:

Unsaturated polyester is produced by the chemical reaction between unsaturated acids or their
anhydrides such as PAN and polyhydric alcohol such as ethylene or propylene glycol. When these
polyester are dissolved in a monomer such as styrene, a resin is produced .The UPS are usually blended
with glass fibers to produce fiberglass-reinforced plastics. This composite material is used extensively
in the construction industry, marine transportation industries and automobile and patching compounds.
1.3.3 Alkyd Resins:

Phthalic anhydride is used to make PA-based alkyd resins. They are produced by reacting the
unsaturated polybasic anhydride or acid with large amount of polyhydric alcohols. Due to their
hardness and durability, alkyd resins made with PAN are mostly used in the different industries of
paints and coatings.
1.3.4 Pharmaceuticals:
When phthalic anhydride is reacted with cellulose acetate, the cellulose acetate phthalate is produced
(CAP) it is a polymer phthalate which is further used in the formation of pharmaceutical, like enteric
coatings of tablets or capsules and for controlled release formulations.[5]
1.3.5 Other uses:

Phthalic anhydride is also used in the production of dyes and pigments, detergents, herbicides and
insecticides, fire retardants, saccharin and polyester resin cross-linking agents.
1.4 Production and Consumption in Pakistan:

Phthalic Anhydride (PA) is the main product being manufactured by the Nimir chemicals for which it
is the only producer in the country. The initial capacity of PA plant was 12,000 TPA which was later
increased to 16,000 TPA in 2004. In order to fully satisfy the domestic requirement of PA which is
currently at over 28,000 TPA, the company further expanded its plant by 12,000 tons per annum. By
now the capacity of the plant is expanded to 28,000 TPA.[6]
Consumption of PA in Pakistan is around 50,000 TPA. Pakistan import 22,000 TPA of PA from India,
China to full fill the country demand
1.5 Production and Consumption in world:

In 2013, the worldwide production volume was estimated to be about 5 million tons per year.
Worldwide growth rates expected to be around 3.0-3.5%/year. This growth is led by the Asia-Pacific
region where demand is forecast to increase at 4.0-4.5%/year. Demand growth in the US and Western
Europe is much lower at 1.0-1.5%/year.
4
The largest markets for phthalic anhydride are plasticizers, unsaturated polyester resins, and alkyd
resins for surface coatings. Commercial phthalic anhydride is 99.8–99.9% pure (99.5% is generally
guaranteed) and is available in two forms—flake and molten. Most worldwide consumption of phthalic
anhydride is molten.
The largest market for phthalic anhydride is in the manufacture of phthalate plasticizers, which
accounted for about half of all phthalic anhydride consumed in 2016. The manufacture of alkyd resins
accounted for about 22% of consumption in 2016, followed by unsaturated polyester resins (UPR)
with more than 13% of the total. Asia (Northeast Asia, Southeast Asia, and the Indian Subcontinent)
is the largest consumer of phthalic anhydride, accounting for more than 60% of global consumption in
2016, led by China. The next-largest markets for phthalic anhydride outside of Asia are in Western
Europe and North America. [7]
The global PA market is highly fragmented in nature, and in 2013 the top 5 companies dominated less
than one-third share of the market. Some of the key corporations in the global PA market include UPC
Technology Corporation, Exxon Mobil Corporation, BASF SE, and Aekyung Petrochemical Co. Ltd
Estimated production volume world wide

Other countries
1%
Western Eyrope
24%
Asia
36%
USA
15%
Middle East
2%
Central America Japan
8% Eastern Europe 9%
5%
Western Eyrope USA Japan Eastern Europe Central America Middle East Asia Other countries
Figure 1.4: Production in World
1.6 Future Trends:

The production of Phthalic anhydride in Pakistan is just 28000 metric ton per year with a annual growth
rate of 4-4.5 %. Pakistan import 20000 metric ton per year to full fill the country demand. Almost all
the PAN in Pakistan is consumed in plastic industry. As plastic industry grows up day by day in
Pakistan there is need of more PA to full fill the requirement.
1.7 Market Assessment:

Phthalic anhydride is a main constituent of plastic. As country demand increases of plastic so this result
in the increase demand of PA. As phthalic anhydride is also require in resin and unsaturated polymers
5
its market increases in near future. High demand for PVC in construction and the automotive industry
is expected to fuel the demand for plasticizers and ensure the stable revenue source for the country
phthalic anhydride market over the forecast period. Demand of PA in Asia is increasing and its growth
rate is 4%.Most of the country in Asia import it from china. The raw material require in the production
of Phthalic anhydride is xylene. As xylene is cheap and easily available in Pakistan. As new aromatic
plant is set up in Pakistan the production of xylene increases the production of xylene become
increases. So Pakistan have best chance to producing the PA and export in nearby future
1.8 Handling:
 Avoid process temperatures above decomposition temperatures. Overheating may occur at
excessively high cylinder heats
 Avoid all personal contact, including inhalation.
 Wear protective clothing when risk of exposure occurs.
 Use in a well -ventilated area.
 Avoid contact with moisture.
 Avoid contact with incompatible materials.
 Avoid physical damage to containers
 Atmosphere should be regularly checked against established exposure standards to ensure safe
working conditions are maintained
1.9 Storage:
PAN should be stored in cool dry well-ventilated area out of direct sunlight and away from ignition
and heat. Protect from accidental contact with water. The product should be stored in containers
provided with fire resistant materials. Store away from strong oxidizers strong acid and bases ammonia
amines rubber. Keep containers tightly closed and labeled. Do not use aluminum or galvanized
containers. Reacts with mild steel, galvanized steel / zinc producing hydrogen gas which may form an
explosive mixture with air. Avoid storage with reducing agents.
1.10 Transportation:
The product can be sold in molten state as well as in flake (solids) If production is in the molten form
where the liquid phthalic anhydride is transferred by sealed heated pipeline to tanker container at 170
(oC). Phthalic anhydride is maintained in the liquid state (above the melting point) in the tanker
container during transport by either steam jacket or internal heating. The intrinsic heat hazard of the
liquid form and need to keep it as a liquid dictates that is retained within sealed pipelines and vessel at
all time
6
Chapter # 2 Manufacturing Process
Chapter # 2
Manufacturing process
2 Production method:
Phthalic anhydride produced by various types of method world widely. Phthalic anhydride are mainly
produced by oxidation of ortho- xylene and naphthalene. The process description of method of
production of phthalic anhydride are
2.1 Production from naphthalene:

Naphthalene base feed stock is made up of vaporized naphthalene and compressed air. It is transferred
to the fluidized bed reactor and oxidized in the presence of a catalyst vanadium pentaoxide at 350 oC.
Cooling tube in the catalyst bed remove the exothermic heat which is used to produce high pressure
steam. The reactor effluent consists of PAN vapors entrained catalyst and various by products and non-
reactant gases. The catalyst is removed by the filtering and then returned to the reactor .The reaction
is
9
C10H8 + O2 C8H4O3 + 2H2O + 2CO2
2
2.2 Production of O-xylene:

In PAN production o-xylene is used as a basic feedstock filtered air is preheated compressed and mixed
with vaporized o-xylene and fed in to fixed bed tabular reactor the reactor contain the catalyst
vanadium pentaoxide operated at 340oC to385oC Exothermic heat is removed by Dowtherm (A heat
transfer fluid) circulated around the reactor tube. The reaction that occur in the production in PAN
from o-xylene [2]
C8H10 + 3O2 C8H4O3 + 3H2O

2.3 Raw materials:
The raw material that are used in the production of phthalic anhydride are
 Air
 O-Xylene
 Naphthalene
2.3.1 O-xylene:
O-Xylene (ortho-xylene) is an aromatic hydrocarbon with the formula C6H4(CH3)2. With two methyl
substituents bonded to adjacent carbon atoms of a benzene ring (the ortho configuration). It is a
constitutional isomer of m-xylene and p-xylene, the mixture being called xylene or xylenes. O-Xylene
is a colorless slightly oily flammable liquid
Petroleum contains about one weight percent xylenes. Most o-xylene is produced by cracking
petroleum, which affords a distribution of aromatic compounds, including xylene isomers. M-Xylene
is isomerized to o-xylene. Net production was approximately 6x106 tons in the year 2010.
7
Xylenes are produced mainly as part of the BTX aromatics (benzene, toluene, and xylenes) extracted
from the product of catalytic reforming known as reformate. The xylene mixture is a slightly greasy,
colorless liquid commonly encountered as a solvent.
The melting point of o-xylene is −47.87 °C and the boiling point is around 140 °C The density is
around 0.87 g/mL and thus is less dense than water
A large amount of o-xylene that is 2.3x105 barrel per year is producing by byco petroleum Pakistan.
National Refinery Karachi also produce 2.5x105 barrel per year of BTX [8]
Xylene uses as a solvent in paints, varnishes, herbicide, pesticide, leather, printing and rubber
industries. Pakistan import 3.1x10^5 barrels of xylene in year 2011 from Taiwan, South Korea and
China to full the country demand
2.3.2 Naphthalene:
Naphthalene is an organic compound with formula C10H8. It is the simplest polycyclic aromatic
hydrocarbon, and is a white crystalline solid
Most naphthalene is derived from coal tar. From the 1960s until the 1990s, significant amounts of
naphthalene were also produced from heavy petroleum fractions during petroleum refining, but today
petroleum-derived naphthalene represents only a minor component of naphthalene production.
Naphthalene is the most abundant single component of coal tar. Although the composition of coal tar
varies with the coal from which it is produced, typical coal tar is about 10% naphthalene by weight. In
industrial practice, distillation of coal tar yields an oil containing about 50% naphthalene
In Pakistan a very small amount of naphthalene is produced by cracking of coal tar which is used in
production of sodium naphthalene and mothballs
2.4 Comparison of Naphthalene & O-xylene Process:

Naphthalene and O-xylene are produced by two different processes. The process uses naphthalene Is
called Badger-Sherwin-Williams and the process uses xylene is called BASF process. Both methods
has their own characteristic. Each account 50% of total production. Naphthalene base process only use
in those country uses catalytic cracking of coal tar. The comparison shown in table shows the best
process.
Table 2.1: Comparison between two processes
Naphthalene O-Xylene
1 Less yield of phthalic anhydride is produced High overall yield of Phthalic Anhydride
in this process product
2 Naphthalene require more drastic condition High concentration of o-xylene in the feed gas
to make a mixture with air results lower investment and operation costs.
3 This process uses fluidized bed reactor which Application of fixed bed reactor shows near-
emit more gases than BASF Process complete removal of undesired by-products
and minimization of burning of Phthalic
Anhydride.
8
4 Fluidized bed reactor is difficult to maintain. Fixed bed reactor(s) results in flexible
And in reactor effluent small amount of operation.
catalyst is come out which cost an separator
after the reactor
5 Naphthalene price is higher than o-xylene. It is cheaper than naphthalene and provides a
Its price is 1100 $/ton more efficient process. Its price is 950$/ton
6 In naphthalene 2 carbon atom is converted In this process less emission of carbon dioxide
into carbon dioxide occur
2.5 Selection of BASF process:

We select BASF process as it yield more PAN than BSW process and that the main reason is that total
loses is of PAN and MAN are less. Hence the recovery of PAN and MAN is economically more
attractive .Recovery of both material solves the most troublesome emission. BASF process is selected
due to availability of raw material in Pakistan. The BASF process accounts world total of 50% and
trend is shifting to BASF process. Naphthalene base process only uses in counties which carry out
thermal cracking of coal tar
2.6 Capacity Selection:

The consumption of PA in Pakistan is around 50,000 TPA. While Pakistan total production of PA is
28000 Metric ton per year with a growth rate of 4-4.5%. Pakistan imports 22000 TPA per year to full
fill the requirement. PA is used as a plasticizer almost all the PA in Pakistan is consumed in very fast
growing plastic industry. For production raw material are cheap and easily available and for the current
growing rate the consumption of PA in Pakistan is 2023 is around 60000 TPA.
As Nimir chemical is only plant in Pakistan since 2001 that produces PA. Assuming that in near future
no new PA plant will install in Pakistan We select our plant capacity is 40,000 TPA to fulfill the
country demand as Pakistan don’t need to import it anymore as Pakistan chemical industry growing
rapidly in near future beside plastic PA can also be used in alkyd resin, unsatured polymers so there in
increase demand of PA in Pakistan in nearby future
2.7 Process description of selected process:

When Air is react with vaporized xylene in reactor following reaction occur
C8H10 + 3O2 C8H4O3 + 3H2O (Main reaction)
O-xylene Phthalic anhydride
C8H10 + 15/2O2 C4H2O3 + 4H20 + 4CO2 (side reaction)
O- xylene Maleic anhydride

21
C8H10 + O2 8CO2 + 5H20
2
Air is compressed to approximately 250 kPa in a single-stage centrifugal compressor (C-101) and
heated to 360°C using high-pressure steam in heat exchanger E-201. This hot compressed air is then
9
mixed with o-xylene feed that has been pumped to approximately 250 kPa using P-301A/B and
subsequently heated and vaporized in E-202 using high-pressure steam. The combined o-xylene and
air stream enters the fixed-bed catalytic reactor, R-401, at 360 °C and 240 kPa. For safety reasons, the
concentration of o-xylene is kept at or below the lower explosive limit of 1 mol%. The ratio of o-
xylene to air is set using a ratio controller between the compressor and the control valve on the pump.
In the reactor, the o-xylene is subject to a variety of oxidation reactions to produce the desired product
of PA, byproduct maleic anhydride (MA), products of combustion, and a small amount of benzoic
acid. All these reactions are highly exothermic, and the temperature of the reactor is controlled by
heat exchange with a stream of cooling medium (Dowtherm) that flows cocurrently through the shell-
side of the reactor. The Dowtherm A is circulated through the reactor in a closed loop by pumps P-
302A/B. Heat is removed from the Dowtherm in heat exchanger (E 205) by cooling water.
The reactor effluent leaves the reactor at 360(°C) and 160 kPa. The pressure drop across the reactor
is caused by the flow of the reactant gases through the catalyst-filled tubes. This stream is cooled in
heat exchanger (E-203), (E-204) in which the temperature of the process stream is reduced to 145(°C)
.The cooled reactor effluent is a two-phase mixture at this point, and it is then sent to a Flash drum (F-
501) to recover the PA. Gases removed which are mainly air, unreacted oxygen, product of combustion
are removed from the top of the flash drum while phthalic anhydride and maleic anhydride removed
from the bottom of the flash drum The raw PA is further purified by sending the liquid stream from
the flash drum through a pressure-reducing valve and the stream enters PA tower (T-601) at 145(oC)
.In the PAN tower, 99.9 mol% PA is produced as a bottom product and MA of purity >95 mol% is
produced overhead. The MA by-product is eventually sold.
Table 2.2: Fractional Conversion of O-Xylene
T(°C) Maleic anhydride CO2 Phthalic anhydride
300 1.00 0.00 0.00
320 0.536 0.0339 0.425
340 0.215 0.102 0.683
360 0.100 0.200 0.700
380 0.0463 0.356 0.598
400 0.0215 0.602 0.377
420 0.00 1.00 0.00
2.8 Selection of Catalyst:

It is a combination of Vanadium Pentaoxide (V2O5) and very small amount Titanium dioxide (Ti2O5).It
is prepared by heating a suspension containing compounds and spray coating the suspension onto a
support which can be either 6mm porcelain spheres. Surface Area available for reaction is about 10-
12 m2/g.
10
2.9 Choice of a reactor:

Reactor R-401 is a packed bed reactor similar to a shell and tube heat. Reaction is highly exothermic
the maximum conversion of PAN Is occur at 360(oC) to maintain the temperature a Dowtherm A is
circulate around the tubes in a shell side of a reactor
11
E-206 E-207
C-101 P-301 E-201 E-202 R-401 P-302 E-203 E-205 E-204 D-601 Maleic V-101 Phthalic
Feed Air O-xylene Air O-xylene Packed bed Dowtherm A Product Gas Dowtherm A Product Gas F-501 Distillation Anhydride Melic Anhydride Anhydride
Compressor Feed pump Heater Vaporizer Reactor Pump Cooler Cooler Cooler Flash Drum Column condenser Reflux Drum Reboiler
Air to treatment
11
Air
1 CW CW
E-206
F-501
8 9 10 CW
Flash Drum
C-101
E-203 E-204
E-201 R-401 cw
Maleic
2 V-101 Anhydride
7
13
Steam
E-205
D-601
6
12
E-202
P-302
4 5
3
O-xylene Steam
P-301
Phthalic
E-207 Anhydride
14
Process Flow Diagram of Phthalic Anhydride via O-Xylene Oxidation
12
Table 2.3: Stream Table
Stream No 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Temperature 25 360 25 360 360 115 45 360 250 145 145 145 165 180
(oC)
Pressure 1 2.38 1 2.32 2.37 1.8 2.6 1.57 1.40 1.25 1 1 0.06 0.06
(atm)
Flow rate 42418.4 42418.4 5331.8 5331.8 47750.24 803.76 803.76 47750.24 47750.24 47750.24 42327.12 5424 366.7 5057
(kg/hr)
13
Chapter # 3 Material Balance
Chapter # 3
Material Balance
3 Material Balance:
A mass balance, also called a material balance, is an application of conservation of mass to the analysis
of physical systems. By accounting for material entering and leaving a system, mass flows can be
identified which might have been unknown, or difficult to measure without this technique. The exact
conservation law used in the analysis of the system depends on the context of the problem, but all
revolve around mass conservation, i.e. that matter cannot disappear or be created spontaneously.
The general form quoted for a mass balance is the mass that enters a system must, by conservation of
mass, either leave the system or accumulate within the system.
Input – Output + Generation – Consumption = Accumulation

Plant Capacity:
The production capacity of plant is = 40000Tons/Year
Operating Time:
Operating time of plant is 330 days/year
Production Rate:
Production rate of plant is = 40000tons/year
40000 Ton 1000 Kg 1 Year 1 Days
Year 1 Ton 330 Days 24 Hr
The production rate of Phthalic Anhydride for the working days of 330 is 5050.50 kg/hr or
34.12kmol/hr.
Basis;
100kmol/hr of xylene
Air :O-xylene Ratio = 8:1 [9]
8*106*100 = 84800/29
=2924.1 kmol/hr
Oxygen = 2924.1*0.21
=614.06 kmol/hr
14
Inert = 2924.1 – 614.06

=2310.04 kmol/hr
3.1 Material Balance Around Mixing Point:

Inert = 2310 kmol/hr
Oxygen = 614.04 kmol/hr

O-Xylene = 100kmol/hr
O-Xylene = 100kmol/hr 4 5
Figure 3.1: Mixing Point
Table 3.1: Inlet and Outlet Stream of Mixing Point
Components Inlet Streams Outlet Streams

2 4 5
(kmol/hr) (kmol/hr) (kmol/hr)
Inert 2310.04 _ 2310.04
O2 614.06 _ 614.06
O-Xylene _ 100 100
Total 3024.1 3024.1
3.2 Material Balance Around Reactor (R-401):

The combined O-xylene and air streams enters the fixed-bed catalytic reactor and form the phthalic
anhydride, maleic anhydride and products of combustion
15

Phthalic Anhydride = 70kmol/hr
Maleic Anhydride = 10 kmol/hr
Water = 350 kmol/hr
8 Carbondioxide =200kmol/hr
cw
7
R-401
E-205
Inert = 2310 kmol/hr P-302

5
Figure 3.2: Reactor (R-401)
Table 3.2: Inlet and Outlet Stream Of Reactor
Components Inlet Streams Outlet Streams
5 8
(Kmol/hr) (Kg/hr) (Kmol/hr) (Kg/hr)
O2 614.06 19649.92 119.06 3809.92
Inert 2310.04 64681.12 2310.04 64681.12
O-Xylene 100- 10600 _ _
Phthalic Anhydride _ _ 70 10360
Maleic Anhydride _ _ 10 980
Carbon dioxide _ _ 200 8800
Water _ _ 350 6300
Total 3024.1 94931.04 3059.1 94931.04
16
Reactions
Main Reaction:
C8H10 + 3O2 C8H4O3 + 3H20

O-Xylene Phthalic Anhydride
Side Reactions:
C8H10 + 7.5O2 C8H2O3 + 4H20 + 4CO2

O-Xylene Maleic Anhydride
C8H10 + 10.5O2 5H20 + 8CO2

By Extent of reaction:
As conversion of first reaction = 70%
Conversion of second reaction = 10%
Conversion of third reaction is = 20% [10]
Moles out=moles in ± (stoichiometric coefficient) [11]
no = nin ± v𝛆
𝒏xylene = 100 - ε1- ε2- ε3
ήo2 = 614.06 - 3ε1 - 7.5ε2 - 10.5ε3
ήc8H O = 𝛆1
4 3
ήH O = 3ε1 + 4ε2 + 5ε3

2
ήc4H O = ε2
2 3
ήCO2 = 4ε2 + 8ε3

Phthalic Anhydride=(0.70*100*1mol c8H4O3/1 mole c8H10 )
=70mol c8H4O3/hr
𝛆1 =70mol/hr
Maleic anhydride =(0.10*100*1mol c4H2O3/1 mole c8H10)
𝛆2 =10mol c4H2O3/hr
17
As conversion of o-xylene is 100%, so no unreacted xylene left
0=100-70-10- ε3
𝛆3 = 20mol/hr
ήCO2=(4*10)+(8*20)
ήCO2=200mol/hr
ήH2o=(3*70)+(4*10)+(5*20)
ήH2o=350mol/hr
Oxygen Reaming:
ήo2 = 614.06 - 3(70) - 7.5(10) - 10.5(20)
ήo2 = 614.06 - 495

ήo2 = 119.06 kmol/hr
3.3 Material Balance around Flash Drum (F-501):
Phthalic Anhydride = 2.01 kmol/hr

Maleic Anhydride = 2.67 kmol/hr
Water = 350 kmol/hr
11
Carbondioxide = 200kmol/hr
Oxygen = 119.06kmol/hr
Inert = 2310.04 kmol/hr

Water = 350 kmol/hr 10
Carbondioxide = 200kmol/hr
Oxygen = 119.06kmol/hr
Inert = 2310.04 kmol/hr
Phthalic Anhydride = 67.99 kmol/hr

12 Maleic Anhydride = 7.33 kmol/hr
Figure3.3: Flash Separator (F-501)
18
The cooled reactor effluent is a two-phase mixture at this point, and it is then sent to a Flash drum (F-
501) to recover the PA. Gases removed which are mainly air, unreacted oxygen, product of combustion
are removed from the top of the flash drum while phthalic anhydride and maleic anhydride removed
from the bottom of the flash drum
Table 3.3: Inlet and Outlet Stream of Flash Separator
Components Inlet streams Outlet Streams
10 11 12
(kmol/hr) (kg/hr) (kmol/hr) (kg/hr) (kmol/hr) (kg/hr)
Phthalic 70 10360 2.01 297.48 67.99 10062.52

Anhydride
Maleic Anhydride 10 980 2.67 261.66 7.33 718.34
Carbon dioxide 200 8800 200 8800 - -
Water 350 6300 350 6300 - -
Nitrogen 2310.04 64681.12 2310.04 64681.12 - -
Oxygen 119.06 3809.92 119.06 3809.92 - -
Total 3059.1 94931.04 2983.76 84150.18 75.32 10780.86
Table 3.4: Antoine Coefficient
Components A B C
Phthalic Anhydride 15.9984 4467.01 -83.15
Maleic Anhydride 16.2747 3765.65 -82.15
Water 18.306 3616.44 -46.13
Carbon dioxide 22.5898 3103.39 -0.16
Oxygen 15.4075 734.55 -6.46
Nitrogen 14.952 588.72 -6.5
Temperature = 145oC
Pressure = 1atm =760mmHg
19
Antoine equation is used to find the vapor pressure of each component:

𝑩
𝑳𝒏 (𝒑°) = 𝑨 −
𝑪+𝑻
𝑳
+𝟏
𝑿𝒊 = 𝑽 x 𝑿𝒇𝒊
𝑳
+ 𝟏
𝑽
𝑳
+𝟏
𝒚𝒊 = 𝒌𝒊𝑿𝒊 = 𝑽 x 𝒌𝒊 x 𝑿𝒇
𝑳
𝑽 + 𝒌𝒊
Table 3.5: Flash Calculations
Component Xf Po K Yi
Phthalic Anhydride 0.022 30.26 0.0398 6.73*10-4
Maleic Anhydride 3.26*10-3 157.96 0.2078 8.94*10-4
Water 0.114 3104.99 4.0855 0.117
Carbon dioxide 0.065 3846134.03 5060.70 0.067
Oxygen 0.038 824607.00 982.26 0.0399
Nitrogen 0.755 746524.68 1085.009 0.774
Overall Mass Balance:

F=V + L
L/V = 0.025
F = 3059.1kmol/hr
L = 75.32 kmol/hr
V = 2983.78 kmol/hr
Phthalic Anhydride Balance:

F=V + L
Fxf = Vyv + Lxl

3059.1*0.022 = 2983.78 *6.73*10-4+ 75.32 *Xl
Xl = 0.905
Maleic Anhydride Balance:

F=V + L
20
Fxf = Vyv + Lxl

3059.1*3.26*10-3 = 2983.78 *8.94*10-4+ 75.32 *Xl
Xl = 0.095
Water Balance:
F=V + L
Fxf = Vyv + Lxl

3059.1*0.114 = 2983.78 *0.117 + 75.32 *Xl
Xl = 0.00
Carbon dioxide Balance:

F=V + L
Fxf = Vyv + Lxl

3059.1*0.065 = 2983.78 *0.067 + 75.32 *Xl
Xl = 0.00
Oxygen Balance:
F=V + L
Fxf = Vyv + Lxl

3059.1*0.038 = 2983.78 *0.0399 + 75.32 *Xl
Xl = 0.00
Nitrogen Balance:
F=V + L
Fxf = Vyv + Lxl

3059.1*0.755 = 2983.78 *0.774 +75.32 *Xl
Xl = 0.00
21
3.4 Material Balance Around Distillation Tower (D-601):
E-206
CW
D-601
V-101
13
Phthalic Anhydride=0.28kmol/hr
Phthalic Anhydride=67.9kmol/hr Maleic Anhydride=7.03kmol/hr
Maleic Anhydride=7.33kmol/hr
12
E-207
14
Phthalic Anhydride=67.7kmol/hr
Maleic Anhydride=0.29kmol/hr
Figure 3.4: Distillation Column (D-601)
In flash calculations we use Rachford-Rice flash equation to find out the desired calculations. First we
calculate the flash calculation for the vapor and liquid flow rate and composition in the top and bottom
flow [12][13]
Temperature = 145oC
Table 3.6: Antoine Coefficient [14]
Components A B C
Phthalic Anhydride 15.9984 4467.01 -83.15
Maleic Anhydride 16.2747 3765.65 -82.15
Antoine equation is used to find the vapor pressure of each component:

𝑩
𝑳𝒏 (𝒑°) = 𝑨 −
𝑪+𝑻
22
𝑳
+𝟏
𝑿𝒊 = 𝑽 x 𝑿𝒇𝒊
𝑳
𝑽+𝟏
𝑳
+𝟏
𝒚𝒊 = 𝒌𝒊𝑿𝒊 = 𝑽 x 𝒌𝒊 x 𝑿𝒇
𝑳
+ 𝒌𝒊
𝑽
Table 3.7: Flash Calculations
Xf PO K X y
Phthalic Anhydride 0.92 33.214 0.7283 0.99 0.039
Maleic Anhydride 0.08 172.416 3.7810 0.001 0.961
Overall Mass Balance:

F= D + W
L/V= 9.27
Feed = 75.32 kmol/hr
V = 7.33 kmol/hr
L = 67.99 kmol/hr
Phthalic Anhydride Balance:

F=V + L
Fxf = Vyv + Lxl

75.32*0.905 =0.239*7.33 + 67.99*XL
Xl = 0.999
Maleic Anhydride Balance:

F=V + L
Fxf = Vyv + Lxl

75.32*0.095 = 0.961*7.33 + 67.99* XL
Xl = 0.0001
23
Table 3.8: Inlet and Outlet Stream of Distillation Column
Component Inlet Stream Outlet Stream

12 13 14
Kmol/hr Kg/hr Kmol/hr Kg/hr Kmol/hr Kg/hr
Phthalic Anhydride 67.99 10062.52 0.28 32.47 67.71 10030.8
Maleic Anhydride 7.33 718.34 7.033 699.60 0.29 18.42
Total 75.32 10780.86 7.313 731.07 67.99 10049.4
Scale up ratio:
5050.5/10030.8 =0.503
24
Table 3.9: Molar Flow rate
Component 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Inert 1161.95 1161.95 - - 1161.95 - - 1161.95 1161.95 1161.95 1161.95 - - -
O-xylene - - 50.3 50.3 50.3 - - - - - - - - -
Oxygen 308.87 308.87 - - 308.87 - - 59.88 59.88 59.88 59.88 - - -
Water - - - - - - - 176.05 176.05 176.05 176.05 - - -
Carbondioxide - - - - - - - 100.6 100.6 100.6 100.6 - - -
Phthalic - - - - - - - 35.21 35.21 35.21 1.011 34.19 0.14 34.05
Anhydride
Maleic - - - - - - - 5.03 5.03 5.03 1.34 3.68 3.53 0.15
Anhydride
Dowtherm A - - - - - 2.47 2.47 - - - - - - -
Sum 1470.82 1470.82 50.3 50.3 1521.12 803 803 1538.72 1538.72 1538.72 1500.83 37.87 3.67 34.19
(100kmol/hr O-xylene basis)
25
Table 3.10: Mass Flow rate
Component 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Inert 32534.6 32534.6 - - 32534.6 - - 32534.6 32534.6 32534.6 32534.6 - - -
O-xylene - - 5331.8 5331.8 5331.8 - - - - - - - - -
Oxygen 9883.84 9883.84 - - 9883.84 - - 1916.16 1916.16 1916.16 1916.16 - - -
Water - - - - - - - 3168.9 3168.9 3168.9 3168.9 - - -
Carbondioxide - - - - - - - 4426.4 4426.4 4426.4 4426.4 - - -
Phthalic - - - - - - - 5215.30 5215.30 5215.30 149.74 5064.2 20.7 5043
Anhydride
Maleic - - - - - - - 492.94 492.94 492.94 131.32 361.6 347 13.7
Anhydride
Dowtherm A - - - - - 803 803 - - - - - - -
Sum 42418.4 42418.4 5331.8 5331.8 47750.2 803 803 47750.2 47750.2 47750.2 42327.1 5424.8 367 5056
26
Chapter # 4 Energy Balance
Chapter # 4
Energy Balance
4 Energy Balance:
Energy balance is the calculations of the energy requirements for the process, like the heating, cooling,
pressure, and enthalpy. Energy is categorized in several forms like kinetic energy, potential energy,
heat energy, electrical energy, mechanical energy. According to law of conservation of energy, energy
can neither be created nor be destroyed. A general equation of conservation of energy is: [14]
Accumulation = Energy in + Generation – Energy out – Consumption
4.1 Energy Balance around Air heater (E-201):
Saturated Steam
Pressure = 86 bar
Temperature = 365oC
Temperature = 30 oC Temperature = 360 oC
Inert = 32434.6 kg/hr Inert = 32434.6 kg/hr

1 2
Oxygen = 9883.84kg/hr Oxygen = 9883.84kg/hr
Saturated Steam
Pressure = 86 bar
Temperature = 365oC
Figure 4.1: Air Preheater (E-201)
Inlet Temperature = T1 = 30oC = 303K

Outlet Temperature = T2 = 360oC = 633K
Reference Temperature = Tref = 25oC = 298K
Heat Capacity of Air at 303K = 1.006 kJ/kgK

Heat Capacity of Air at 633K = 1.006 kJ/kgK
Mass flow rate = 42418.4 kg/hr
Q in = m*Cpavg*(T1 - TREF)
Qin = 42418.4 *1.006(303-298)
27
Qin = 213152.46 kJ/hr

Qout = m*Cpavg*(T2 – T1)
Qout =42418.4 *1.006(330)
Qout = 14081927.64 kJ/hr
ΔQ = Qout – Qin
ΔQ = 13868565.14 kJ/hr
Now the mass flow rate of saturated steam
Latent heat of vaporization of saturated steam at 365oC = 702.18 kJ/kg
m = Q/ λ
m = 19755 kg/hr
4.2 Energy Balance O-Xylene Vaporizer (E-202):

Saturated Steam
Pressure = 86 bar
Temperature = 365oC
Temperature = 30oC Temperature = 360 oC
O-Xylene = 5331.8 kg/hr O-Xylene = 5331.8 kg/hr

3 4
Saturated Steam
Pressure = 86 bar
Temperature = 365oC
Figure 4.2: O-Xylene Vaporizer (E-202)
Inlet Temperature = T1 = 30oC =303K
Vaporization Temperature = Tvap = 144oC = 417K
Reference Temperature = TREF = 25oC =298K
28
Table 4.1: Heat Capacity [15]
Temperature (K) Heat Capacity Kj/kgK

298 1.86
303 1.87
417 2.22
633 3.92

Qin = m*Cpavg*(T1 - TREF)
Qin = 5331.8*1.86*5
Qin = 49585.74 kJ/hr
Q1 = m*Cpavg*(Tvap – T1)
Q1 =5331.8*2.04*(114)
Q1 = 1239963.4 Kj/hr
Q2 = m*Cpavg*(Tout– Tvap)
Q2 =5331.8*3.07*(216)
Q2 = 3535623.2 kJ/hr
Latent heat of vaporization of O-Xylene = 347 Kj/kg
m λ = 347*5331.8
m λ = 1850134.6
ΔQ = Q2 + Q1 + m λ – Qin
ΔQ = 6576135.46 kJ/hr
Now the mass flow rate of saturated steam
Latent heat of vaporization of saturated steam at 365oC = 702.18 kJ/kg
m = Q/ λ
m = 9367 kg/hr
29
4.3 Energy Balance around Reactor (R-401):

Water = 350 kmol/hr
8 Carbondioxide =200kmol/hr
cw
7
R-401
E-205
Inert = 2310 kmol/hr P-302

5
Figure 4.3: Reactor (R-401)
Inlet Temperature = 30oC= 303K

Table 4.2: Heat Capacity [15]
Component 25oC 30oC 360oC

O-xylene 1.86 1.87 3.92
Air 1.006 1.006 1.059
Phthalic Anhydride 0.89 0.89 1.42
Maleic Anhydride 1.71 1.71 2.23
Carbon Dioxide 0.871 0.871 1.10
Cp = Cpavg*xxylene + Cpavg*xair
Cp = (2.89* 0.111) + (1.006* 0.88)
Cp = 1.21 kJ/kgK
Qin = m*Cp*(T1 – Tref)
Qin = 47750.24 *1.21 *(335)
Qin = 19355559.78 kJ/hr
30
Outlet Temperature = 360oC= 633K

Cp = Cp*xair + Cp*xPa + Cp*xMa + Cp*xwater + Cp*Carbondioxide

Cp = (1.006* 0.721) + (1.15* 0.109) + (1.97* 0.01) + (4.49* 0.066) + (0.98* 0.092)
Cp = 1.25 kJ/kgK
Qout = m*Cp*(T2 – TREF)
Qout = 47750.24 *1.25*(335)
Qout = 19995413 kJ/kg
Heat of formation:
Table 4.3: Heat of Formation [16]
Component Heat of formation kJ/mol

O-Xylene (g) 19.00
O-Xylene ( l) -24.44
Water (g) -285.5

Phthalic Anhydride (g) -297.65
Maleic Anhydride (g) -538.29
Maleic Anhydride (l) -787
Carbon dioxide (g) -393.51
Heat of Reaction:
Heat of 1st Reaction at at Reference Temperature =25oC= 298K = -1171 kJ/mol
ΔHr of 2nd reaction at Reference Temperature = -3273.33 kJ/mol
ΔHr of 3rd reaction at Reference Temperature = 298K= -4594.2 kJ/mol
ΔHrx (T) = ΔHorx (Tr) + ΔCp (T-Tr)
Overall Heat of Reaction = - 162263.443 kJ/hr
Mass flowrate of Dowtherm A:

Inlet Temperature = 45oC = 318K
Outlet Temperature = 115oC = 388K
ΔT = 70 K
Heat Capacity of Dowtherm A at 318K = 2.808 kJ/KgK
31

m = 803.76 kg/hr
4.4 Energy Balance around Dowtherm A Cooler (E-205):

Cooling Water
Temperature = 40oC
Temperature = 115oC Temperature = 45oC
Dowtherm A = 803.76 kg/hr Dowtherm A = 803.76 kg/hr

6 7
Cooling Water
Temperature = 25oC
Figure 4.4: Dowtherm A Cooler (E-205)

Heat Capacity of Dowtherm A at 298K= 2.72 kJ/KgK [17]
Qin= m*Cpavg*(T1 – TREF)
Qin = 803.76 *2.88*90
Qin =208334.592 kJ/hr
Qloss = m*Cpavg*(T2 – T1)
Qloss = 803.76*2.76*(-70)
Qloss = -155286.43 kJ/hr
Qout = 53048.6 kJ/hr
32
Calculating Mass flow rate of cooling water:

ΔT = 15K
Heat Capacity of Cooling Water = 4.18 kJ/KgK
m = Q/Cp* ΔT
m = 2615.10 kg/hr
4.5 Energy Balance on Product Gas Cooler (E-203):

Cooling Water
Temperature = 49oC
Temperature = 250oC
Temperature = 360oC
Mass flowrate = 4770.24 kg/hr
Mass flowrate = 4770.24 kg/hr 8 9
Cooling Water
Temperature = 25oC
Figure 4.5: Product Gas Cooler (E-203)

Condensation Temperature = Tcond = 285oC = 558K

Cp = (1.006* 0.721) + (1.15* 0.109) + (1.97* 0.01) + (4.49* 0.066) + (0.98* 0.092)
Cp = 1.25 kJ/kgK
Qin = 19995413 kJ/kg
Q1 = m*Cp*(Tcond – Tin)
Cp = (1.006* 0.721) + (1.09* 0.109) + (1.91* 0.01) + (4.46* 0.066) + (0.96* 0.092)
33
Cp = 1.22 kJ/kgK
Q1 = 47750.24 *1.22*(-75)
Q1 = -4404959.64
Outlet Temperature =T2 = 250oC = 523K
Heat Capacity of Air at 250oC = 1.006 kJ/kgK
Heat Capacity of Phthalic Anhydride at 250oC = 1.21 kJ/kgK
Heat Capacity of Maleic Anhydride at 250oC = 2.119 kJ/kgK
Heat Capacity of Carbon dioxide at 250oC = 1.01 kJ/kgK
Cp = (1.006* 0.721) + (1.07* 0.109) + (1.88* 0.01) + (4.42* 0.066) + (0.94* 0.092)
Cp = 1.21 kJ/kgK
Q2 = m*Cp*(Tout – Tcond)
Q2= m*Cp*ΔT
Q2 = 47750.24 *1.21*(-35)
Q2 = -2022222.66 kJ/hr
Latent heat of condensation of phthalic anhydride = -440KJ/kg

Q = m λ = -2294820 kg/hr
Qout = 1127330.76 kJ/hr
Calculating mass flow rate of Cooling water:

Inlet Temperature = 25oC
Outlet Temperature = 49oC
Q = 8721782.24 Kg/hr
m = Q/(Cp* ΔT)
m =86939 kg/hr
34
4.6 Energy Balance on Product Gas Cooler (E-204):

Cooling Water
Temperature = 49oC
Temperature = 145oC
Temperature = 250oC
Mass flowrate = 4770.24 kg/hr
Mass flowrate = 4770.24 kg/hr 9 10
Cooling Water
Temperature = 25oC
Figure 4.6: Product Gas Cooler (E-204)
Qin = 1127330.76 kJ/hr

Condensation Temperature = Tcond = 202oC = 475K
Heat Capacity of Water at 202oC = 4.42 kJ/kgK
Cp = (1.006* 0.721) + (1.04* 0.109) + (1.84* 0.01) + (4.39* 0.066) + (0.93* 0.092)
Cp = 1.19 kJ/kgK
Q1 = m*Cp*(Tcond – T1)
Q1 = 47750.24*1.19*(-48)
Q1 = -2727480 kJ/hr
Latent heat of condensation of maleic anhydride = -446.6 kJ/kg

For maleic anhydride = Q = m λ = -220142.07 kg/hr
35

Heat Capacity of Water at 145oC = 4.28 kJ/kgK
Cp = (1.006* 0.721) + (1* 0.109) + (1.78* 0.01) + (4.3* 0.066) + (0.91* 0.092)
Cp = 1.17 kJ/kgK
Q2 = m*Cp*(T2 – Tcond)
Q2 = 47750.24*1.17*(-57)
Q2 = -3184447.5 kJ/hr
Qout = 5141560.5 kJ/hr
Calculating mass flow rate of cooling water:

Inlet Temperature = 25oC
Outlet Temperature = 49oC
Q = 6147299.136 kJ/hr
m = Q/(Cp* ΔT)
m = 61125 kg/hr
4.7 Energy Balance Around Distillation Column (D-601):

Liquid = 5056 kg/hr
Latent heat of vaporization of Maleic anhydride = 446.6 kJ/kg
Latent heat of condensation of Phthalic anhydride = 440 kJ/kg
Feed Temperature = 145oC
Temperature of Top Product = 159oC
Latent Heat = (0.039*440) + (446.6*0.961)
Latent Heat = 445.7 kJ/kg
Q = V*(latent heat + Cp ΔT)
Q = 366.7 * (445.7 + 1.13*14)
Q = 169239.38 kJ/hr
Calculating mass flow rate of cooling water
36

ΔT = 20K
Heat Capacity of Cooling Water = 4.18 kJ/KgK
m = Q/Cp* ΔT
m = 2024.87 kg/hr
Temperature of Bottom Product = 177oC
Q= L *(Cp* ΔT)
Q = 5056*(1.05*31)
Q= 1645728.76
Calculating Mass flow rate of saturated steam
Latent heat of vaporization of saturated steam at 177oC= 2052.7 kJ/kg
M= 802 kg/hr
37
Chapter # 5 Equipment Design
Chapter # 5
Equipment Design
5 Air Preheater design (E-201):
A heat exchanger is a device used to transfer heat between two or more fluids. The fluids can be single
or two phase and, depending on the exchanger type, may be separated or in direct contact.
Δt:
Hot Fluid Cold Fluid Difference

365oC Hot Temperature 360 oC 5 oC Δt2
365oC Cold 30 oC 335 oC Δt1
Temperature
0 Difference 330 oC -330 oC Δt2 – Δt1
Calculation of LMTD:
LMTD = [∆t2 - ∆t1]/ln (∆t2/∆t1)
LMTD = 78.48 0C
Heat Duty:
Q = 3911646.56 W
Heat Transfer Area:

Q = UD ∆T
A = Q / UD∆T
Where,
UD = Heat transfer coefficient Assumed
Assume
UD=250 W/m2.0K (From figure D.3 Appendix D)
Heat transfer area, A = 44.51 m2 = 480ft2
a” = 0.1963 ft2/lin ft (From figure D.2 Appendix D)
Number of tubes = 480/ 0.1963*16
n = 154
1
Assume two passes nearest count 166 tubes in 17 4 in ID shell
Corrected Area:
A = NT x L x a
38
= 521 ft2 = 48.5 m2
Corrected Co-efficient UD:

UD = Q / (A×∆TLMTD)
UD = 236.21 W/m2 0K = 42 BTU /(hr)(ft2)(oF)
Cold Fluid: Shell side, Air Hot Fluid: Tube side , Steam
Flow area:
Flow area:
B = ID/5
at = 0.302 in (Table 10)
= 17.25/5
at= Nt*A t/144n
= 3.5 In 166∗0.302
=
as = ID*C*B/144Pt 144∗2
= 0.104 ft2 =0.174ft2
Mass velocity: Mass velocity:
G = W/as Gt =W/at
= 93516/0.014 = 43552/0.174
= 610730 lb/(ft2).(hr) = 250298 lb/(ft2).(hr)
At Tavg = 383oF De = 0.62/2 (Table `10)
µ = 0.035*2.42 = 0.0517 ft
= 0.0847 lb/(ft).(hr) At 689oF
De = 0.95/2 (Fig 28) µ = 0.034 *2.42
= 0.079 ft = 0.08228 lb/(ft).(hr)
Re = DeG/µ Re =Di*Gt / μ
0.079∗610730 0.0517 ∗ 250298

Re = 0.08228
0.0847
Re = 569630.10 Re = 157272
JH = 480
C = 0.24 BTU/lboF Condensation of Steam
k = 0.0270 BTU/(hr)(ft2)(oF/ft) hio = 1500Btu/(hr).(ft 2 ).(0F)
1
𝐶 ∗ µ (3)
( )
𝑘
= 0.979
39
Shell Side Coefficient

h0 = JH.k/De (Cp μ/k)⅓.Φ
0.0270
ho = 480 ∗ ( ) ∗ 0.979
0.079
= 160 BTU/(hr).(ft 2 ).(0F)
Clean Overall Coefficient: Uc

= ho* hio /(ho + hio)
= 1500*160/1500+160
= 144 BTU/(hr)(ft2)(oF) = 817 W/m2K
Dirt Factor:
Rd = (UC – UD)/ UC.UD
= 0.003 (hr)(ft2)(oF)/Btu
Pressure Drop:
Shell Side Tube Side

No. of crosses
Specific volume of steam
N+1 = 12 L/B = 55
V= 0.115 ft2/lb
Da = 17.25/12
S = (1/0.115)/62.5
= 1.53ft
S = 0.144
S= 1
f = 0.000155 ft2/in2
∆Ps = f G 2 (N+1)Da /5.22x10 DeΦs
∆Pt = ½ * f G2 xLn/5.22x10 DΦt
f = 0.000091 ft2/in2
= 1.67/2
∆Ps = 1.64 psi
0.83 psi
40
SPECIFICATION SHEET
Identification
Item Shell and tube heat exchanger E-101
Type 1-2 horizontal heat exchanger
Function
To Increase the temperature of Air
No. Required: 1 Operation: Continuous
Heat duty: 13347090 BTU/hr Area: 521ft2
Shell side Tube side

Fluid handled: Cold Air Fluid handled: Steam
Flow rate: 93516 lb/h Flow rate: 261024.7 lb/h
t1=30oC t2= 360 oC T1=: 365 oC T2= 365 oC
Tubes: 3/4 in OD, 16 BWG
Shell: 17.25 in dia. Number of tubes: 166
Passes: 1 Passes: 2
Baffles spacing: 3.5 in Pitch: 1 in square
Reynold number: 569630.10 Reynold number:157272
JH:489 Heat transfer coefficient:1500 Btu/hr ft2 oF
Heat transfer coefficient:144 Btu/hr ft2 oF Pressure drop: 0.83 psi
Pressure drop:1.64 psi
Btu Btu
UD assumed: 45 UD calculated: 42
(ℎ𝑟 𝑓𝑡 2 )̊(F) ( ℎ𝑟 𝑓𝑡 2 )̊(F)
41
5.1 Vaporizer Design:

Vaporizers are heat exchangers which are specially designed to supply latent heat of vaporization to
the fluid. In some cases it can also preheat the fluid then this section of vaporizers will be called upon
preheating zone and the other section in which latent heat is supplied; is known as vaporization zone
but he whole assembly will be called upon a vaporizer.
Vaporizers are called upon to fulfill the multitude of latent-heat services which are not a part of
evaporative or distillation process.
There are two principal types of tubular vaporizing equipment used in industry: Boilers and Vaporizing
Exchangers. Boilers are directly fired tubular apparatus, which primarily convert fuel energy into latent
heat of vaporization. Vaporizing Exchangers are unfired and convert latent or sensible heat of one fluid
into the latent heat of vaporization of another. If a vaporizing exchanger is used for the evaporation of
water or an aqueous solution, it is now fairly conventional to call it an Evaporator, if used to supply
the heat requirements at the bottom of a distilling column, whether the vapor formed be stream or not,
it is a Reboiler; when not used for the formation of steam and not a part of a distillation process, a
vaporizing exchanger is simply called a vaporizer. So any unfired exchanger in which one fluid
undergoes vaporization and which is not a part of evaporation or distillation process is a vaporizer.
The commonest type of vaporizer is the ordinary horizontal 1-2 exchanger or one of its modifications,
and vaporization may occur in the shell or in the tubes. If steam is the heating medium, the corrosive
action of air in the hot condensate usually makes it advantageous to carry out the vaporization in the
shell.
When a 1-2 exchanger is used as a vaporizer, it is filled with tubes and cannot be adapted for blow
down, since all the feed to a vaporizer is usually of value and a rejection as blow down is prohibitive.
If the feed were completely vaporized in the vaporizer, it would emerge as a vapor and any dirt which
was originally present would be left behind on the tube surface over which total vaporization of
occurred, fouling it rapidly, If the 1-2 exchanger (vaporization) were over- designed, that is, if it
contained too much surface, disengagement would have to occur on the tubes and due to the excess
surface the vapor would superheat above its saturation temperature.
The feed to a vaporizer should not be vaporized completely. The value of this rule is apparent. If less
that 100 percent to the feed is vaporized in 1-2 exchangers, the residual liquid can be counted on to
prevent the accumulation of dirt directly on the surface of the heating element. Maximum of about
80 percent vaporization appears to provide favorable operation in 1-2 exchanges, although higher
percentages may be obtained in vessels having interval disengagement space.
The true temperature difference is the weighted temperature difference for the two zones, and the clean
coefficient is the weighted clean coefficient.
Vaporizers tend to accumulate dirt, and for his reason higher circulation rates and large dirt factors
will often be desirable. Preference should be given to the use of square pitch and a removable tube
bundle. Although it may reduce the possibility of using a 1-2 vaporizing exchanger for other services,
the baffle spacing can be increased or staggered form inlet to outlet to reduce the pressure drop of the
fluid vaporizing in the shell.[17]
42
Design Calculation:
To prevent the total vaporization in the shell, total liquid entering the vaporizer will be…
Liquid entering the vaporizer = 11754/0.8 = 14692.5 lb/hr
The vapor should then disengaged from the liquid in the drum and the excess liquid return to the pump
suction for recombination with 11754 lb/hr of new feed.
The liquid separated from vapors in vaporizer drum = 14692.5 - 11754 = 2938 lb/hr
Thus for every 11754 lb/hr of O-xylene coming at 30oC, 2938 lb/hr at 360oC will also mixed with it
so that the inlet temperature will be 30*0.8 + 360*0.2 = 96oC
LMTD for Preheating:

Temperature
LMTD = [∆t2 - ∆t1]/ln (∆t2/∆t1)
LMTD = 244.41 0C
LMTD for Vaporization:

Temperature
LMTD = [∆t2 - ∆t1]/ln (∆t2/∆t1)
LMTD = 66.24 0C
Heat Duty:
Qp = 330660.46 W
Qv = 1496043.8 W
Weighted LMTD:
qp = 330660.46 / 244.41
43
qp = 1352.89
qv = 1496043.8 /57
qv = 26246.38
∑q/ΔT = 1826704/ 27600.27
∑q/ΔT = 66.380C = 339.38 K
Heat Transfer Area:

Q = UD ∆T
A = Q / UD∆T
Where,
Assume
UD=120 W/m2 K
Heat transfer area, A = 44.85 m2 = 482ft2
a” = 0.1963 ft2 /lin ft (From figure D.3 Appendix D)
n = 151
1
Corrected Area:
A = NT x L x a
= 521 ft2 = 48.5 m2

UD = 111 W/m2 0K = 20 BTU /(hr)(ft2)(oF)
44
Cold Fluid: Shell side, O-Xylene Hot Fluid: Tube side , Steam
Preheating:
Flow area:
Flow area:
at = 0.302 in (Table 10)
B = ID/5
at= Nt*A t/144n
= 17.25/5 166∗0.302
=
= 3.5 In 144∗2
as = ID*C*B/144Pt =0.174ft2
= 0.104 ft2 Mass velocity:
Mass velocity: Gt =W/at
G = W/as = 20650/0.174
= 11754/0.104 = 118678 lb/(ft2).(hr)
= 113019 lb/(ft2).(hr) De = 0.62/2 (Table `10)
At Tavg = 248oF = 0.0517 ft
µ = 0.31*2.42 At 689oF
= 0.747 lb/(ft).(hr) µ = 0.034 *2.42
De = 0.95/2 (Fig 28) = 0.08228 lb/(ft).(hr)
= 0.079 ft Re =De*G / μ
0.0517 ∗ 118678
Re = DeG/µ
0.08228
0.079∗113019
Re = Re = 74570
0.747
Re = 11952 Condensation of Steam
JH = 75 hio = 1500Btu/(hr).(ft 2 ).(0F)
At 248oF (47API)
1
𝐶 ∗ µ (3)
( )
𝑘
= 0.41 (From Fig 16)

k = 0.09 BTU/(hr)(ft2)(oF/ft)
45
0.09
ho = 75 ∗ ( ) ∗ 0.41
0.079
= 32 BTU/(hr).(ft 2 ).(0F)
Clean Overall Coefficient for Preheating Up

= 1500*32/1500+32
= 31.5 BTU/(hr)(ft2)(oF)
= 182 W/m2K
Ap = qp / Up (ΔTp)
Ap = 1352.89/182
Ap = 7.5 m2 = 80 ft2
Condensation of Steam
For Vaporizing:
hio = 1500Btu/(hr).(ft 2 ).(0F)
At Tavg = 292oF
µ = 0.22*2.42
= 0.50 lb/(ft).(hr)
De = 0.95/2 (Fig 28)
= 0.079 ft
Re = DeG/µ
0.079∗113019
Re =
0.50
Re = 17585
JH = 125
At 248oF (47API)
1
𝐶 ∗ µ (3)
( )
𝑘
= 0.87 (From Fig 16)

k = 0.087 BTU/(hr)(ft2)(oF/ft)
0.087
ho = 125 ∗ ( )∗ 0.87
0.079
46
= 118 BTU/(hr).(ft 2 ).(0F)
Clean Overall Coefficient for Vaporizing Uv

= 1500*118/1500+118
= 110 BTU/(hr)(ft2)(oF)
= 624W/m2K
Av = qv / Uv (ΔTv)
Av = 26246/624
Av = 41.2 m2
Total Clean Area:

Ac= Av + Ap
Ac = 41.2 + 7.5
Ac = 48.7 m2
Weighted Clean Overall Coefficient:
Uc = ∑ UA/Ac
Uc = (1352.89 + 26246)/48.7
Uc = 566 W/m2K
Uc = 101 BTU/(hr)(ft2)(oF)
Dirt Factor:
= 0.0031 (hr)(ft2)(oF)/BTU
47
Pressure Drop

Preheat:
Specific volume of steam from Table 7
Re = 11952
V= 0.115 ft2/lb
f = 0.000130 ft2/in2
S = (1/0.115)/62.5
Length of preheat zone
S = 0.144
Lp = L*Ap/Ac
f = 0.000160 ft2/in2
Lp =16*80/521
∆Pt = ½ * f G2 xLn/5.22x10 DΦt
Lp = 2.88 ft
= 1.4/2
No. of crosses
= 0.7 psi
N+1 = 12* Lp/B = 9.87
Da = 17.25/12
= 1.43ft
∆Ps = f G 2 (N+1)Da /5.22x10 DeΦs
∆Ps = 1.11 psi
Vaporization:
Re = 17585
f = 0.000127 ft2/in2
Length of Vaporization zone

= 16 – 2.88
=13.12ft
No. of crosses
N+1 = 12 *Lv/B = 44.98
Specific gravity at inlet= 0.81
Specific gravity at outlet = 0.09
S mean = 0.475
∆Ps = 1.39
∆Pt = 1.39 + 1.11 = 2.5psi
48
SPECIFICATION SHEET
Identification
Item Vaporizer E-202
Function
To Vaporize the Ortho -Xylene
Heat duty: 6232972 BTU/hr Area: 521 ft2
Fluid handled: O- Xylene Fluid handled: Steam
Flow rate: 11754 lb/h Flow rate: 20650 lb/h
t1=30 oC t2= 360 oC T1=: 365oF T2=365 oF
Shell: 17.25 in dia. Tubes:
Passes: 1 1 inch OD, 16 BWG, 1in square Pitch
Preheating: Number of tubes = 166
Reynolds number =11952 Length of tube = 16 ft
Heat transfer coefficient = 32 Btu/hr ft2F Passes: 2
Vaporization: Reynolds number = 99809
Reynolds number = 17585 Heat transfer coefficient = 1500 Btu/hr ft2 F
Heat transfer coefficient =110 Btu/hr ft20F Pressure drop = 0.7 psi
Pressure Drop = 2.50 psi
49
5.2 Reactor Design:

Introduction:
The reactor is the heart of a chemical process. It is the only place in the process where raw materials
are converted into products, and reactor design is a vital step in the overall design of the process. The
design of an industrial chemical reactor must satisfy the following requirements:
 The chemical factors: the kinetics of the reaction. The design must provide sufficient residence
time for the desired reaction to proceed to the required degree of conversion.
 The mass transfer factors: with heterogeneous reactions the reaction rate may be controlled by
the rates of diffusion of the reacting species; rather than the chemical kinetics.
 The heat transfer factors: the removal, or addition, of the heat of reaction.
 The safety factors: the confinement of hazardous reactants and products, and the control of the
reaction and the process conditions.
Principal types of reactor:

The following characteristics are normally used to classify reactor designs:
 Mode of operation: Batch or Continuous.
 Phases present: Homogeneous or Heterogeneous.
 Reactor geometry: Flow pattern and Manner of contacting the phases

Reactors are classified in the following broad category:
 Stirred tank reactor
 Tubular reactor
 Packed bed, fixed and moving

Including these there are also other types i.e. fluidized bed, micro channel reactor etc. In choosing the
reactor conditions, particularly the conversion, and optimizing the design, the interaction of the reactor
design with the other process operations must not be overlooked.
The degree of conversion of raw materials in the reactor will determine the size, and cost, of any
equipment needed to separate and recycle unreacted materials. In these circumstances the reactor and
associated equipment must be optimized as a unit.[18]
Selection of Reactor:
Selection of the reactor type for a given process is subjected to a number of considerations
 Temperature and pressure of the reaction.
 Need for removal or addition of the reactants and products.
 Phase of reaction
50
 Required pattern of the product delivery.
 Catalyst use consideration such as requirement for solid catalyst particle & contact with fluid
reactants and products.
 Relative cost of the reactor.

The design of the reactor must satisfy the following requirements:
Chemical factors: The design must provide sufficient residence time for the desired reaction to
proceed to the required degree of conversion.
Mass transfer factors: For example with heterogeneous reactions the reaction rate may be controlled
by the rates of diffusion of the reacting species; rather than the chemical kinetics.
Heat transfer factors: Removal or addition of the heat of the reaction.
Safety factors: The confinement of hazardous reactants and products, and the control of the reaction
and the process conditions.
Packed Catalytic Bed Reactor:

Catalysts change the reaction mechanism and therefore the rate of the reaction. If the reaction rate
increases, the reaction volume will decrease, reducing the cost of the reactor. Many chemical syntheses
are impractical without using a catalyst. If a pure catalyst is structurally weak and cannot be formed
into a pellet or is too expensive to use as a pellet, then the catalyst is deposited as a thin film on an
inert support. Because the reaction rate is proportional to the catalyst surface area, the pellet must be
porous to achieve a large surface area. Besides chemical properties of the catalyst, the mechanical
properties of the support material must also be considered when selecting a catalyst. Support materials
are mostly alumina, silica, activated carbon or diatomaceous earth, but alumina is more widely used
than the other materials. Pellets are usually molded or extruded into spheres, cylinders, or rings.
Extrusion is a lower cost operation than molding. The most common pellet diameters are 1/32, 1/16,
and 1/8 in (0.794, 1.59, and 3.18 mm). Pellets should have a high compressive strength to resist
crushing and abrasion and a low pressure drop to minimize compressor and power costs. Because
pellets are packed in a bed, the bulk crushing strength of the pellets limits the bed height. Selecting a
pellet size, shape, and porosity (void fraction in the pellet) is a trade-off between achieving high
reactivity, high crushing strength, and low pressure drop. Promoting high reactivity requires a porous
pellet with a large internal surface area, which requires small pores. Small pores, however, lower the
diffusion rate, reducing the pellet activity. The rate of diffusion increases with increasing pore size,
but the increased pore size reduces surface area and therefore reactivity. Consequently, there is an
optimum pore size that maximizes pellet reactivity.
Catalyst pellets are contained in a reactor in a single bed, multiple beds in a single shell, several packed
tubes in a single shell, or a single bed with imbedded tubes. Deviation from the simple single bed may
be required because of the need to add or remove heat, to redistribute the flow to avoid channeling, or
to limit the bed height to avoid crushing the catalyst.
51
Reactor Design:
Operating Conditions:
Inlet temperature = Tin = 663K
Outlet temperature = Tout 663k
Reaction Temperature = 633K
Reactions:
Main Reaction:
C8H10 + 3O2 C8H4O3 + 3H2O
O-xylene Phthalic anhydride
Side Reactions:
C8H10 + 15/2O2 C4H2O3 + 4H20 + 4CO2
O-Xylene Maleic anhydride

21
C8H10 + O2 8CO2 + 5H20
2
Mole Balance:
In – Out + Generation = Accumulation
𝑋
𝐹𝐴𝑂
𝑊= ∫ 𝑑𝑥 /−𝑟𝐴
0
Partial Pressure of O-Xylene = 0.223 atm

Partial Pressure of Oxygen = 0.413 atm
Rate law for first reaction:

27000
-rA = 𝑘𝑜 𝑒𝑥𝑝(19.837 − )p1p2
𝑅𝑇
R= 1.987 cal/mol K
ko = 1 kmol/(hr)(kg-cat)(atm)2
𝑟𝐴 = 0.018
𝐹𝐴 = 251.41 𝑘𝑚𝑜𝑙/ℎ𝑟
𝑊 = 9777 kg-cat
52
Rate law for second reaction:

27900
-rA = 𝑘𝑂 𝑒𝑥𝑝(19.837 − )p1p2
𝑅𝑇
𝑟𝐴 = 4.78 ∗ 10−3
𝑊 = 749 kg-cat
Rate law for third reaction:
28600
-rA = 𝑘𝑜 𝑒𝑥𝑝(18.97 − )p1p2
𝑅𝑇
R= 1.987 cal/molK
𝑟𝐴 = 2.12 ∗ 10−3
𝑊 = 6776 Kg-cat
Total Weight of Catalyst = 17302 Kg
Density of Catalyst = 3350 kg/m3
Volume of Catalyst = W/𝜌
Volume of Catalyst = 5.16 m3

Catalyst Particle density = 1.68g/cc
Catalyst Bulk density = 0.9 g/cc
Φ = 1 - Bulk density/ Particle density
Φ = 0.47
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐶𝑎𝑡𝑎𝑙𝑦𝑠𝑡
Volume of Reactor = 1−𝜑
5.16
=
1−0.47
=9.73m3
Diameter Calculation
𝜋𝐷2 𝐿
𝑉=
4
L/D =4
L =4D
𝜋4𝐷3
𝑉=
4
53
𝑉
𝐷3 =
𝜋
𝐷 = 1.45𝑚
𝐿 = 4 ∗ 1.45
𝐿 = 5.83𝑚
Space Time:
Space time = reactor volume/volumetric flow rate
Volumetric flow rate = 2.02 m3/s
Space time = 9.73/2.02
Space time = 5 s
No of Tubes:
Tube diameter is assumed to be 15-20 times the catalyst particle diameter
Dp =3mm
Assuming the diameter of one tube = 54mm
𝜋𝐷2 𝐿
Volume of one tube =
4
3.14∗0.0542 ∗5.83
=
4
= 0.0133m3
No of Tubes = Volume of Reactor / Volume of one Tube
No of Tubes = 529
Pressure Drop:
G(1 − Φ) 150(1 − 𝛷)µ
𝜷𝒐 = [ + 1.75𝐺]
gcρDpΦ3 𝐷𝑝
Ac = 1.13m2
G = Volumetric Flow rate /Ac *Density
G = 866 kg/m2s
Φ = 0.47
gc for metric system =1
Dp =0.003m
µ = 0.0013 kg/ms
54
Feed density = 433.4 kg/m3

Putting values in above eq. gives
𝜷𝒐 = 0.109= atm/m
𝑃 2𝛽𝑜𝐿 1/2
𝑦= (1 − )
𝑃𝑜 𝑃𝑜
P = 0.60Po
P = 1.2
ΔP = 0.8 atm
55
SPECIFICATION SHEET
Identification
Item Reactor R-401
Type Packed Bed Tubular

Reactor
Operating Pressure 2.4atm
Operating 633K
Temperature
Volume of Reactor 9.73 m3
Volume of Catalyst 5.16 m3
Weight of Catalyst 17303 kg
Diameter of Shell (D) 1.45 m
Height of Shell (L) 5.83 m
Pressure Drop 0.8atm
56
5.3 Gas Cooler Design (E-203):

Thermal Conductivity Btu/(hr)(ft2)(oF/ft)
Components 680oF 545 oF 482 oF
Air 0.0213 0.0217 0.0293
Water 0.0283 0.236 0.022
Carbon Dioxide 0.147 0.159 0.0236
Viscosity lb/(ft)(hr)
Components 680oF 545 oF 482 oF
Air 0.0914 0.069 0.064
Water 0.145 0.2213 0.2571
Carbon Dioxide 0.0934 0.0871 0.0826
LMTD for Desuperheating:

680oF Hot Temperature 98.78 oF 581.22 oF Δt2
545oF Cold 77 oF 468oF Δt1
Temperature
135 Difference 21.78 113.22 oF Δt2 – Δt1
LMTD = [∆t2 - ∆t1]/ln (∆t2/∆t1)
LMTD = 521 0F
LMTD for Condensation:

545oF Hot Temperature 104.35 oF 440.65 oF Δt2
545oF Cold 98.78 oF 446.22 oF Δt1
Temperature
0 Difference 5.57 oF -5.57 oF Δt2 – Δt1
LMTD = [∆t2 - ∆t1]/ln (∆t2/∆t1)
57
LMTD = 4430F
LMTD for Subcoolng:

545oF Hot Temperature 120 oF 425 oF Δt2
482oF Cold 104.35 oF 337.65 oF Δt1
Temperature
63 Difference 15.65oF 47.35 oF Δt2 – Δt1
LMTD = [∆t2 - ∆t1]/ln (∆t2/∆t1)
LMTD = 4010F
Heat Duty:
Total Heat duty = 7161216.9 Btu/hr
Qds (Desuperheating) = 4175096.50 Btu/hr
Qcond (Condensation) = 1068501.9 Btu/hr
Qsb (Suabcooling) = 1916697.20 Btu/hr
Mass flow rate of water = 191667.7 lb/hr
ΔT water for Desuperheating = 4175096.50/191667.7 = 21.78 oF
ΔT water for condensation = 1068501.9/191667.7 = 5.57 oF
Weighted LMTD:
Qds = 4175096.50/521
Qds = 8013
Qcond = 1068501.9/443
Qcond = 2411.96
Qsb = 1916697.20/401
Qsb = 4780
∑q/ΔT = 7161216.9/ 15204.96

∑q/ΔT = 471 oF
Heat Transfer Area:

Q = UD ∆T
A = Q / UD∆T
58
Where,
Assume
UD = 45 Btu/(hr)(ft2)(oF)
Heat transfer area, A = 337ft2
a” = 0.1963 ft2 /lin ft (From figure D.3 Appendix D)
n = 109
1
Corrected Area:
A = NT x L x a
A = 124*16*0.1963
A = 390 ft2

UD = 39 BTU /(hr)(ft2)(oF)
Hot Fluid: Shell side, Gases Hot Fluid: Tube side , Steam
Desuperheating:
Flow area:
Flow area:
at = 0.302 in (Table 10)
B = ID/5
at= Nt*A t/144n
= 15.25/5 124∗0.302
=
= 3 In 144∗2
as = ID*C*B/144Pt =0.130ft2
= 0.079 ft2 Mass velocity:
Mass velocity: Gt =W/at
G = W/as = 191667/0.130
= 105270.73/0.079 = 1474361 lb/(ft2).(hr)
= 1332540 lb/(ft2).(hr) De = 0.62/2 (Table `10)

= 0.0517 ft
59
At Tavg = 600oF At 67oF
µ = 0.236 lb/(ft).(hr) µ = 1.96 lb/(ft).(hr)

De = 0.95/2 (Fig 28) Re =De*G / μ
= 0.079 ft 0.0517 ∗ 1474361
1.96
Re = DeG/µ
Re = 38890
0.079∗1332540
Re =
0.236
Re = 445635 Heat Transfer Coefficient of Water
JH = 380 hio = 800Btu/(hr).(ft 2 ).(0F)

1
𝐶 ∗ µ (3)
( )
𝑘
= 0.529

k = 0.0267 BTU/(hr)(ft2)(oF/ft)
0.0267
ho = 380 ∗ ( ) ∗ 0.529
0.079
ho = 65 BTU/(hr).(ft 2 ).(0F)
Clean Overall Coefficient for desuperheating

= 800*65/800+65
= 58 BTU/(hr)(ft2)(oF)
Ads = Qds / Uds (ΔTds)
Ads = 8013/58
Ads = 151 ft2
For Condensation:
Heat Transfer Coefficient of Water:
At T = 545oF
hio = 800Btu/(hr).(ft 2 ).(0F)
µ = 0.294 lb/(ft).(hr)
De = 0.95/2 (Fig 28)
= 0.079 ft
60
Re = DeG/µ
0.079∗1332546
Re =
0.294
Re = 358065
JH = 300
1
𝐶 ∗ µ (3)
( )
𝑘
= 0.527
k = 0.0273 BTU/(hr)(ft2)(oF/ft)
0.0271
ho = 300 ∗ ( ) ∗ 0.527
0.079
ho= 47 BTU/(hr).(ft 2 ).(0F)
Clean Overall Coefficient for Condensation

= 800*47/800+47
Acond = Qcond / Ucond (ΔTcond)
Acond = 2411.96/42
Acond = 68 ft2
For Sub cooling:

At T = 500oF
Heat Transfer Coefficient of Water:
µ = 0.312 lb/(ft).(hr)
hio = 800Btu/(hr).(ft 2 ).(0F)
De = 0.95/2 (Fig 28)
= 0.079 ft
Re = DeG/µ
0.079∗1332546
Re =
0.312
Re = 3100208
JH = 280
61
1
𝐶 ∗ µ (3)
( )
𝑘
= 0.526
k = 0.0271 BTU/(hr)(ft2)(oF/ft)
0.0271
ho = 280 ∗ ( ) ∗ 0.526
0.079
ho= 41 BTU/(hr).(ft 2 ).(0F)
Clean Overall Coefficient for Condensation

= 800*41/800+41
Asb = Qsb / Usb (ΔTsb)
Asb = 4780/38 = 123 ft2
Total Clean Area:

Ac= Ads + Acond + Asb
Ac = 344 ft2
Weighted Clean Overall Coefficient:
Uc = ∑ UA/Ac
Uc =15204.96/144
Uc = 46 Btu/(hr)(ft2)(oF)
Dirt Factor:
= 0.0036 (hr)(ft2)(oF)/BTU
62
Pressure Drop

Desuperheat:
Re = 38890
Re = 446835
f = 0.00019 ft2/in2
f = 0.00011 ft2/in2
∆Pt = f G2 xLn/5.22x10 DΦt
Length of desuperheating zone
0.00019∗14743612 ∗16∗2
Lds = L*Ads/Ac ∆P=
5.22∗1010 ∗0.0517∗1∗1
Lds =16*151/390 ∆P = 4.89psi
Lds = 6.19ft 4∗𝑛 𝑉2
∆P =
𝑠
(2𝑔)
No. of crosses
4∗2
N+1 = 12* Lds/B = 24 ∆P = (0.02)
1
Da = 15.25/12 ∆P = 0.16 psi

= 1.27ft ∆PT = 5.05 psi
S 0.78
∆Pds = f G 2 (N+1)Da /5.22x10 DeΦs
0.0011∗13325402 ∗24
∆Pds =
5.22∗1010 ∗1.27∗1∗0.8
∆Pds = 0.88 psi
Condensation:
Length of desuperheating zone
Lcond = L*Acond/Ac
Lcond =16*68/390
Lcond = 2.78 ft
No. of crosses
N+1 = 12 *Lcond/B = 11
∆Pds = f G 2 (N+1)Da /5.22x10 DeΦs
0.0011∗13325402 ∗11
∆Pds =
5.22∗1010 ∗1.27∗1∗0.8
∆Pds = 0.4 psi
63
Sub cooling:
Length of zone = 7.03
No. of crosses
N+1 = 12 *Lb/B = 28
∆Psb = f G 2 (N+1)Da /5.22x10 DeΦs
0.0011∗13325402 ∗28
∆Psb =
5.22∗1010 ∗1.27∗1∗0.8
∆Psb = 1.21 psi
∆Pt = 0.4 + 0.8 + 1.21 =2.41 psi
64
SPECIFICATION SHEET
Identification
Item Gas Cooler (E-203)
Function
To lower the temperature of Product Gases
Heat duty: 7161216.9 BTU/hr Area: 521 ft2
UD assumed: 45 Btu/hr ft20F UD calculated: 38 Btu/hr ft20F
Fluid handled: Product Gases Fluid handled: Water
o o
t1=680 F t2= 482 F T1=: 77oF T2=120 oF
De superheating: Number of tubes = 124
Reynolds number =445635 Length of tube = 16 ft
JH = 380 Passes: 2
2
Heat transfer coefficient = 58 Btu/hr ft F Reynolds number = 38890
Condensation: Heat transfer coefficient = 800 Btu/hr ft2 F
Reynolds number = 358065 Pressure drop = 5.05 psi
JH = 300
Heat transfer coefficient =42 Btu/hr ft20F
Sub cooling:
Reynolds number = 3100208
JH = 280
65
SPECIFICATION SHEET
Identification
Item Gas Cooler (E-204)
Function
To lower the temperature of Product Gases
Heat duty: 7161216.9 BTU/hr Area: 521 ft2
UD assumed: 45 Btu/hr ft20F UD calculated: 36 Btu/hr ft20F
Fluid handled: Product Gases Fluid handled: Water
t1=482 oF t2= 293 oF T1=: 77oF T2=120 oF
De superheating: Number of tubes = 124
Reynolds number = 395400 Length of tube = 16 ft
JH = 380 Passes: 2
2
Heat transfer coefficient = 54 Btu/hr ft F Reynolds number = 27342
Condensation: Heat transfer coefficient = 800 Btu/hr ft2 F
Reynolds number = 289060 Pressure drop = 3.81 psi
20
Heat transfer coefficient =40 Btu/hr ft F
Sub cooling:
Reynolds number = 265128
66
5.4 Vapor liquid separator design

Introduction:-
The vapor liquid separators are used to separate two phase inlet into pure vapors and pure liquid. It
basically helps in recovering valuable products and improves product purity. If two phase separators
are used after flashing a hot liquid across a valve, it is called a flash separator.
Types of Separators:
 Vertical Separator.
 Horizontal Separator.
 Knockout Drum.
Vertical Separator:
 Used where vapor flow is large as compared to liquid flow.
 Good separation efficiency.
 By rule of thumb it is commonly preferable in oil refineries.
 50% LL must be retained in the separator during operation.
Horizontal Separator:
 Used when the liquid content of the incoming stream is high.
L/D ratio specification:
 (L/D) ratio is 2 for the case of knockout drum.
 If length to diameter (L/D) ratio lies between 3 and 5, then it will be vertical separator.
 If length to diameter (L/D) ratio is greater than 5 then it will be horizontal separator.
Phenomenon:
The vapor & liquid mixture is separated by gravity and impaction in the separator. The mixture enters
the separator and strikes the splash plate where it loses its momentum. Most of the liquid flows
downwards and vapors along with liquid drop flow upward. As the vapor rises, large drops settle to
the bottom of separator by gravity. Normal separation efficiency is 95% which can be increased to
99.9% by using a mist eliminator. Vortex formation must be prevented to reduce gas entrainment in
the liquid by using a vortex breaker at the bottom
Internal Accessories:
 Splash Plate.
 Vortex Breaker
67
 Mist Eliminator
Figure 5.0.1: Vertical Separator
Splash Plate:
It is used to cause the initial bulk separation of liquid and gas. It provides a means to cause a sudden
and rapid change of momentum (velocity and direction) of the entering stream. If it is not present then
the vapors will escape very rapidly without contacting with liquid to establish equilibrium.
Vortex Breaker:
A vortex breaker is normally installed on the liquid outlet to prevent formation of vortex when the
liquid outlet valve is open. The formation of a vortex at the liquid outlet may result in withdrawal and
entrainment of gas with the exiting liquid. This causes the loss of valuable vapors, pump damage and
abnormal liquid level readings.
Mist Eliminator:
Mist elimination or demisting can be defined as the mechanical separation of liquids from gases. Mesh
usually consists of 0.011inch diameter wires to form a pad of 4 to 6 inches thick & pressure drop is
less than 1inch of water.
Design steps:
 Calculate vapor velocity.
 Calculate cross-sectional area.
 Calculate diameter.
 Calculate vapor height.
 Calculate volume.
68
 Calculate liquid height.
 Calculate total length.
 Check L/D ratio. [14]

Operating conditions:
 Design Pressure = 1.01 bar
 Design Temperature = 145oC
 Mass flow rate of liquid = 5424.8 kg/hr
 Mass flow rate of vapor = 42327 kg/hr
 Volumetric flow rate liquid = 0.001 m3/s
 Volumetric flow rate of vapor = 12.73 m3/hr
 Density of liquid = ρl = 1288 kg/m3
 Density of vapor= ρv = 77.35 kg/m3
Component Density (kg/m3)

Nitrogen 0.808
Oxygen 0.921
Carbon Dioxide 1.267
Water 926
Phthalic Anhydride 1297
Maleic Anhydride 1191
Calculation of vapor velocity:
Select Kv value and put in the equation given below:
Kv = 1.34 m/s with a mist eliminator
Maximum vapor velocity (Shouder Brown Equation):

𝜌𝑙 − 𝜌𝑣 1/2
𝑣𝑣 = 𝑘𝑣 ∗ ( )
𝜌𝑣
Where,
Velocity factor Kv= 1.34 m/sec
ρv= density of liquid kg/m3
ρl= density of vapor kg/m3
Vv = 4.89 m/s
Calculation of cross-sectional area:
69
A = Q v /Vv
A = 12.73/4.89
A = 2.61 m2
Where Qv=volumetric flow rate of vapor (m3/s).
Calculate diameter:
4𝐴
𝐷=√
𝜋
Put the value of A in above equation.
4 ∗ 2.61
𝐷=√
3.14
D = 1.81m
Selection of surge time:

Feed to column:
Surge time = 5min.
Height of separator:
Vapor Height hv:
hv = 1.5D + 1.5
hv = 1.5 (1.81)+ 1.5= 4.215 m
Liquid Height hL :
hL = (Q L× t)/A
hL = (0.007 * 5)/1.81= 0.19 m
Total height:
h = hL+ hv
= 4.21+0.19
= 4.31
Check L/D ratio:

L/D = 4.31/1.81m = 2.138 > 2
So we can use vertical separator
70
SPECIFICATION SHEET
Identification
Item Gas liquid separator F-501
Type Phase separator

Function
To separate the vapor and liquid.
No. Required 1
Mist Eliminator Vane type
Pressure 1atm
Temperature 145°C
Diameter 1.81m
Length 4.31m
71
5.5 Dowtherm A Cooler Design (E-205):
Dowtherm A
Temperature = 115oC
Cooling Water
Temperature = 40oC
Cooling Water
Temperature = 25oC
Dowtherm A
Temperature = 45oC
Figure 5.0.2: Dowtherm A Cooler
Cold Stream (water)
tin = 77℉
t out = 104℉
t mean = (77 F + 104 F)/2
t mean = 90.5 ℉
µ = 1 cp
Hot Stream (Dowtherm)
Tin = 239℉
Tout = 113℉
T mean = (239F + 113F)/2
T mean =176F
µ = 0.42 cp
Δt = (T1 – t2)-(T2 – t1)/ln(T1- t2)/ T2- t1)
Δt = 74.90 ℉
Kc=0.93
72
Fc = 0.94
Assume
UD = 70 45 Btu/(hr)(ft2)(oF)
A = Q/Ud* Δt
A =47.83 ft2
Calculation of Tc & tc
Tc = T1 + Fc*(T1 – T2)
Tc= 157℉
tc= t1+Fc*(t2-t1)
tc= 87 ℉
Hot Fluid: Annulus (Dowtherm) Cold Fluid: Inner Pipe (water)

Flow area: Flow area:
D2 = 2.067 D=1.38 in.
D2 =2.067/12 D=1.38/12
D2 =0.1725 ft D=0.115 ft
D1 = 1.66
D1 =1.66/12 πD2
ap =
D1=0.138 ft 4
3.14×0.1152
= 4
Area
= 0.0104 ft 2
aa= ᴫ(D22-D12)/4
aa= 3.14*(0.17252-0.1382)/4 Mass velocity:
=0.00826 ft2 Ga=W/a
Ga=5767/0.0104
Equivalent diameter: =554326.9 lb/hr.ft2
De=(D22-D12)/ D1
De=(0.17252-0.1382)/0.138 Reynold’s number:
=0.0762 ft At T = 87 oF μ= 0.8 cp
µ = 0.8×2.42
Mass velocity: µ= 1.93 lb/ft.hr
Ga=W/a
Ga=1770/0.00826 Re = De Ga/ μ
=215853.73 lb/(hr)(ft2) =33029.84
Reynold’s number JH= 95

At T = 157 oF μ= 1.43 cP Prandtl number
At t = 87℉
73
μ = 1.43 cp × 2.42 c = 0.97 Btu/(lb).(℉)

μ =3.46 lb / (ft)(hr) k = 0.356 BTU/(hr)(ft2)(oF/ft)
Rea = De Ga/ μ 𝐤 𝟑 𝐜𝛍
𝐡𝐢 = 𝐣𝐡 𝐝 √ 𝐤
=4753.77
= 500.19 Btu/(hr)(ft2)(℉)
JH = 25
Correct hi to the surface at the OD
Prandtl number
𝐈𝐃
At t = 157 ℉ 𝐡𝐢𝐨 = 𝐡𝐢 × 𝐎𝐃
c = 0.42 Btu/(lb)(℉) hio = hi * (ID/OD)
k = 0.0720 BTU/(hr)(ft2)(oF/ft) = 415.56 Btu/(hr)(ft2)(℉)
𝐤 𝟑 𝐜𝛍 Uw=1.93lb / ft.hr
𝐡𝟎 = 𝐣𝐡 𝐃 √ 𝐤
𝐞
= ( μ/ μw)0.14
= 58.28Btu/(hr)(ft2)(℉) =1
tw=tc+ho / hi + ho(Tc-tc)
Tw=95.39F
Uw =2.8*2.42
μw =6.77 lb / (ft)(hr)
=( μ/ μw)0.14
=0.90
ho=0.90*58.2
=52.97
Clean overall coefficient, Uc

hio ×ho
Uc =
hio +ho
415×52.97
Uc =
415+52.97
=47 Btu/hr.ft2. ℉
Design overall coefficient, UD

1 1
= + Rd
UD UC
1 1
= + 0.006
UD 47
UD = 36.37 Btu/hr.ft2. ℉
74
Required surface:
Q
A=
UD ×∆t
155655.18
A=
36.37 × 74.08
A = 70.84 ft2
Required length =70.84/0.435 = 162 lin. Ft
This can be fulfilled by connecting Four 40-ft hairpins in series.
The surface supplied will actually be

A =162*0.435 =71 ft2
Actual design coefficient is,
Q
UD =
A′ × ∆t
UD =30.51 Btu/(hr)(ft2)(℉)
U −U
R d = UC×UD
C D
R d = 0.0055 (hr)(ft2)(℉)/(Btu)
Pressure Drop
Annulus: Dowtherm For Rep =33029.2

.De ′ for pressure drop differs from 0.264
f = 0.0035 + 0.42
De for heat transfer. Rep
De= (D2 − D1 ) 0.264
f = 0.0035 +
De= 0.1725 − 0.138 33029.20.42
=0.0345 ft f = 0.0063
De′ Ga S = 0.96
Rea ′ = μ
ρ = 62.5× 0.8
Rea ′ = 2152.39 = 60.75 lb/ft3
0.264
f = 0.0035 + Re0.42 𝟒𝐟𝐆𝐩𝟐 𝐋
a .∆𝐅𝐩 = 𝟐𝐠𝛒𝟐 𝐃
0.264
f = 0.0035 + 2152.390.42 4 × 0.0041 × 527837.52 × 310
f = 0.0140 ∆Fp =
2 × 4.18 × 108 × 53.752 × 0.115
S = 0.87 ∆Fp =7.22 Ft
ρ = 62.5× 0.84 =54.5 lb/ft3
∆Fp × ρ
∆Pp =
144
75
𝟒𝐟𝐆𝟐 𝐋 7.22 × 53.75

∆𝐅𝐚 = 𝟐𝐠𝛒𝟐𝐚𝐃 ∆Pp =
𝐞′ 144
∆Fa = 8.68 ft ∆Pp = 2.69 psi
𝐆
𝐕 = 𝟑𝟔𝟎𝟎𝛒
417969.73
V=
3600 × 52.5
V = 1.211 fps
V2
Ft = 3 × ( )
2g′
1.2112
Ft = 3 × ( )
2 × 32.2
=0.056 ft
ρ
∆Pa = (∆Fa + Fl ) ×
144
∆Pa = 5.8 psi

Allowable ∆Pa=10 psi
76
Specification sheet
Identification
Item: Heat Exchanger (E-205)
Type: Double Pipe
Function:
To increase the temperature of Dowtherm A
Heat Duty: 113350.18 Btu/hr
Annulus Inner Pipe
Fluid: Hot Fluid: Cold
Flow rate: 803 kg/hr Flow rate: 2490 kg/hr
0
Temperature: 239 to 113 F Temperature: 77 to 104 C0
Uc Calculated: 21.89 Btu/hr.ft2.F0 UD Calculated: 19.51 Btu/hr.ft2.F0
Dirt Factor: 0.0055 Btu/hr.ft2.F0 Number of Hairpins: 8(20ft Each)
Pressure Drop: 5.8 psi Pressure Drop: 2.69 psi
77
5.6 Distillation Column Design:

Introduction to distillation column
In industry it is common practice to separate a liquid mixture by distilling the components, which have
lower boiling points when they are in pure condition from those having higher boiling points. This
process is accomplished by partial vaporization and subsequent condensation.
“It is a process in which a liquid or vapor mixture of two or more substances is separated into
its component fractions of desired purity, by the application and removal of heat”.
The creation or addition of another phase in distillation is obtained by the repeated vaporization and
condensation of the fluid. The separation process exploits the differences in vapor pressure of key
components in the mixture initiate the separation.
The advantages of distillation are its simple flow sheet, low capital investment and low risk. The
separation process is able to handle wide ranges of feed concentrations and throughputs while
producing a high purity product.
Types of distillation column:
There are many types of distillation columns, each designed to perform specific types of separations,
and each design differs in terms of complexity.
 Batch columns
 Continuous columns
Batch Columns:
In batch operation, the feed to the column is introduced batch-wise. That is, the column is charged
with a 'batch' and then the distillation process is carried out. When the desired purification of product
is achieved, a next batch of feed is introduced.
Continuous Columns:
In contrast, continuous columns process a continuous feed stream. No interruptions occur unless there
is a problem with the column or surrounding process units. They are capable of handling high
throughputs and are the more common of the two types. We shall concentrate only on this class of
columns.
Choice between packed and plate column

Vapor liquid mass transfer operation may be carried either in plate column or packed column. These
two types of operations are quite different. A selection scheme considering the factors under four
headings,
 Factors that depend on the system i.e. scale, foaming, fouling factors, corrosive systems, heat
evolution, pressure drop, liquid holdup.
 Factors that depend on the fluid flow moment.
78
 Factors that depends upon the physical characteristics of the column and its internals i.e.
maintenance, weight, side stream, size and cost.
 Factors that depend upon mode of operation i.e. batch distillation, continuous distillation,
turndown, and intermittent distillation.
The relative merits of plate over packed column are as follows:
 Plate column are designed to handle wide range of liquid flow rates without flooding.
 If a system contains solid contents, it will be handled in plate column, because solid will
accumulate in the voids, coating the packing materials and making it ineffective.
 Dispersion difficulties are handled in plate column when flow rate of liquid are low as
compared to gases.
 For large column heights, weight of the packed column is more than plate column.
 If periodic cleaning is required, man holes will be provided for cleaning. In packed columns
packing must be removed before cleaning.
 For non-foaming systems the plate column is preferred.
 Design information for plate column is more readily available and more reliable than that for
packed column.
 Inter stage cooling can be provide to remove heat of reaction or solution in plate column.
 When temperature change is involved, packing may be damaged.
 Plates are mostly used for large diameter more than 0.6m
Choice of plates in column:

There are four main tray types, the bubble cap, sieve tray, ballast or valve trays and the counter flow
trays. I have selected sieve tray because:
 They are lighter in weight and less expensive. It is easier and cheaper to install.
 Pressure drop is low as compared to bubble cap trays.
 Peak efficiency is generally high..
Main components of distillation column:

Column internals such as trays/plates and/or packing which are used to enhance component
separations.
 A reboiler to provide the necessary vaporization for the distillation process. The liquid removed
from the reboiler is known as the bottoms product or simply, bottoms.
 A condenser to cool and condense the vapor leaving the top of the column. The condensed
liquid that is removed from the system is known as the distillate or top product.
79
 A reflux drums to hold the condensed vapor from the top of the column so that liquid (reflux)
can be recycled back to the column. The condensed liquid is stored in a holding vessel known
as the reflux drum. Some of this liquid is recycled back to the top of the column and this is
called the reflux.
Factor affecting the distillation column operation:
Vapor Flow Conditions:
Adverse vapor flow conditions can cause:
 Foaming.
 Entrainment.
 Weeping/dumping.
 Flooding.
Foaming: Foaming refers to the expansion of liquid due to passage of vapor or gas. Although it
provides high interfacial liquid-vapor contact, excessive foaming often leads to liquid buildup on trays.
In some cases, foaming may be so bad that the foam mixes with liquid on the tray above. Whether
foaming will occur depends primarily on physical properties of the liquid mixtures, but is sometimes
due to tray designs and condition. Whatever the cause, separation efficiency is always reduced.
Entrainment: Entrainment refers to the liquid carried by vapor up to the tray above and is again caused
by high vapor flow rates. It is detrimental because tray efficiency is reduced: lower volatile material is
carried to a plate holding liquid of higher volatility. It could also contaminate high purity distillate.
Excessive entrainment can lead to flooding.
Weeping/Dumping: This phenomenon is caused by low vapor flow. The pressure exerted by the vapor
is insufficient to hold up the liquid on the tray. Therefore, liquid starts to leak through perforations.
Excessive weeping will lead to dumping. That is the liquid on all trays will crash (dump) through to
the base of the column (via a domino effect) and the column will have to be re-started. Weeping is
indicated by a sharp pressure drop in the column and reduced separation efficiency.
Flooding: Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the
vapor up the column. The increased pressure from excessive vapor also backs up the liquid in the down
comer, causing an increase in liquid holdup on the plate above. Depending on the degree of flooding,
the maximum capacity of the column may be severely reduced. Flooding is detected by sharp increases
in column differential pressure and significant decrease in separation efficiency.
Reflux Conditions: Minimum trays are required under total reflux conditions, i.e. there is no
withdrawal of distillate. On the other hand, as reflux is decreased, more and more trays are required.
Vacuum Distillation:
Vacuum distillation is considered when the boiling point of the component (or the solvent) is very high
(Tb >150oC) in order to distill the compound without substantial decomposition. Vacuum distillation
80
is the distillation of liquids achieved at a pressure under atmospheric pressure to take benefit of the
statement that decreasing the pressure depresses the boiling point of liquids.
The distillation process that take place under one atmosphere and in vacuum is known as as vacuum
distillation. Low pressure allows vaporization at low temperatures. Due to this, heating and cooling
both needs fewer energy and make it energy effective process
Design calculations:
 Designing steps of distillation column:
 Bubble point and dew point calculations.
 Calculation of Minimum number of stages.(Nmin).
 Calculation of Minimum Reflux Ratio Rm.
 Calculation of Actual Reflux Ratio R.
 Calculation of theoretical number of stages.
 Calculation of actual number of stages.
 Determination of Physical properties of top and bottom product.
 Calculation of diameter of the column.
 Calculation of weeping point, entrainment etc.
 Calculation of pressure drop.
 Calculation of the height of the column.
Bubble point and dew point calculations:

For feed:
Bubble point:
P= 0.06 atm
Tb = 145 °C [Bubble point]
Components Xf Po K Y
Phthalic Anhydride 0.859421 12.7003 0.2785 0.2367
Maleic Anhydride 0.146915 232.307 5.0944 0.7641
ΣY = 1
P = 0.06 atm
Td = 177 °C [Dew point]
81
Components Xf Po K X
ΣX = 1
For Top Product:

P = 0.06 atm
Tb = 140 °C [Bubble Point]
Components Xd Po K Y
ΣY = 1
P = 0.06 atm
Td =165°C [Dew point]
Components Xd Po K X
ΣX = 1
For Bottom Product:

P = 0.06 atm
Tb = 180 °C [Bubble Point]
Components Xf Po K Y
ΣY = 1
P = 0.06 atm
Td = 190 °C [Dew point]
82
Components Xf Po K X
ΣX = 1
F = 5424.8 kg/hr
V = 366.7 kg/hr
L = 5056 kg/hr
Vapor pressure of Phthalic Anhydride
A B C
15.99 4467.23 -83.15
T =145oC
Ln P = A – B / (C + T)
𝑙n P = 15.99 – 4467.23 / (284+ 273) + (−83.15)
PPa= 376.53 mmHg
Vapor pressure of Maleic Anhydride
A B C
16.15 3765.65 -82.15
T = 145oC
Ln P =A - B / (C + T)
𝑙n P = 16.15 – 3765.65 / (202+ 273) + (−82.15)
PMa = 715.51mmHg
Now
Relative volatility = (vapor pressure of MA/ vapor pressure of PA)

= 1.90
𝑎𝑥
Y=
1+(𝑎−𝑥)∗𝑥
83
X 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

Y 0.17 0.32 0.45 0.560.65 0.65 0.740 0.81 0.88 0.94 1
Calculating minimum reflux ratio

As we know that :
𝑅𝑚𝑖𝑛 𝑋𝑑−𝑌′
=
𝑅𝑚𝑖𝑛+1 𝑋𝑑− 𝑥′
Y’=0.91
0.96−0.91
=0.96−0.85
Rmin = 0.81
R =1.5*Rmin
=1.2
Top operating line

1
Yn+1 = 𝑅+1xd
Y1 =0.43
Calculating no. of theoretical and real plates:

From graph;
No. of plates = n-1
=16-1
=15
Assuming efficiency =75%
𝑛𝑜 𝑜𝑓 𝑖𝑑𝑒𝑎𝑙 𝑝𝑙𝑎𝑡𝑒𝑠
ῃ = 𝑛𝑜 𝑜𝑓 𝑟𝑒𝑎𝑙 𝑝𝑙𝑎𝑡𝑒𝑠
15
No. of real plates = 0.75 = 20
84
Figure 5.0.3: Mccabe thiele Method
Calculating flooding velocity

At top plates
Ln = R*D
= 1.2*421.11
=505.332
Vn = Ln +D
=505.33+ 421.11
=926.44
At bottom plates
W = 5044.8
Lm = Ln + F
=505.33 + 5555.71
85
=6061.04
Vm = Lm – W
=6061.04– 5044.8
=1016.24
Density at top
Temp = 145oC
ρ =404.99Kg/m3 (density of liquid)
ρ =2.81kg/m3 (density of Vapor)
Density at Bottom
Temp = 177oC
ρ =4895.5Kg/m3 (density of liquid)
ρ =3.75kg/m3 (density of Vapor)
Calculation for diameter of column:

For calculation of diameter of column we have to calculate the maximum volumetric flow rate of top
and bottom vapors and liquid.
Maximum volumetric flow rate of Vapor:

926.44
Top =
2.81∗3600
= 0.09m3/s
𝟏𝟎𝟏𝟔.𝟐𝟒
Bottom =
𝟐.𝟖𝟏∗𝟑𝟔𝟎𝟎
=0.097 m3/s
Maximum Volumetric flow rate of liquid:

505.32
Top =
404.9∗3600
= 0.000346 m3/s
6061.04
Bottom =
4895.5∗3600
=0.000347 m3/s
86
Calculate FLV = liquid vapor flow factor:

For Top:
505.332 2.81
FLV = 926.44 √404.99
=0.045
For Bottom:
6061 3.75
FLV = 1016.24 √44895.5
=0.16
Select trial spacing:
Initially let’s assume that our diameter of column is 1-3m.
And for that a tray spacing of Ts=600 mm.
Flooding parameter:
Now from the graph the flooding parameter is selected:
We have K1 = 0.134 (for top condition)
And also K1 = 0.101(for bottom condition)
liquid surface tension = 53.7 dynes/cm or 0.0355N/m
Vnf = gas velocity through the net area at flood, m/s
At Top.
Vnf = K1 × (σ/20) 0.2 × [(ρL – ρV)/ ρv] 0.5
Vnf =1.602 m/s
At Bottom
Vnf = K1 × (σ/20) 0.2 × [(ρL – ρV)/ ρv] 0.5
Vnf =2.97 m/s
let assume that our Flooding = 85 %
At Top
Actual velocity, Vn = 0.85× Vnf
i-e Vn = 1.3m/s
87
At Bottom
Actual velocity, Vn = 0.85× Vnf
i-e Vn =2.97m/s
Net column area used in separation is

An = Qmax/Vn
An = 0.091/1.3
An = 0.8m2
For Bottom Section

An = Q/Vn
An =0.97/2.97
= 0.329m2
Diameter of the column at the bottom
D = √ (4 * Ac/)
= √ (4×0.329)/ (3.14)
D = 0.686 m (based on bottom condition).
So this is for top conditions same procedure is adopted for bottom condition so for bottom the diameter
is D = 0.68 m (based on bottom condition).
Provisional Plate Design:
Column diameter (base) = 0.68 m
Column Area Ac  d 2

4
Ac = 0.36m2
Down comer area Ad  0.36  0.12 = 0.0432m2

Net area An = Ac – Ad
Net area An =0.362 - 0.043= 0.319m2
Active area Aa =Ac – 2Ad =0.36– 2× (0.043) = 0.276 m2
Hole area AH:
Take 10% Aa as first trial = 0.1 ×0.8585 = 0.0276m2
88
Weir length:
First calculate the ratio of down comer area to the total cross-sectional area:
Ad / Ac= 0.043/ 0.362 = 0.118
Ad / Ac= 0.11×100 = 12%
(From figure A.1 Appendix A)
Lw/dc = 0.78
Lw  0.78  0.68 =0.53 m
Weir height:
(Recommended = 40 to 50mm)
Take weir height, hw= 50 mm=0.05m
Hole diameter, dh = 5 mm = 0.005m
Plate thickness = 5 mm= 0.005m
Check Weeping:
Maximum liquid rate= Lw = 1.68m3/sec
Minimum liquid rate at 70% turn down  0.7  1.68= 1.176m3/sec
Height of liquid crest over segmental weir:
how = weir crust
For segmental down comer:

1.176
Maximum h ow = 750*(409.99∗0.51)2 3 /
=23.84 mm of liquid (minimum)
At minimum hw + how = 50 + 23.84= 73.84 mm liquid
Minimum design vapor velocity:
(From figure A.2 Appendix A) we get;
K2= 30.60
Now as we know the value of K2 and also the dh hole diameter so we get the minimum vapor velocity.
30.6−0.9(25.4−5)
Umin  m/s
(√2.81
minimum vapor volumetric flow rate

Actual minimum vapor velocity = 𝐴𝑘

0.7∗0.091
 
0.276

=2.73m/s
89
Pressure drop:
There are two types of pressure drops one known as dry plate pressure drop and the other is when the
liquid is present on the plate the total pressure is the sum of all the pressure drops on the plate. The
relationship of pressure drop is given by:[14]
ht = hd + (hw + how) + hr
Dry Plate pressure drop (hd):

Vapor velocity through holes is
Uh = Vapor volumetric flow Rate/Hole Area
Uh =0.091/0.0276 = 3.848 m/sec
Plate thickness / hole dia = 5 / 5 = 1.0
And
Ah/Ap = Ah/Aa = 0.1or 10%
(From fig A.3 Appendix A)
Co = 0.84
Now
3.29 2 2.81
Hd =51( )( )
0.84 404.62
=5.42 mm liq.
Residual Head:
12.5∗1000
hr = 404.99
=30.45 mm liq.
Total Pressure Drop:
Total pressure drop = 3.39 + (80.18) + 13
ht = 96.47 mm liquid.
Down comer Liquid Backup:
Take hap = hw – 10 = 40 mm
Area under apron = hap×Lw

= 0.51× (0.4/1000) = 0.020 m2
90
0.14
hdc =166( )2
404∗0.02
=7mm liq.
Backup in down comer
hb= (hw + how) + ht + hdc=(64.73) + 112.42 +1.78
=183.76 mm liquid = 0.183 liquid m

½ (Tray spacing + weir height) = [½ × (600 + 50)] = 0.350m
0.183 < ½ (Tray spacing + weir height)
Check Residence Time:
tr = (Ad* hbc* ρL)/Lwd

tr=0.093*0.183*404.99/1.68
tr = 5.7sec
It should be > 3 sec. so, result is satisfactory.
Check Entrainment:
Uv = Maximum Volumetric Flow Rate of vapors/Net Area
UV = 0.09 /0.3= 0.33 m/s
Percent flooding = 0.33/2.9
= 33 or 33 %
From figure 11.29
Fractional Entrainment  = 0.025well below 0. 1 Satisfactory
No of Holes:
Diameter of one hole = 5 mm =0.005 m
Area of one hole = 22/7*(0.005 /2)2 = 1.9635 *10-6
Total Hole Area = 0.05*0.276=0.013 m2
No of Holes =0.013 m2 / 1.9635 * 10-6 = 665.16 holes
Height of column can be calculated by following formula:
Hc= (Nact-1) Hs+ ∆H+ plates thickness.

Number of plates = 16
Spacing between each plate = 600 mm.
Space for disengagement of vapor and liquid on top = 600 mm.
Space for disengagement of vapor and liquid in bottom = 600 mm
Total thickness of trays = 0.005×11 = 0.055 m
91
Height of column = [(number of plates - 1) × (space between each plate)] + (space for disengagement
on top and bottom) + plate thickness.
= [((16-1) x 0.6 + 0.60 + 0.60 + 0.055*16)]
= 8.7 m
So height of column = 8.7m
92
SPECIFICATION SHEET
Identification: Tray Distillation Column (D-601)
Function: To separate Maleic Anhydride from Phthalic Anhydride.
Operation: Continuous
Material Handled:
Feed = 5424.7 kg/hr
Overhead Product = 336 kg/hr
Bottom Product = 5056.7kg/hr
Design Data:
Operating temperature 473 K Diameter of column 0.68 m
Operating pressure 0.06 atm Plate Thickness 5 mm
Number of trays 16 Weir height 50 mm
Reflux ratio 1.2 Weir length 4.83 m
Tray spacing 0.5 m Active area 0.276 m2
Height of column 8m % flooding 33
Number of Holes 663.26
93
Chapter # 6 Mechanical Design
Chapter # 6
Mechanical Design
6 Mechanical Design of Heat Exchanger:

Product Gas Cooler (E-203):
Hot fluid (Product Gases) inlet temperature = T1 = 360oC
Cold fluid (Water) inlet temperature = t1 = 25oC
Hot fluid (Product Gases) outlet temperature = T2 = 250oC
Cold fluid (Water) outlet temperature = t2 = 49oC
Design Pressure
Should be 10% greater than maximum operating temperature.
Shell side
Operating pressure = 1.6 bar = 0.16 N/mm2
Design pressure = 1.76 bar = 0.176 N/mm2
Tube side
Operating pressure = 1 bar = 0.10 N/mm2
Design pressure = 1.1 bar = 0.11 N/mm2
Design Temperature:
Should be 10oC greater than maximum operating temperature.
Shell side
Max operating temperature = 360oC
Design temperature = 380oC
Tube side
Max operating temperature = 49oC
Design temperature = 60oC
Material of Construction:
1. Stain less Steel is mostly used as material of construction for many equipment’s in chemical
industries
2. Stain less steel is selected as material of construction for shell, tube sheet and heads because of
its higher operating temperatures, corrosion resistance and reasonable cost.
94
Maximum allowable stress:

Maximum allowable stress for carbon steel = 80.66 N/mm2 (from figure A.4 Appendix A)
Thickness of Shell:
p ∗ Ds
ts = +c
f ∗ j − 0.6 ∗ p
Let joint efficiency = 100%, j = 1

Shell ID = 15.25 in. = 387 mm
Design Pressure = P = 0.176 N/mm2
Allowable stress = f = 80.66 N/mm2
Let corrosion allowance = c = 3 mm
0.176 ∗ 387
ts = +3
79.23 ∗ 1 − 0.6 ∗ 0.176
ts = 3.86𝑚𝑚
Support:
Saddle type supports are common for horizontal shell and tube heat exchangers Two saddle supports
are installed to support structure of Heat Exchanger
Thickness of head:
Mostly used head is torispherical head
Diameter of shell = 87 mm
Crown radius = Ri = 1 x Ds = 387 mm
Knuckle radius = ri = 6% of Ds = 0.06*387 = 23.22mm
Corrosion allowance = c = 3 mm
1 Ri
W= (3 + √ )
4 ri
Stress Corrosion factor = W= 1.77
Thickness of head:
p ∗ Ri ∗ W
Th = +C
2f ∗ j − 0.2 ∗ P
95
0.176 ∗ 387 ∗ 1.77

Th = +3
2 ∗ 80.66 ∗ 1 − 0.2 ∗ 0.176
𝑇ℎ = 3.74𝑚𝑚
Depth of Head:
1
Ds Ds 2
hi = Ri − [(Ri − ) (Ri + ) + 2ri]
2 2
1
387 387 2
hi = 387 − [(387 − ) (387 + ) + 2 ∗ 23.22]
2 2
hi = 51.77𝑚𝑚
Effective Exchanger Length:

Length of tube = L = 16 ft = 4.88 m
Effective length = Le = L + 2hi = 4.88 + (2*0.05177) = 4.98 m = 4980 mm
Tube Sheet Thickness:

Tube sheet factor = F = 1 (fixed tube sheet)
Diameter over which pressure is acting = Gp = Shell ID = Ds = 387 mm (for fixed tube sheet)
Tube pitch = Pt = 1 in. = 25.41 mm triangular pitch
Outside diameter of tube = 0.75 in. = 19.05 mm
Mean Efficiency = k
For Square Pitch

0.907
k= 1− 1
𝑃𝑡 2
(𝐷𝑜)
0.907
k=1− 1
25.41 2
( )
19.05
k = 0.49
Tube Sheet Thickness:
𝑃
𝐹 ∗ 𝐺𝑝
Ts = √𝑘 ∗ 𝑓
3
96
1 ∗ 387 0.176
Ts = √0.49 ∗ 80.66
3
Ts = 6.89mm
97
Mechanical Design Specification Sheet
Item Heat Exchanger
Type Shell & Tube Heat Exchanger
Mechanical Design
Design Temperature Shell side: 380⁰C
Tube Side: 60⁰C
Design Pressure Shell side: 1.76 bar

Tube side: 1.01 bar
Material of Construction Carbon Steel
Maximum allowable stress 80.66 N/mm2
Shell Thickness 3.86 mm
Tori spherical Head Thickness 3.74 mm
Effective exchanger length 4980 mm
Tube sheet thickness 6.89 mm
Support Saddle type support
98
Chapter #7 Pumps And Compressor
Chapter # 7
Pumps And Compressor Calculation
7 Pumps:
Pump is a device that imparts momentum and mechanical energy to the process fluid. Pumps are used
to transfer fluid from one location to other. A pump is a device used to raise, compress, or transfer
fluids. The motors that power most pumps can be the focus of many best practices. It is common to
model the operation of pumps via pump and system curves. Pump curves offer the horsepower, head,
and flow rate figures for a specific pump at a constant rpm. System curves describe the capacity and
head required by a pump system.
7.1 Pump Types

Various types of pumps are used in the chemical industry, including centrifugal, reciprocating, and
helical rotor pumps.
7.1.1 Centrifugal Pumps

Centrifugal pumps operate by applying a centrifugal force to fluids, many times with the assistance of
impellers. These pumps are typically used in moderate to high flow applications with low-pressure
head and are very common in chemical process industries. There are three types of centrifugal
pumps—radial, mixed, and axial flow pumps. In the radial pumps, pressure is developed completely
through a centrifugal force, while in axial pumps pressure is developed by lift generated by the
impeller. Mixed flow pumps develop flow through a centrifugal force and the impeller.
7.1.2 Reciprocating Pumps

Reciprocating pumps compress liquid in small chambers via pistons or diaphragms. These pumps are
typically used in low-flow and high-head applications. Piston pumps may have single or multiple
stages and are generally not suitable for transferring toxic or explosive material. Diaphragm pumps are
more commonly used for toxic or explosive materials.
7.1.3 Helical Rotor Pumps

Helical rotor pumps use a rotor within a helical cavity to develop pressure. These pumps are useful for
submersible and waste applications.
7.2 Selection Criteria of Pumps

Many different factors can influence the final choice of the pump for an operation. The major factors
that govern the pump selection are following:
 The amount of liquid that must be pumped out.

 The properties of the fluid.
 Cost and mechanical efficiency of the pump.
7.3 Pump Sizing Calculation Steps

 Select the pump.
 Estimate z1 and z2.
 Estimate Frictional pressure losses ED and ES.
99
 Calculate Pump Work.

 Calculate Pump shaft horsepower & estimate its Efficiency.
 Calculate electric-motor horsepower & estimate its Efficiency.
 Select a standard electric-motor horsepower.
 Calculate NPSH.[19]
7.4 O- Xylene Pump (P-301):

This pump is used for to pump O-Xylene to Vaporizer
O-Xylene = 5331.8 kg/hr

Pressure = 2.5atm
O-Xylene = 5331.8 kg/hr

Pressure = 1atm
Figure 7.1: O-Xylene Pump
Pump Selection
Pump type is selected from figure B.1 Appendix B
Capacity = 23.51 gpm
Head = 36ft
Hence, the Pump Selected Centrifugal Pump.
Define the inlet and outlet pressures

The inlet pressure is = P1 = 1 bar
The outlet pressure is = P2 = 2.53 bar
Locate the process equipment

Locate the process equipment according to the rule of thumb listed below. As we need to pump the
liquid in to the Heat Exchanger.
Estimation of z1 & z2:

(From figure B.2 Appendix B)
Z1 with respect to pump = 0
Z2 = 3 ft
100
Estimation Frictional pressure losses ED and ES

So, ES & ED is equal to 0.35, (From figure B.3 Appendix B)
Calculate the pump work

g P1 − P2
W= (z1 − z2 ) + − (ES − ED )
gC ʃ
9.8 (1 − 2.53) ∗ 105 (0.35 + 0.35) ∗ 105

𝑊= (0 − 3) + −
32 880 880
𝑁𝑚
𝑊 = − 311.05
𝐾𝑔
Calculate the pump shaft horsepower

Efficiency of Pump is selected from the figure B.4 Appendix B
𝑚𝑊
𝑃=
ɳ
5339.15 ∗ 311.05
𝑃=
0.45
P = 3690634.04 J/hr
P = 1.37 hp
Calculate Electric-Motor Horsepower & Estimate its Efficiency

On the basis of horsepower the selected motor is Squirrel Cage Induction Motor having power range
of 1 to 5,000 hp from B.5 Appendix B.
Efficiency of motor is selected to be = 0.86
𝑃𝑃
The power of motor is calculated as = PE = 𝑃𝐸 = ɳ
1.37
𝑃𝐸 =
0.86
PE = 1.59 hp
Select a Standard Electric Motor Horsepower

Figure B.6 Appendix B shows the most common standard size motor available in market
Net Positive Suction Head (NPSH)

1 𝑃𝑎 − 𝑃𝑣
𝑁𝑃𝑆𝐻 = ( − ℎ𝑓𝑠 ) − 𝑍𝑎
𝑔 ʃ
Absolute pressure at the surface of reservoir = Pa = 1 bar = 1*105 Pa
101
Vapor pressure of O-Xylene = Pv =0.007*105pa

Friction losses in suction line = hfs = 0
Za = 0
1 1 ∗ 105 − 0.007 ∗ 105

𝑁𝑃𝑆𝐻 = ( − 0) − 0
9.8 880
NPSH = 12 m
102
Specification Sheet
Identification
Item Pump
Item No. P-301
Type Centrifugal
Function
To increase pressure from 1bar to 3.03 bar
Feed Flow Rate 5339.15 kg/hr
Inlet Pressure 1 bar
Outlet Pressure 2.53 bar
Power of pump 1.37 hp
Power of electric motor 1.59 hp
NPSH 12 m
Specification Sheet
Identification
Item Pump
Item No. P-102
Type Centrifugal
Function
To increase pressure from 1bar to 3 bar
Feed Flow Rate 803.15 kg/hr
Inlet Pressure 1.82 bar
Power of pump 0.175 hp
Power of electric motor 0.25 hp
NPSH 9.7 m
103
7.5 Compressors
A device that pressurizes fluids generally. Compressors are similar to pumps: both increase the
pressure on a fluid and both can transport the fluid through a pipe. Compression of gases and vapors
is an important operation in chemical and petrochemical plants. It is necessary to be able to specify the
proper type of equipment by its characteristic performance. The compression step is conveniently
identified for the process design engineer by the principal operation of the equipment:
 Reciprocating.
 Centrifugal.
 Rotary displacement.
 Axial flow.
Compression may be from below atmospheric as in a vacuum pump or above atmospheric as for the
majority of process applications. A gas compressor is a mechanical device that increases the pressure
of a gas by reducing its volume. An air compressor is a device specifically for compressing air to
power other tools.
7.6 Positive Displacement Compressor

 Reciprocating compressors
 Ionic liquid piston compressor.
 Rotary screw compressors.
 Rotary Vane compressors.
 Rolling piston.
 Scroll compressors.
 Diaphragm compressors.
7.7 Dynamic compressor

 Air bubble compressor.
 Centrifugal compressors.
 Continuous Blade Compressor.
 Diagonal or mixed-flow compressors.
 Axial-flow compressors.
7.8 Compressor Sizing Calculation Steps

 Select the compressor type.
 Calculate the reduce temperature and pressure and then calculate compressibility at the inlet of
compressor.
 Calculation of specific volume.
 Calculation of volumetric flow rate.
 Calculate hydraulic efficiency.
 Calculate the work of compressor.
 Calculate the discharge temperature.
 Calculate the reduce temperature and pressure at outlet conditions.
 Calculate the overall compressibility factor.
104
 Calculate the shaft work.

 Power calculation.
 Standard compressor size selection.[19]
7.9 Air Compressor (C-101) :
Air = 42418 kg/hr
Pressure = 2.5atm
Air = 42418 kg/hr

Pressure = 1atm
Figure 7.2: Air Compressor (C-101)
Flow rate = 42418 kg/hr. = 35675.33 m3/hr.

P1 = 1.01 bar
P2 = 2.53 bar
T1 = 25℃
Selection of the Compressor

Hence the compressor selected is centrifugal compressor.
The advantages of centrifugal compressor are following:
 Can handle wide range of flow rate

 Compatible for corrosive fluids
 They can deal liquid with large amounts of solids.
 Maintenance costs are lower than from other types of compressors.
Calculation of critical temperature and critical pressure of gaseous mixture
Components k Pc(bar) Tc(K)
Air 1.40 37.7 132.8
105
Calculate the reduce temperature and pressure and then calculate compressibility
Reduced temperature:
TR = T1/Tc = 2.24
Reduced Pressure:
PR = P1/Pc = 0.026
Compressibility:
Z = 0.99 (From fig B.8 Appendix B)
Volumetric flow rate = 210004.15 ft3/min
Calculate hydraulic efficiency

From graph the Polytrophic efficiency = ηp= 0.74 (From fig B.9 Appendix B)
n  1 (k  1) / k

n p
𝒏−𝟏
= 0.38
𝒏
Calculate the work done

Let assume that initially we have only one stage N=1
 n 1

'
ZR T  p2 n'
  
WPN  1
   1

(n  1) / n  p1 
 
WP1 = 1.04*106 J/kmol.
Calculate the discharge temperature
R'
WCN  (TD  T1' )
(k  1) / k
TD = 302.8 K
Critical Properties of Gases at outlet

Calculate the reduce temperature and pressure and then calculate compressibility.
Reduced temperature:
TR = T1/Tc = 2.28
Reduced Pressure:
106
PR = P1/Pc = 0.081
Compressibility:
ZD = 0.96
Z = (Z1 + ZD ) / 2
Z = 0.97
Shaft Work Calculation
WPN
WCN 
 p s B G
1.04∗10^6
WCN =
0.74∗0.98∗0.95∗0.95
WCN = 1.36*106 J/kmol
Shaft Work Power Calculation

Gas flow rate = 1470 kmol/hr
PCP = 1.36*106*(1470/3600)
PCP = 557 kW
Motor Power Calculation

𝑃𝑐𝑝
PE = ,
ŋ𝐸
ŋE = 0.94
PE = 798 hp
We select standard motor of 800 hp.
107
Specification Sheet
Identification
Item Compressor
Item No. C-101
Type Centrifugal
Function
To increase the pressure of air
Feed Flow Rate 1470 kg/hr
Inlet Pressure 1.01 bar
Power 800 hp
108
Chapter #8 Cost Estimation
Chapter # 8
Cost Estimation
8 Cost of Packed Bed Tubular Reactor:

Material of construction = Stainless Steel
Length = 5.83m
Diameter = 1.45m
Material Factor = 2
Pressure Factor = 1
Purchase Cost in 2004 = bare cost*material factor*pressure factor
= 18000*2*1
= 36000 $
Cost index in 2004 = 520
Cost index in 2017 = 676.6
Index in 2017
Cost in 2017 = cost in 2004*
Index in 2004
= 46840 $
8.1 Cost of Flash Separator :

Material of construction = Stainless Steel
Length = 4.31m
Diameter = 1.81m
Material Factor = 2
Pressure Factor = 1
= 8000*2*1
= 16000 $
Index in 2017
Index in 2004
109
= 20818 $
8.2 Cost of Air-Preheater :

Type: Shell and tube heat exchanger
Material: Carbon steel
Area = 48.50 m2
Ce = a + bSn [14]
Where
Ce = Purchased Equipment Cost
S = Size parameter
N = Exponent for that type of equipment
a , b are constants
a = 24000
b = 46
n = 1.2
S = 48.50 m2
Purchased Equipment Cost in 2007 = 24000 + (46)(48.50)1.2
Purchased Equipment Cost in 2007 = 28848 $
Index in 2017
Index in 2007
= 33449 $
8.3 Cost of Gas Cooler (E-203):

Material: Stainless Steel
Area = 36.23 m2
Ce = a + bSn
S = 36.23 m2
110

Material Factor = fm =1.3
C = Ce*fm
C = 27416 *1.3
C = 35642 $
Index in 2017
Index in 2007
= 41327$
8.4 Cost of O-Xylene Vaporizer:

Area = 48.50 m2
Ce = a + bSn
S = 48.50 m2
Index in 2017
Index in 2007
= 33449 $
8.5 Cost of Dowtherm A Cooler:

Type: Double Pipe Heat Exchanger
Area = 12 m2
Ce = a + bSn
S = 12 m2
Purchased Equipment Cost in 2007 = 24000 + (46)(12)1.2
111

Index in 2017
Index in 2007
= 28900 $
8.6 Cost of Pump (P-301):

Type: Centrifugal
Ce = a + bSn
S = 1.68 L/s
a = 6900
b = 206
n = 0.9
Index in 2017
Index in 2007
= 13930 $
8.7 Cost of Pump (P-302):

Type: Centrifugal
Ce = a + bSn
S = 0.22 L/s
a = 6900
b = 206
n = 0.9
112

Index in 2017
Index in 2007
= 13400 $
8.8 Cost of Compressor:

Type: Centrifugal
Ce = a + bSn
S = 596 KW
a = 490,000
b = 16,800
n = 0.6
Purchased Equipment Cost in 2007 = 490,000 + (16800)(596)0.6
Purchased Equipment Cost in 2007 = 1267064.4 $
Index in 2017
Index in 2007
= 2441901 $
8.9 Cost of Distillation Column

Material = Carbon Steel
Height = 8m
Diameter = 0.68m
Material Factor = 1, Pressure Factor = 1
= 15000*1*1
= 15000$
𝐼𝑛𝑑𝑒𝑥 𝑖𝑛 2017
Cost in 2017 = cost in 2004*𝐼𝑛𝑑𝑒𝑥 𝑖𝑛 2004
= 19517$
113
8.10 Cost of Plates:

Plate type = Sieve tray
Diameter of Plate = 0.637
Cost of Plate = 250 $ [20]
Material Factor = 1, Number of Plates = 16
Total Cost = 4000 $ , Total cost of column = 23517 $
8.11 Total Cost of Equipment In 2018:

Table 8.1: Total Cost of Equipment
Equipment’s No Required Costs ($)

Cost of Packed Bed Tubular Reactor 1 46840
Cost of Flash Drum 1 20818
Cost of Air-Preheater 1 33449
Cost of O-Xylene Vaporizer 1 33449
Cost of Gas Cooler 2 82654
Cost of Pump 2 27300
Cost of Compressor 1 2441901
Cost of Distillation Column 1 23517
Cost of Dowtherm A Cooler 1 28900
Total 11 2738828
8.12 Direct Cost:

Table 8.2: Direct Cost
Items Range % Cost ($)

Purchased equipment --- 100% 2738828
Installation 25-55% of purchased equipment cost 40% 1095531.2
Instrument and Control 6-30% of purchased equipment cost 15% 410824.2
Piping 40-80% of purchased equipment cost 50% 1369414
Electricity 10-15% of purchased equipment cost 12% 3286593.6
Building 15% of purchased equipment cost 15% 410824.2
Land 4-8% of purchased equipment cost 4% 109553.12
Service facility 30-80% of purchased equipment cost 40% 1095531.2
Yard Improvement 10-20% of purchase equipment cost 10% 273882.8
Insulation cost 8-9% of purchased equipment cost 8% 219106.24
Total --- --- 11010088
114
8.13 Indirect Cost:

Table 8.3: Indirect Cost
Items Range % Cost ($)

Engg. & supervision 8% of total direct cost 8% 880807
Contractor fee 2-8% of direct plant cost 3% 330302.6
Construction Expenses 10% of Total direct plant cost 10% 110100.88
Contingences Direct plant cost 8% 880807.04
Total --- --- 2202017.52
Total capital investment = Fixed capital investment + working capital investment

Fixed capital investment = direct cost + indirect Cost
Fixed capital investment = 13212105.5 $
Working capital investment = 15% of fixed capital investment
Working capital investment = 1981815.8 $
Total capital investment = Fixed capital investment + working capital investment
Total capital investment = 15193920.5 $
8.14 Variable Cost:

Raw Material Cost
Cost of Air:
Flow rate of air = 34626 m3/hr
For 330 days of operating time = 2.78*108 m3/year
Price of air per m3 = 0.0006 $/ m3
Total price of air = 164542 $/year
Cost of O-Xylene:
Flow rate of O-xylene = 5331.8 kg/hr
For 330 days of operating time = 42227.8ton/year
Price of o-xylene per ton = 950 $/ ton

Total price of o-xylene = 40116463.2 $/year
Catalyst Cost:
Price of catalyst = 1 $/kg
Weight of catalyst = 17303 kg
115
Price of catalyst = 17303 $
Steam Cost:
Flow rate of Steam = 29.92 ton/hr
For 330 days of operating time = 236966.4 ton/year
Price of steam per ton = 12 $/ ton
Total price of steam = 2843596.8 $/year
Miscellaneous Material
It is 10% of maintenance cost
Maintenance cost = 7% of FCI
Maintenance cost = 924847.3 $
Miscellaneous Material = 92484 $
8.15 Utilities:
Cooling water
Flow rate of Cooling water = 153.68 ton/hr
For 330 days of operating time = 1217193.12 ton/year
Price of cooling water per ton = 0.01 $/ ton
Total price of cooling water = 12171.93 $/year
Variable cost = raw material cost + miscellaneous cost + utilities cost

Variable cost = 7146560.93 $/year
8.16 Fixed Cost:

Table 8.4: Fixed Cost
Maintenance 7 % of FCI 924847.3

Operating Cost of Labor 10% of TPC 0.1*TPC
Laboratory Cost 1.5% of TPC 0.015*TPC
Supervision Cost 2% of TPC 0.02*TPC
Plant Overheads 5% of TPC 0.05*TPC
Capital Charges 10% of FCI 1321210
Insurance 1% of FCI 132121
Local Taxes 2% of FCI 264242.1
Royalties 1% of FCI 132121
Fixed Cost - 2774541.4 + 0.185*TPC
116
Direct production cost = variable cost + fixed cost

Direct production cost = 9921101.4 + 0.185*TPC
8.17 Overhead Charges:

30% of direct production cost
Overhead charges = 0.30*(9921101.4 + 0.185*TPC)
= 2976330.42 + 0.0555*TPC
Put all the values in equation below
Total production cost = variable cost + fixed cost + overhead charges
TPC = 7146560 + 2774541.4 + 0.185*TPC + 2976330.42 + 0.0555*TPC
TPC = 12897431.82+ 0.2405*TPC
TPC-0.2405TPC = 12897431.82
0.7595*TPC=12897431.82
TPC = 16981477.05 $/year
Total production rate = 39940560 kg/year
Production cost ($/kg) = Total production cost / Total production rate
= 0.43 $/kg
= 430 $/ton
Below this we cannot sale our product.
And the price of phthalic anhydride in the market is 850$/ton.
Our goal is to get the maximum profit we sale the product with market rate after comparing with the
market.
Selling Price:
Selling price of product = 700 $/ton
8.18 Profitability Analysis:

Production Cost = 0.43 $/kg
Selling Price = 0.700 $/kg
Profit = Selling price - production cost = 0.270 $/kg
Total Production per year = 39940560 kg/year
Profit per year = 10783951.2 $/year
117
8.19 Total Income:

Selling Price = 700 $/ton
Total Production per year = 39940 ton/year
Total Income = 27958000 $/year
Gross Profit
Gross Profit = Total Income - Total Production Cost = 10976522.9 $/year
Net Profit
Let the tax rate is 30%
Taxes = 0.3*Gross Profit = 3292956.8 $/year
Depreciation
Assume that the Fixed Capital Investment depreciate by straight line method for 20 years.
Assuming 5 % Salvage value at the end of plant life.
Depreciation = D = (V-VS)/N
V = F.C.I = 13212105.5$
VS = 0.05*F.C.I = 660605.27$
N = No of Years = 20 Years
Depreciation = D = (V-VS)/N = 627575.0 $
Net Profit = Gross profit - Taxes – Depreciation = 6873213.61 $/year
Rate of return
Rate of return = (Net profit/Total capital investment)*100
Rate of return = 29.96 %
Payback Period
Payback Period = 1/rate of return
Payback period = 3.39 year
118
Chapter #9 Instrumentation And Control
Chapter # 9
Instrumentation And Control
9 Introduction
Control in process industries refers to the regulation of all aspects of the process. Precise control of
level, temperature, pressure and flow is important in many process applications. This module
introduces you to control in process industries, explains why control is important, and identifies
different ways in which precise control is ensured. The objective of an automatic process control is to
use the manipulated variable to maintain the controlled variable at its set point in spite of disturbances.
Instruments are provided to monitor the key process variables during plant operations. Instruments
monitoring critical process variables will be fitted with automatic alarms to alert, the operations to
critical and hazardous situations.
9.1 Importance of Process Control:

Refining, combining, handling, and otherwise manipulating fluids to profitably produce end products
can be a precise, demanding, and potentially hazardous process. Small changes in a process can have
a large impact on the end result. Variations in proportions, temperature, flow, turbulence, and many
other factors must be carefully and consistently controlled to produce the desired end product with a
minimum of raw materials and energy. Process control technology is the tool that enables
manufacturers to keep their operations running within specified limits and to set more precise limits to
maximize profitability, ensure quality and safety.
Process:
Process as used in the terms process control and process industry, refers to the methods of changing
or refining raw materials to create end products. The raw materials, which either pass through or remain
in a liquid, gaseous, or slurry (a mix of solids and liquids) state during the process, are transferred,
measured, mixed, heated or cooled, filtered, stored, or handled in some other way to produce the end
product. Process industries include the chemical industry, the oil and gas industry, the food and
beverage industry, the pharmaceutical industry, the water treatment industry, and the power industry.
Process Control:
Process control refers to the methods that are used to control process variables when manufacturing a
product. For example, factors such as the proportion of one ingredient to another, the temperature of
the materials, how well the ingredients are mixed, and the pressure under which the materials are held
can significantly impact the quality of an end product. Manufacturers control the production process
for three reasons:
 Reduce variability.
 Increase efficiency.
 Ensure safety.
Safe plant operation:
 To keep the process variables within known safe operating limits.
119
 To detect dangerous situations as they develop and to provide alarms and automatic shutdown
systems.
 To provide interlocks and alarms to prevent dangerous operating procedures.
9.2 Process Control Terms:

Process Variable: A process variable is a condition of the process fluid that can change the
manufacturing process in some way. In the example of you sitting by the fire, the process variable was
temperature. Common process variables include:
 Pressure
 Flow
 Level
 Temperature
 Density
 Ph (acidity or alkalinity)
 Mass
Set point: The set point is a value for a process variable that is desired to be maintained.
Measured variables: The measured variable is the condition of the process fluid that must be kept at
the designated set point.
Manipulated variable: The variable that can be variate in order to manage the control variable at its
desired value.[21][22]
9.3 Hardware elements of control system:

The measuring instruments or sensors: These are the instruments which are used to measure
disturbance, controlled variables.
Transducers: A transducer is device that converts one form of energy to another. Usually a transducer
converts a signal in one form of energy to a signal in another.
Transmission line: It is used to carry out the measurement signal from the measuring device to
controller.
Controller: This receives the formation from the measuring devices that decides either the information
is correct or not.
The final controller element: The Final control element is a device controlled by a controller to
change the operating conditions of a process. Final control elements require energy to operate against
the process. It is the hardware element that implements the decision taken by controller.[23]
9.4 Classification of control systems:

For instrumentation and control of different sections and equipment’s of plants, following control
loops are most often used.
 Feed-back control loop
120
 Feed forward control loop

 Ratio control loop
 Split range control loop
 Cascade control loop
Here is given a short outline of these control schemes, so that to justify out selection of a control loop
for specified equipment.
Feed Back Control Loop: A method of control in which a measured value of a process variable is
compared with the desired value of the process variable and any necessary action is taken. Feedback
control is considered as the basic control loops system. Its disadvantage lies in its operational
procedure. For example, if a certain quantity is entering in a process, then a monitor will be there at
the process to note its value. Any changes from the set point will be sent to the final control element
through the controller so that to adjust the incoming quantity according to desired value (set point).
But in fact changes have already occurred and only corrective action can be taken while using feedback
control system.
Feed Forward Control Loop: A method of control in which the value of disturbance is measured
than action is taken to prevent the disturbance by changing the value of a process variable. This is a
control method designed to prevent errors from occurring in a process variable. This control system is
better than feedback control because it anticipates the change in the process variable before it enters
the process and takes the preventive action. While in feedback control system action is taken after the
change has occurred.
Ratio Control: A control loop in which, the controlling element maintains a predetermined ratio of
one variable to another. Usually this control loop is attached to such a system where two different
systems enter a vessel for reaction that may be of any kind. To maintain the stoichiometric quantities
of different streams, this loop is used so that to ensure proper process going on in the process vessel.
Split Range Loop: In this loop controller is preset with different values corresponding to different
actions to be taken at different conditions. The advantage of this loop is to maintain the proper
conditions and avoid abnormalities at very differential levels.
Cascade Control Loop: This is a control in which two or more control loops are arranged so that the
output of one controlling element adjusts the set point of another controlling element. This control
loop is used where proper and quick control is difficult by simple feed forward or feed backward
control. Normally first loop is a feedback control loop.[24] [25]
9.5 Control Scheme of Reactor:

Control Objectives
 Temperature inside the Reactor

 Temperature of coolant
Manipulated variables
121
The manipulated variable is coolant flow rate Fc
Loads or Disturbances:
Following are typical disturbances
 Flow rate of feed

 Temperature of feed.
 Coolant Flow Rate
 Coolant temperature
Description:
We have to maintain the temperature inside the reactor constant at 360°C. The temperature in the
tubular reactor vary along the length of the reactor. The highest temperature is called the hot spot. The
location of the hot spot moves along the length of the reactor depending on the feed conditions
(temperature, concentration, flow rate) and the catalyst activity. The value of the hotpot temperature
also depends on the factors listed above and the temperature and flow rate of the coolant. The cascade
control loop is used to control the level and temperature inside the reactor.
The control of such systems is a real challenge .The primary control objective is to keep the hot-spot
temperature below an upper limit. Therefore, we need a control system that can identify the location
of the hot spot and provide the proper control action. This can be achieved through:
 Placement of several thermocouples along the length of the reactor

 If T goes up, increase the flow rate of the coolant to remove heat. Decrease the coolant rate,
when T decreases
 We can have two control loops using two different measurements, T and Tc but sharing a
common manipulated variable, Fc
 The loop that measures T (controlled variable) is the dominant or primary, or master control
loop and uses a set point supplied by the operator.
 The loop that measures Tc uses the output of the primary controller as its set point and is called
the secondary or slave loop.
122
Feed out
Set point Set point
T
TT
T
TT
T AC Sc
TT
T
TT TT
FCE Tc
Inlet Feed Coolant
Figure 9.1: Control Loop on Reactor
123
Chapter #10 HAZOP Study
Chapter # 10
HAZOP Study
10 HAZOP:
A Hazard and Operability (HAZOP) study is a structured and systematic examination of a planned or
existing process or operation in order to identify and evaluate problems that may represent risks to
personnel or equipment, or prevent efficient operation.
The HAZOP technique was initially developed to analyze chemical process systems, but has later been
extended to other types of systems and also to complex operations and to software systems. A HAZOP
is a qualitative technique based on guide-words and is carried out by a multi-disciplinary team
(HAZOP team) during a set of meetings
10.1 Perform a HAZOP

The HAZOP study should preferably be carried out as early in the design phase as possible to have
influence on the design. On the other hand; to carry out a HAZOP we need a rather complete design.
As a compromise, the HAZOP is usually carried out as a final check when the detailed design has been
completed. A HAZOP study may also be conducted on an existing facility to identify modifications
that should be implemented to reduce risk and operability problems.
10.2 Why HAZOP Carry out?

To identify (areas of the design that may possess a significant hazard potential).
To identify and study features of the design that influence the probability of a hazardous incident
occurring.
 To familiarize the study team with the design information available.

 To ensure that a systematic study is made of the areas of significant hazard potential.
 To identify pertinent design information not currently available to the team.
 To provide a mechanism for feedback to the client of the study teams detailed comments.
10.3 Guide words

These are simple words which are used to qualify or quantify the intention in order to guide and
stimulate the brainstorming process and so discover deviations. The guide words shown in Table are
the ones most often used in a HAZOP; some organizations have made this list specific to their
operations, to guide the team more quickly to the areas where they have previously found problems.
Each guide word is applied to the process variables at the point in the plant (study node) which is being
examined.
124
Table 10.1: HAZOP Terminology
Term Definition
Sections of equipment with definite boundaries (e.g., a line between two
vessels) within which process parameters are investigated for
Process Sections or deviations. The locations on P&IDs at which the
(Study Nodes) process parameters are investigated for deviations (e.g. Distillation
Column)
Discrete actions in a batch process or a procedure analyzed by a

Operating Steps HAZOP analysis team. May be manual, automatic, or software
implemented actions. The deviations applied to each step are somewhat
different than the ones used for a continuous process
Definition of how the plant is expected to operate in the absence of

deviation. Takes a number of forms and can be either descriptive or
Intention diagrammatic (e.g., process description, flow
sheets, line diagrams, P&IDs)
Simple words that are used to qualify the design intention and to
Guide Words guide and stimulate the brainstorming process for identifying
process hazards
Physical or chemical property associated with the process.
Process Parameter Includes general items such as reaction, mixing, concentration, pH,
and specific items such as temperature, pressure, phase, and flow
Departures from the design intention that are discovered by
Deviations systematically applying the guide words to process parameters (flow,
pressure, etc.) resulting in a list for the team to review (no flow, high
pressure, etc.) for each process section. Teams often
supplement their list of deviations with ad hoc items
Reasons why deviations might occur. Once a deviation has been
Causes shown to have a credible cause, it can be treated as a meaningful
deviation. These causes can be hardware failures, human errors,
unanticipated process states (e.g. change of composition), external
disruptions (e.g. loss of power), etc.
Results of deviations (e.g. release of toxic materials). Normally, the
Consequences team assumes active protection systems fail to work. Minor
consequences, unrelated to the study objective, are not
considered
Engineered systems or administrative controls designed to
Safeguards prevent the causes or mitigate the consequences of deviations
(e.g. process alarms, interlocks, procedures)
125
Actions (or Suggestions for design changes, procedural changes, or areas for
Recommendations) further study (e.g. adding a redundant pressure alarm or reversing the
sequence of two operating steps)
10.4 HAZOP Study on Distillation Column

Table 10.2: HAZOP Study on Distillation Column
Study node Process Deviation Possible causes Possible Action

paramete (guide consequences required
word)
Stream No. 1. Flow NO Pipe broken or Loss of feed into Schedule
plugging (D-601) achieve inspection.
into desired output.
Level decrease in
(D-601).
Off specification
product.
Stream No. 1. Flow LOW Pipe partial Level decrease in Install check
plugged or leakage. (D-601) valves.
Off specification
product.
Back flow of
material.
Stream No. 1. Flow HIGH High pressure from Flooding in (D- Install check
source. 601) valves
Distillation Level HIGH Output pipeline Over-pressure of Install high
column (D- blockage reflux drum. level alarm.
601) Condensed liquid Scheduling
back flow to (D- inspection.
601)
Distillation Level LOW Pipe partial Level decrease in Scheduling
column (D- clogged or leakage. the vessel. inspection.
601) Valve closed. -Install
Backflow of valve.
material.
Distillation Temperat HIGH Low incoming Off specification Install
column (D- ure flow from (E-207) product. temperature
601) (E-207) cause sensors.
overheating.
126
Distillation Temperat LOW High incoming Low level inside Scheduling

column (D- ure flow from (E-206) (E-207). inspection.
601) Off specification Install
product. sensors
Distillation Pressure HIGH -Water failure in (E-206) vent will Pressure

column (DC- (E-206) act as relief valve. indicator on
601) (DC-601)
Condenser Flow NO Condenser line Reflux drum low Compressor
(E-206) heavy leakage level trip
Reflux drum indication
depressurization Level
transmitter
with low
level alarm
Condenser Flow LESS (E-206) low low level (v-101) Level
(E-206) performance indicator on
(E-206) line miner reflux drum
leakage
Condenser Flow MORE Depressurization of Level increased (V- Level
(E-206) downstream 101) controller
section (LLC)
Condenser Temperat LESS Due to leakage Adiabatic -Install
(E-206) ure lower system depressurization temperature
pressure may cause sub - indicator at
zero temperature (E-206)
outlet
temperature
Condenser Temperat MORE Cooling medium Level low of (v- Install
(E-206) ure fail of (E-206) 101) temperature
indicator at
(E-206)
outlet
Condenser Pressure LESS Condenser line Level low Compressor
(E-206) leakage Depressurization of trip
Compressor trip reflux drum indication
Level
transmitter
with low
level alarm
Condenser Pressure MORE Valve close Line over pressure Compressor
(E-206) failure
127
Stream Flow LESS Leakage in Level low in Level

No.2 upstream system (E-206) controller
Reboiler (E-207)
low level
Stream Flow MORE (E-207) high level Level high in Level
No.2 Leakage in (E-206) controller
(E-206)
128
Chapter #11 Environmental Study
Chapter # 11
Environmental Study
11 Introduction
The production methods of phthalic anhydride and the chemical itself both directly impact the
environment. The plants that produce Phthalic anhydride create by-products which, in turn, affect the
environment; as well, the chemical can be released into the ecosystem at the end of its lifecycle as a
consumer product, thus also affecting the environment.
11.1 Environmental Release:

Phthalic anhydride is released to the environment from chemical Plants, mainly those that manufacture
the chemical or use it in the production of plastics and resins. The major sources of these releases are
process off-gases and industrial effluents; however, the use of catalytic oxidation now reduces the
release of pollutants in off-gases. Phthalic anhydride has been detected in arctic air at the concentration
of10 mg/mᶟ (however, the EPA review notes that the presence of the anhydride could have resulted
from the hydrolysis of phthalate esters followed by dehydration in the GC injection port), and has been
identified but not quantified in U.S. drinking water and in the volatile flavor components of baked
Idaho potatoes (U.S. EPA 1986). In 1992 environmental releases of the chemical, as reported to the
Toxic Chemical release inventory by certain types of US industries, totaled about 756 thousand
pounds, including 750 thousand to the atmosphere, 1 thousand pounds to land, and 5 thousand pounds
to surface water.
11.2 Transport:
No information was found for the transport of atmospheric phthalic anhydride. However the water
solubility of the chemical suggests that wet deposition may occur prior to its conversion to phthalic
acid, a less soluble chemical. Because vapor phase particle adsorption usually occurs with chemicals
having a vapor pressure of 10-7 mm Hg adsorption is not a likely vapor phase removal mechanism for
phthalic anhydride. No information was found for the transport of phthalic anhydride in the aquatic
environment. However, the rapid hydrolysis of phthalic anhydride to phthalic acid that occurs in
aqueous media would preclude any significant transport of the chemical in the aquatic environment.
Its low vapor pressure and henry’s Law constant (1.6*10¬¯⁸ atm mᶟ/mol) indicate that the chemical
will slowly volatilize from water. The chemical is soluble in water (6,200 mg/L at 25⁰C) and has a low
KOC (36, estimated) and therefore has a low potential for sedimentation or adsorption to particles,
respectively, No information was found for the transport of phthalic anhydride in soil. In moist soil,
the chemical will hydrolyze to phthalic acid and significant leaching is not expected to occur, other
than in the case of a large spill. Significant volatilization from soil is also unlikely based on the
chemical’s low vapor pressure (0.00052 mm Hg).
11.3 Transformation /Persistence:

Air: The rate constant for the reaction of phthalic anhydride with OH radicals is estimated to be
5.0*10¯¹³ cmᶟ molecule¯¹ s¯¹. Assuming the concentration of OH in the atmosphere to be 106
molecules per cubic centimeter, the estimated half-life for this reaction is 21 days.
129
Soil: No information was found regarding the fate and transport of phthalic anhydride in the soil. Based
on its rapid hydride is also expected to undergo biodegradation in soil, as it does in water Under aerobic
soil conditions, phthalic anhydride in regulated and unregulated waste streams and in contaminated
soil, groundwater, or surface water resulting from hazardous waste mismanagement incidents, the U.S.
EPA (1988b) (under section 4 of the Toxic Substances Control Act) required testing of phthalic
anhydride for soil adsorption. The soil adsorption isotherm test was required, in accordance with
796.2750 (U.S EPA 1988). Optional biodegradation testing was also recommended.
Water: Hydrolysis and biodegradation are the two processes that may significantly degrade phthalic
anhydride in water. The hydrolytic half-life for the chemical is about 1.5 minutes (calculated based on
in the rate constant for the forward reaction in aqueous solution, 7.9*10¯³ s¯¹ at 25⁰C
Biodegradation values, reported in (U.S. EPA 1988) for various wastewater treatment conditions are
as follows:
 44-78% mineralization in 5 days based on theoretical biological oxygen demand (incubation

of 1-4 mg/L of phthalic anhydride with sewage as microbial inoculum).
 ̴21% degradation in 5 days using the standard dilution method (incubation of 2 mg/L with
sewage).
 ̴18% degradation using the seawater dilution method.
 33% degradation in 24 hours using chemical oxygen demand removal (incubation of 9 mg/L
phthalic anhydride with activated sludge).
 >30% degradation in 2 weeks using the Japanese MITI test (100 mg/L phthalic anhydride
incubated with activated sludge, pH 7 at 20⁰C).
In addition phthalic acid was 50% degraded in 1.5 weeks in the river die-away test (using phthalic acid
in a model aquatic ecosystem. [27]
11.4 Health effects:

Absorption: Oral toxicity data for animals, and other human and data provide indirect evidence that
the phthalic anhydride or its hydrolysis product, phthalic acid, is absorbed from the gastrointestinal
tract and lungs. No information was found concerning dermal absorption was found. Phthalic
anhydride is a skin irritant, and skin damage is known to result in increased absorption of chemicals.
Distribution: Limited information was found on the distribution of phthalic anhydride or its hydrolysis
product, phthalic acid. One study, using an exposure route of questionable relevance to human
exposure, indicates that fetuses from CD-1 fetal mice injected with 80 mg/kg 14⁰C-phthalic anhydride
on days 11, 12, and 13 of gestation exhibited covalently bound radioactivity in all tissues.
Metabolism: Phthalic anhydride is expected to undergo hydrolysis to phthalic acid in the aqueous
media of the body. No information on the metabolism of phthalic anhydride was found in the secondary
sources searched.
Excretion: Human exposed to phthalic anhydride in workplace air excreted phthalic acid in the urine
as free acid.
130
11.5 Acute Effects:

Acute exposure to phthalic anhydride produces irritation of the eyes, skin and respiratory tract and
lung sensitization in humans. Phthalic anhydride causes sensitization in animals as well.
Humans: The acute toxicity of phthalic anhydride is characterized by irritation of the eyes and skin,
allergic rhinitis, and asthma.
Animals: LD50 values for phthalic anhydride administered orally to animals are 800 to 1600 mg/kg
for rats and 2210 mg/kg for mice guinea pigs were sensitized to 0.1% phthalic
11.6 Sub chronic/Chronic Effects:

Workers exposed to moderate to high concentration of atmospheric phthalic anhydride have
experienced irritation of the eyes, skin, and respiratory tract, and have developed hypersensitivity,
bronchial asthma, and emphysema. Animals exposed chronically to high concentration of phthalic
anhydride in the diet exhibited lung, kidney, and adrenal gland toxicity. EPA has derived a chronic
reference dose of 2,mg/kg/day for phthalic anhydride
Humans: Workers exposed to atmospheric phthalic anhydride powder at levels of ̴24.9 to 77.3 ppm
(21 to 67 mg/kg/day) experienced higher incidences of irritation of the eye and respiratory tract than
workers exposed to 1 ppm. Irritation of the skin has also been reported in workers.
Case studies document the induction of hypersensitivity and bronchial asthma in humans exposed to
phthalic anhydride dust; specific antibody binding against the compound has been reported. Workers
currently or formerly employed in plants producing alkyd and/or polyunsaturated resins were
evaluated for respiratory ailments. Time-weighted-average breathing zone sample measured 3 to 13
mg/m3 in areas where bags containing flaked phthalic anhydride were cut open and emptied manually
into reactors several time a day during a 10- to 30 minute period. Of the 118 individuals examined 24
% had rhinitis, 11% had productive bronchitis, and 18% had work-associated asthma. The latent period
for the symptoms ranged from 1 to 16 years. Workers exposed to mixtures of phthalic anhydride and
phthalic acid developed conjunctivitis, bloody nasal discharge, atrophy of the nasal mucosa,
hoarseness, cough, occasional bloody sputum, bronchitis, and emphysema. Air concentrations of 30
mg/m³ (5 ppm) and 25 mg/m3 (4 ppm) were associated with conjunctivitis and mucous membrane
irritation, respectively.
11.7 Environmental effects:

Studies with phthalic acid, the hydrolysis product of phthalic anhydride, suggest that the chemical is
toxic to aquatic organisms only at moderate to high concentrations. Experimental studies suggest that
phthalic anhydride is of low acute toxicity to terrestrial animals.
Toxicity to Aquatic Organisms: The 96-hour LC50 for phthalic anhydride in the fathead minnow is
>50 mg/L (U.S. EPA 1986). Sea lampreys were not adversely affected by exposure to 5 mg/L for 24
hour (U.S. EPA 1986). No-effect concentrations (NOECs) reported for the hydrolysis product of
phthalic anhydride, phthalic acid, in various species are as follows: 640 mg/L for Daphnis (48 hour);
56 mg/L for fathead minnows (“acute”); 40 mg/L for Japanese frogs (24 hours); and 5 mg/L for
rainbow trout
131
Toxicity to Terrestrial Organisms: No information was found in the available literature for the
toxicity of phthalic anhydride to terrestrial organisms. The LD50 values of 800 to 1600 mg/kg for rats
and 2210 mg/kg for mice suggest that the chemical would not be acutely toxic to terrestrial animals
unless present in very high concentrations. Acute and chronic toxicity to terrestrial plants is expected
to be low.
Abiotic Effects: No information was found in the secondary sources searched on the abiotic effects of
phthalic anhydride.
11.8 Personal Protection:

Skin Protection: Wear impervious protective clothing, including boots, gloves, lab coat, apron or
coveralls, as appropriate, to prevent skin contact.
Eye Protection:
Use chemical safety goggles and/or full face shield where dusting or splashing of solution is possible.
Maintain eye wash fountain and quick-drench facilities in work area.
Respiratory Protection:
Airborne concentrations should be kept to the lowest levels possible. If vapor, mist or dust is generated
and the occupational exposure limit of the product is exceeded, use appropriate MOSH or MSHA
approved air purifying or air supplied respirator after determining the airborne concentration of the
contaminant. Air supplied respirators should always be worn when airborne concentration of the
contaminant or oxygen’s content is unknown. [28]
132
12 References:
[1] Nomenclature of Organic Chemistry : IUPAC Recommendations and Preferred Names
2013 (Blue Book). Cambridge: The Royal Society of Chemistry.
[2] Kirk‐Othmer. Encyclopedia of Chemical Technology. Voume 18.
[3] https://pubchem.ncbi.nlm.nih.gov/compound/phthalic_anhydride. Pub Chem. [Online]
[4] Noller, Carl R. (1965). Chemistry of Organic Compounds, 3rd ed.
[5] Peter M. Lorz, Friedrich K. Towae, Walter Enke, Rudolf Jäckh, Naresh Bhargava,
Wolfgang Hillesheim (2007). "Phthalic Acid and Derivatives". Ullmann's Encyclopedia of
Industrial Chemistry. Weinheim: Wiley-VCH.
[6] http://www.nimirchemicals.com/Product.html. Nimir Chemicals. [Online]
[7] https://ihsmarkit.com/products/phthalic-anhydride-chemical-economics-handbook.html.
https://ihsmarkit.com. [Online]
[8] http://www.nrlpak.com/. [Online]
[9]. Phthalic Anhydride Production by Osman Mohammed Albashir LAP Lambert Academic
Publishing, 2016 ISBN 3659910953
[10].Patent/US1251440 ASSIGNOB, T0 WESTERN ELECTRIC COM- .PANY
INCORPORATED, OF NEW YORK, N. Y., A CORPORATION OF NEW YORK.
[11] Elementary principles of chemical Process by Richard Felder 5th Edition
[12] Chemical Engineering By Coulson and Richardson volume 2
[13] Transport Processes and Separation Process Principles (Includes Unit Operations) (4th
Edition) By Christe John Geankoplis
[14] Chemical Engineering Design: Chemical Engineering Volume 6: R K Sinnot
[15] Perry's Chemical Engineers' Handbook, Eighth Edition

[16] Basic principles and calculations in chemical engineering by David M Himmelblau 8th
Edition
133
[17]. Process Heat Transfer by Donald Q kern
[18] Elements of chemical Reaction engineering by Scott Fogler 4th Edition

[19] H. Silla, Chemical Process Engineering: Design And Economics. 2003.
[20] M. S. Peters, K. D. Timmerhaus, and R. E. West, Plant Design and Economics for
Chemical Engineers. 1991.
[21] Morris, “Measurement and Instrumentation Principles,” Meas. Sci. Technol., vol. 12,
no. 10, pp. 1743–1744, 2001.
[22] T. R. Kuphaldt, Lessons In Industrial Instrumentation, vol. 13. 2012.
[23] D.Seborg, T. Edgar, D. Mellicamp and F. Doyle III, “Process Dynamics and Control,”
John Wiley Sons, p. 595, 2011.
[24] B. Roffel and B. H. Betlem, Process dynamics and control: modeling for control and
prediction. 2006.
[25] “Chemical_Process_Control_an_Introduction_To_Theory_and_Practice.Pdf.” .
[26] HAZOP: Guide to Best Practice ,3rd Edition Book by Brian Tyler and Frank Crawley
[27] EPA https://cfpub.epa.gov/ncea/risk/hhra/recordisplay.cfm?deid=46450 [Online]
[28] NIH, Toxicology Data Network https://sciencing.com/carbon-dioxide-affect-
environment-8583965.html [Online]
134
13 Appendix:
Appendix A: Equipment Design
Figure A.13.1: Relation between downcomer area and weir length
Figure A.13.2: Weep Point Correlation
135
Figure A.13.3: Discharge Coefficient Sieve Plate
Figure A.13.4: Maximum Allowable Stress
136
Appendix B: Pumps and Compressor
Figure B.1: Selection of Pump
Figure B.2: Rule of thumbs for locating the process equipment
Figure B.3: Estimate Frictional pressure losses ED and ES
137
Figure B.4: Efficiency of Pump
Figure B.5: Efficiency of Electric motor
138
Figure B.6: Standard Sizes
Figure B.7: Selection of Compressor
Figure B.8: Compressibility factor
139
Figure B.9: Hydraulic Efficiency Graph
Figure B.10: Compressor Gear, Bearing, and Seal Efficiencies
140
Appendix C: Cost Estimation
Figure C.1: Cost of Equipment
Figure C.2: Cost of Plates
141
Appendix D: Heat Exchanger
Figure D.1: Heat Exchanger Tube Data
Figure D.2: Tube Sheet Layout
142
Figure D.3: Overall Design Coefficient
Figure D.4: Tube Side Return Pressure Loses
143

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PRODUCTION OF 40,000 TPA OF PHTHALIC

ANHYDRIDE FROM OXIDATION OF O-XYLENE

Engr. Muhammad Rashed Javed

Engr Rabia Sabir

Talha Imtiaz UW-15-Ch.E-BSc-001

Department of Chemical Engineering,

Wah Engineering College,

This report is submitted to the Department of Chemical Engineering, Wah Engineering

Department of Chemical Engineering,

12 References: ................................................................................................................................. 133

Figure 1.1: Phthalic Anhydride ............................................................................................................. 1

Figure 1.1: Structure Figure 1.2: Phthalic Anhydride

1.1 Physical and Thermodynamic Properties:

Table 1.1: Thermodynamic and Physical Properties

Properties Phthalic Anhydride Maleic Xylene

1.2 Chemical Reactions:

C6H4(CO)2O + H2O C6H4(CO2H)2

1.3 Uses and Industrial Applications:

Uses of Phthalic Anhydride

Plasticizers Alkyl resins Polymer resins Other uses

Figure 1.3: Industrial Applications

C8H4O3 + ROH C6H4(CO2H)CO2R

1.3.2 Unsaturated polyester resins:

1.3.3 Alkyd Resins:

1.3.5 Other uses:

1.4 Production and Consumption in Pakistan:

1.5 Production and Consumption in world:

Estimated production volume world wide

Figure 1.4: Production in World

1.6 Future Trends:

1.7 Market Assessment:

 Avoid all personal contact, including inhalation.

 Wear protective clothing when risk of exposure occurs.

 Use in a well -ventilated area.

 Avoid contact with moisture.

 Avoid contact with incompatible materials.

 Avoid physical damage to containers

2.1 Production from naphthalene:

2.2 Production of O-xylene:

C8H10 + 3O2 C8H4O3 + 3H2O

2.4 Comparison of Naphthalene & O-xylene Process:

2.5 Selection of BASF process:

2.6 Capacity Selection:

2.7 Process description of selected process:

C8H10 + 3O2 C8H4O3 + 3H2O (Main reaction)

O-xylene Phthalic anhydride

C8H10 + 15/2O2 C4H2O3 + 4H20 + 4CO2 (side reaction)

O- xylene Maleic anhydride

T(°C) Maleic anhydride CO2 Phthalic anhydride

300 1.00 0.00 0.00

320 0.536 0.0339 0.425

340 0.215 0.102 0.683

360 0.100 0.200 0.700

380 0.0463 0.356 0.598

400 0.0215 0.602 0.377

420 0.00 1.00 0.00

2.8 Selection of Catalyst:

2.9 Choice of a reactor:

Process Flow Diagram of Phthalic Anhydride via O-Xylene Oxidation

Input – Output + Generation – Consumption = Accumulation

Operating time of plant is 330 days/year

40000 Ton 1000 Kg 1 Year 1 Days

Year 1 Ton 330 Days 24 Hr

Inert = 2924.1 – 614.06

Maleic anhydride =(0.101001mol c4H2O3/1 mole c8H10)