Ethanol Production Line

ETHANOL production
Line
No. Team Name Seat No.

1 Alaa Refaay Ghareeb 2
2 Aya Hassaneen Madny 6
3 Aya Atef Hussein 8
4 Aya Abdalla Ali 9
5 Ahmed Ismail Ali 19
6 Ahmed Elsayed Abdelsalam 24
7 Aslam Amgd Gaber 94
8 Hassan Farag Mohamed 142
9 Riham Osama Mohamed 167
10 Abdelrahman Ashraf Mosaad 198
11 Mohamed Khames Mohamed 337
12 Mohamed Reda Tablia 339
13 Mohamed Tarek Mohamed 353
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Table of Contents
Table of Contents ......................................................................................................................... 2
Table of Figures ............................................................................................................................ 7
1 INTRODUCTION ..................................................................................................................... 11
1.1 Physical properties ......................................................................................................... 11
1.2 Chemical properties........................................................................................................ 12
1.3 Manufacture ................................................................................................................... 12
1.4 Uses of Ethanol ............................................................................................................... 13
2 CHAPTER 2: FERMENTATION SECTION.................................................................................. 17
2.1 INTRODUCTION............................................................................................................... 17
2.2 Ethanol Fermentation with Yeast ................................................................................... 18
2.3 What is a Fermentor? ..................................................................................................... 18
2.4 Classification of Fermentation Processes ....................................................................... 22
2.5 The Main Fermenter Layout ........................................................................................... 24
2.5.1 Nutrient Feed Tanks................................................................................................. 24
2.5.2 Sterile Filters ............................................................................................................ 25
2.5.3 Air Compressors ....................................................................................................... 26
2.5.4 Valves ....................................................................................................................... 26
2.5.5 Pumps ...................................................................................................................... 27
2.5.6 Cooling Equipment................................................................................................... 27
2.5.7 Environmental Control............................................................................................. 27
2.5.8 General design data ................................................................................................. 28
2.6 Fermentation section ..................................................................................................... 28
2.6.1 Process Control ........................................................................................................ 30
2.7 Fermentation process ..................................................................................................... 31
2.7.1 Fermentors............................................................................................................... 31
2.8 Centrifugation ................................................................................................................. 33
2.8.1 Biomass Separation (centrifuges) (F-011, F-012)..................................................... 35
2.8.2 Yeast sterilization Tank (A-011) ............................................................................... 35
2.8.3 Ethanol Purification ................................................................................................. 35
3 CHAPTER 3: DISTILLATION AND DEHYDRATION .................................................................... 36
3.1 INTRODUCTION............................................................................................................... 36
3.2 Distillation terminology .................................................................................................. 37
3.3 Types of Distillation ........................................................................................................ 41
3.3.1 Simple Distillation .................................................................................................... 41
3.3.2 Fractional Distillation ............................................................................................... 41
3.3.3 Steam Distillation ..................................................................................................... 42
3.3.4 Vacuum Distillation .................................................................................................. 42
3.3.5 Azeotropic Distillation.............................................................................................. 43
3.4 System components ....................................................................................................... 47
3.4.1 Column shells ........................................................................................................... 47
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3.4.2 Column internals ...................................................................................................... 48
3.4.3 Auxiliary equipment ................................................................................................. 53
3.5 The fractionating column design .................................................................................... 56
3.5.1 The fractionating process ........................................................................................ 56
3.5.2 Number of plates required in a distillation column ................................................. 58
3.5.3 Factors affecting distillation column operation ....................................................... 65
3.5.4 Total plate pressure drop......................................................................................... 68
3.6 Dehydration .................................................................................................................... 69
3.6.1 Theory of adsorption ............................................................................................... 70
3.7 Calculations of distillation unit ....................................................................................... 72
4 CHAPTER 4: WATER AND WASTEWATER TREATMENT ......................................................... 80
4.1 INTRODUCTION............................................................................................................... 80
4.2 Water treatment............................................................................................................. 80
4.2.1 Treatment steps ....................................................................................................... 81
4.3 Wastewater treatment (process condensate)................................................................ 81
4.4 ETP (Effluent Treatment Plant) ....................................................................................... 82
4.4.1 Available treatment options .................................................................................... 83
4.5 Dosing pumps ................................................................................................................. 85
4.5.1 Digital dosing pumps................................................................................................ 85
4.5.2 Mechanical diaphragm dosing pumps ..................................................................... 86
4.6 Biological treatment ....................................................................................................... 87
4.6.1 Equalization tank...................................................................................................... 87
4.6.2 Anaerobic tank ......................................................................................................... 90
4.6.3 Decanter room ......................................................................................................... 92
4.6.4 Decanter Centrifuges ............................................................................................... 93
4.6.5 Aeration tank ........................................................................................................... 94
4.7 Membrane system ........................................................................................................ 101
4.8 Calculations................................................................................................................... 102
4.8.1 Flow calculations .................................................................................................... 102
4.8.2 Velocity calculation ................................................................................................ 102
4.8.3 Chlorine dosage ..................................................................................................... 104
4.8.4 Hypochlorite dosage .............................................................................................. 104
4.8.5 Anaerobic Digestion ............................................................................................... 105
4.8.6 Decanter................................................................................................................. 109
4.8.7 Aeration ................................................................................................................. 110
4.8.8 Reverse osmosis calculations ................................................................................. 112
4.9 References .................................................................................................................... 114
5 CHAPTER 5: EVAPORATION (VINASSE CONCENTRATION UNIT) ......................................... 116
5.1 INTRODUCTION............................................................................................................. 116
5.1.1 Process description ................................................................................................ 116
5.1.2 Purposes of Evaporation ........................................................................................ 118
5.1.3 Industrial Applications ........................................................................................... 118
5.2 Thermodynamics of Evaporation.................................................................................. 118
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5.2.1 What happens during Evaporation? ...................................................................... 118
5.2.2 Mechanism of evaporation .................................................................................... 118
5.2.3 Processing factors – liquid characteristic............................................................... 119
5.2.4 Effect of processing variables ................................................................................ 120
5.3 Thermal design of evaporator ...................................................................................... 120
5.4 Classification of evaporators ........................................................................................ 121
5.4.1 Rising-film Evaporator............................................................................................ 121
5.4.2 Falling Film Evaporators ......................................................................................... 121
5.4.3 Forced circulation evaporators .............................................................................. 122
5.5 Evaporator configuration.............................................................................................. 123
5.5.1 Single stage evaporators ........................................................................................ 123
5.5.2 Multi-effect evaporators........................................................................................ 124
5.5.3 Optimization of Multiple Effect Evaporators ......................................................... 126
5.6 Quadrable effect evaporator ........................................................................................ 127
5.7 Plate evaporator ........................................................................................................... 127
5.7.1 working modes....................................................................................................... 129
5.7.2 AlfaFlash ................................................................................................................. 131
5.7.3 Plate technology .................................................................................................... 131
5.7.4 Patterns .................................................................................................................. 131
5.7.5 Plate Types ............................................................................................................. 132
5.7.6 Plate condensers .................................................................................................... 136
5.7.7 Counter vs co counter ............................................................................................ 136
5.7.8 Arrangement of a plate heat exchanger ................................................................ 137
5.7.9 Plate materials ....................................................................................................... 138
5.7.10 Plate geometry ....................................................................................................... 139
5.7.11 Gaskets ................................................................................................................... 139
5.7.12 Frames materials.................................................................................................... 141
5.7.13 Plate Evaporator Manufacturer: ............................................................................ 141
5.8 AlfaVap.......................................................................................................................... 141
5.9 Separators..................................................................................................................... 144
5.9.1 Selection Criteria for Vapor-Liquid Separators ...................................................... 144
5.9.2 Feed Inlet ............................................................................................................... 145
5.10 Theory of Vertical Separators ....................................................................................... 146
5.10.1 Orientation of the Vessel ....................................................................................... 146
5.10.2 Theory of Separators Applied To V-L Systems ....................................................... 147
5.10.3 Separator Sizing Principles ..................................................................................... 149
5.10.4 Sizing Demister Pads .............................................................................................. 151
5.10.5 Control facilities ..................................................................................................... 153
6 CHAPTER 6: CARBON DIOXIDE LIQUEFACTION UNIT .......................................................... 166
6.1 INTRODUCTION............................................................................................................. 166
6.2 Air pollution .................................................................................................................. 167
6.3 Carbon dioxide .............................................................................................................. 168
6.3.1 Discovery of carbon dioxide................................................................................... 169
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6.3.2 Properties of carbon dioxide ................................................................................. 169
6.4 Sources of carbon dioxide ............................................................................................ 171
6.5 Source of carbon dioxide in the project ....................................................................... 175
6.6 Applications of Carbon Dioxide .................................................................................... 177
6.6.1 Gas CO2 .................................................................................................................. 177
6.6.2 Liquid CO2............................................................................................................... 182
6.6.3 Solid CO2 (dry ice) .................................................................................................. 184
6.6.4 Supercritical CO2 .................................................................................................... 185
6.6.5 Future Thrusts of CO2 in Food and Processing Industries ..................................... 188
6.7 Process equipment's ..................................................................................................... 189
6.7.1 Major Equipment & How the process occurs ........................................................ 191
7 CHAPTER 7: AUXILIARY EQUIPMENT’S ................................................................................ 197
7.1 Cooling tower ............................................................................................................... 197
7.1.1 INTRODUCTION ...................................................................................................... 197
7.1.2 Cooling Tower Types .............................................................................................. 197
7.1.3 Components of Cooling Tower .............................................................................. 197
7.1.4 Tower Materials ..................................................................................................... 199
7.1.5 Cooling tower for fermentation section ................................................................ 200
7.1.6 Cooling tower of rest all section ............................................................................ 203
7.2 Boiler Selection ............................................................................................................. 206
8 CHAPTER 8: FIREFIGHTING .................................................................................................. 220
8.1 Detectors ...................................................................................................................... 220
8.1.1 Heat Detector......................................................................................................... 220
8.2 Foam ............................................................................................................................. 222
8.2.1 How foam extinguishes a flammable liquid fire .................................................... 222
8.2.2 Alcohol resistant-aqueous film forming foam (ar-afff) .......................................... 223
9 CHAPTER 9: TANKS .............................................................................................................. 224
9.1 INTRODUCTION............................................................................................................. 224
9.2 Types of storage tanks .................................................................................................. 224
9.2.1 Fixed-Roof Tank ..................................................................................................... 225
9.2.2 External Floating Roof Tank ................................................................................... 225
9.2.3 Internal Floating Roof Tank.................................................................................... 226
9.2.4 Domed External Floating Roof Tank ...................................................................... 226
9.2.5 Horizontal Tank ...................................................................................................... 227
9.2.6 Variable Vapor Space Tank .................................................................................... 227
9.2.7 LNG Storage Tank................................................................................................... 227
9.3 Floating Roof Tanks ...................................................................................................... 228
9.3.1 History and Introduction........................................................................................ 228
9.3.2 Principles of the Floating Roof ............................................................................... 228
9.3.3 Advantages of the floating roof storage tank ........................................................ 229
9.3.4 Process Description and Requirements ................................................................. 230
9.4 Shell Design................................................................................................................... 232
9.5 Fixation ......................................................................................................................... 237
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9.5.1 Types of pipe support ............................................................................................ 238
9.5.2 Details of drain tube C1 R1 pdf: ............................................................................. 241
9.6 Welding ......................................................................................................................... 242
9.6.1 Types of welding .................................................................................................... 242
9.6.2 Weld Size................................................................................................................ 242
9.6.3 Welding Symbols.................................................................................................... 243
10 APPENDIX I: HYSYS REPORTS ............................................................................................... 247
10.1 Fermentation hysys report ........................................................................................... 247
10.2 Carbon dioxide hysys report ......................................................................................... 258
10.2.1 Streamlines composition ....................................................................................... 259
10.2.2 Process equipment: ............................................................................................... 269
10.2.3 Important functions ............................................................................................... 277
1 APPENDIX II: TANK DRAWINGS ........................................................................................... 278
2 APPENDIX III: P AND ID ........................................................................................................ 282
11 References........................................................................................................................... 286
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Table of Figures
Figure 1-1 Structure of ethanol .................................................................................................. 11
Figure 1-2 Molasses .................................................................................................................... 13
Figure 2-1 Fermentor ................................................................................................................. 19
Figure 2-2 Multistage continuous separation: Multiple separate addition is our case ............. 23
Figure 2-3 level controller .......................................................................................................... 23
Figure 2-4 single stage continuous system................................................................................. 23
Figure 2-5 Domnick -hunter sterile air filter............................................................................... 25
Figure 2-6 Disk-bowl centrifuge ................................................................................................. 34
Figure 2-7 Theory of centrifugation ........................................................................................... 34
Figure 3-1 Distillation unit .......................................................................................................... 36
Figure 3-2 Fractional column ...................................................................................................... 41
Figure 3-3 Steam distillation....................................................................................................... 42
Figure 3-4 Schematic drawing of vacuum distillation ................................................................ 43
Figure 3-5 Azeotropic distillation for the separation of ethanol from water using benzene as
entrainer. .................................................................................................................................... 44
Figure 3-6 Azeotropic Distillation Without an Entraining Agent ................................................ 45
Figure 3-7 Azeotropic Distillation Using Pressure Swings .......................................................... 46
Figure 3-8 Tray column ............................................................................................................... 48
Figure 3-9 Sieve tray ................................................................................................................... 48
Figure 3-10 Tray column ............................................................................................................. 48
Figure 3-11 Dual flow tray ......................................................................................................... 50
Figure 3-12 Valve tray................................................................................................................. 51
Figure 3-13 Bubble cap tray ....................................................................................................... 51
Figure 3-14 Packings ................................................................................................................... 52
Figure 3-15 Vertical reboiler ....................................................................................................... 54
Figure 3-16 Kettle type reboiler ................................................................................................. 54
Figure 3-17 Internal reboiler ...................................................................................................... 54
Figure 3-18 Vent condenser ....................................................................................................... 55
Figure 3-19 Fractional distillation column .................................................................................. 56
Figure 3-20 Mass balance a cross distillation column ................................................................ 60
Figure 3-21 Operating line for the rectification section ............................................................. 61
Figure 3-22 Operating Line for the Stripping Section ................................................................. 62
Figure 3-23.................................................................................................................................. 62
Figure 3-24 tray number using graphical solution ..................................................................... 63
Figure 3-25 Feed line .................................................................................................................. 64
Figure 3-26 Dehydration section ................................................................................................ 72
Figure 4-1 Block flow diagram .................................................................................................... 83
Figure 4-2 Block flow diagram .................................................................................................... 83
Figure 4-3 P and ID ..................................................................................................................... 84
Figure 4-4 Schematic view of equalization-homogenization tank ............................................. 88
Figure 4-5 Process condensate treatment plant ........................................................................ 89
Figure 4-6 Equalization tank ....................................................................................................... 89
Figure 4-7 Anaerobic hybrid reactor .......................................................................................... 91
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Figure 4-8 Anaerobic digestor .................................................................................................... 92
Figure 4-9 Process condensate tank ........................................................................................... 93
Figure 4-10 Flottweg decanter ................................................................................................... 93
Figure 4-11 Decanter ................................................................................................................. 94
Figure 4-12 Aeration tank........................................................................................................... 96
Figure 4-13 Aeration tank real view ........................................................................................... 96
Figure 4-14 Types of Aeration .................................................................................................... 97
Figure 4-15 Types of Diffuser ..................................................................................................... 97
Figure 4-16 Aeration blowers ..................................................................................................... 98
Figure 4-17 Aeration Diffusers ................................................................................................... 99
Figure 4-18 Aeration blowers ..................................................................................................... 99
Figure 4-19 Block flow diagram ................................................................................................ 101
Figure 4-20 Reverse osmosis .................................................................................................... 101
Figure 4-21 RO skid................................................................................................................... 101
Figure 4-22 Reverse osmosis vessel ......................................................................................... 101
Figure 4-23 Schematic drawings of septic tanks ...................................................................... 109
Figure 4-24 Flottweg decanter ................................................................................................. 109
Figure 5-1 General description of how Vinasse can be treated and processed ....................... 117
Figure 5-2 Schematic drawing of evaporator ........................................................................... 117
Figure 5-3 Rising vs Falling Film evaporator ............................................................................. 122
Figure 5-4 Forced circulation evaporator ................................................................................. 123
Figure 5-5 Simplified diagram of single –effect evaporator ..................................................... 124
Figure 5-6 Backward-feed, triple-effect ................................................................................... 125
Figure 5-7 Forward -feed, triple effect ..................................................................................... 125
Figure 5-8 Quadrable effect evaporator .................................................................................. 127
Figure 5-9 Comparison between multi-effect plate and tubular evaporator .......................... 127
Figure 5-10 Plate evaporator.................................................................................................... 128
Figure 5-11 Comparison of plate and sht heat exchanger ....................................................... 129
Figure 5-12 Once through Mode .............................................................................................. 129
Figure 5-13 Forced circulation with boiling .............................................................................. 130
Figure 5-14 Thermo siphon mode ............................................................................................ 130
Figure 5-15 Forced circulation with flashing ............................................................................ 131
Figure 5-16 Typical cathegories of plate corrugations. (a) washboard, (b) zigzag, (c) chevron or
herringbone, (d) protrusions and depressions (e) washboard with secondary corrugations, e (f)
oblique washboard [3]. ............................................................................................................ 132
Figure 5-17 Wide gap plate ...................................................................................................... 132
Figure 5-18 gap between plates ............................................................................................... 133
Figure 5-19 double wall plate ................................................................................................... 133
Figure 5-20 laser welding ......................................................................................................... 134
Figure 5-21 Semi welded plate ................................................................................................. 134
Figure 5-22 Semi welded plate ................................................................................................. 134
Figure 5-23 semi-welded plate ................................................................................................ 135
Figure 5-24 Plate evaporator.................................................................................................... 135
Figure 5-25 Leakage detection hole ......................................................................................... 135
Figure 5-26 plate condenser..................................................................................................... 136
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Figure 5-27 plate vs sht counter flow comparision .................................................................. 137
Figure 5-28 U arrangement and Z arrangement ...................................................................... 138
Figure 5-29 Multi-pass PHE ...................................................................................................... 138
Figure 5-30 Four possible 4-1 arrangements ........................................................................... 138
Figure 5-31 Four possible 3-2 arrangements ........................................................................... 138
Figure 5-32 AlphaVap Models .................................................................................................. 141
Figure 5-33 Comparison between space of sht and plate ....................................................... 143
Figure 5-34 Alignment of demister pad ................................................................................... 152
Figure 6-1 Carbon dioxide levels in the atmosphere................................................................ 168
Figure 6-2 Molecule of carbon dioxide..................................................................................... 170
Figure 6-3 Phase diagram of carbon dioxide ............................................................................ 170
Figure 6-4 Carbon dioxide from fossil fuel combustion ........................................................... 172
Figure 6-5 Human sources of carbon dioxide........................................................................... 172
Figure 6-6 Natural sources of carbon dioxide .......................................................................... 173
Figure 6-7 Industrial carbon dioxide emissions in different countries ..................................... 174
Figure 6-8 CO2 Produced from Brewing................................................................................... 177
Figure 6-9 Demister ped ........................................................................................................... 191
Figure 6-10 Screw compressor structure ................................................................................. 191
Figure 6-11 Oil lubrication compressor .................................................................................... 192
Figure 6-12 After cooler ........................................................................................................... 192
Figure 6-13 High pressure scrubber ......................................................................................... 193
Figure 6-14 Twin tower drayer ................................................................................................. 193
Figure 6-15 Condenser ............................................................................................................. 194
Figure 6-16 Gas- liquid separator ............................................................................................. 194
Figure 6-17 Reflux condenser ................................................................................................... 195
Figure 6-18 Stripping column ................................................................................................... 196
Figure 7-1 Cooling water system .............................................................................................. 197
Figure 7-2 Cooling tower types ................................................................................................ 198
Figure 7-3 Cooling Tower and chiller plant piping.................................................................... 201
Figure 8-1.................................................................................................................................. 220
Figure 8-2.................................................................................................................................. 221
Figure 9-1 Breather Valve (pressure-vacuum Valve)................................................................ 225
Figure 9-2 Storage tank capacities levels ................................................................................. 230
Figure 9-3 Tank bottom Plate ................................................................................................... 230
Figure 9-4 conical bottom with sluice point device ................................................................. 231
Figure 9-5 Rotational of the shell to bottom connection ........................................................ 232
Figure 9-6 Longitudinal Stress .................................................................................................. 233
Figure 9-7 Circumferential stress ............................................................................................. 234
Figure 9-8.................................................................................................................................. 236
Figure 9-9 Tank Shell Testing .................................................................................................... 237
Figure 9-10 Rigid springs .......................................................................................................... 238
Figure 9-11 Variable spring hanger .......................................................................................... 238
Figure 9-12 Variable spring hanger .......................................................................................... 238
Figure 9-13................................................................................................................................ 239
Figure 9-14................................................................................................................................ 239
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Figure 9-15................................................................................................................................ 240
Figure 9-16................................................................................................................................ 240
Figure 9-17................................................................................................................................ 240
Figure 9-18 Drain tube.............................................................................................................. 241
Figure 9-19 Details of drain tube .............................................................................................. 241
Figure 9-20 Sheet clamping ...................................................................................................... 241
Figure 9-21 Welding symbols ................................................................................................... 243
Figure 9-22 Horizontal shell joints ............................................................................................ 244
Figure 9-23 Method for Preparing Lap-Welded Bottom Plates under Tank Shell ................... 244
Figure 9-24 Spacing of Three-Plate Welds at Annular Plates. .................................................. 245
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INTRODUCTION
1 INTRODUCTION
Ethyl Alcohol (Ethanol) C2H5OH is an Aliphatic hydrocarbon containing hydroxyl
group (-OH), Its name is the systematic name defined by the International Union of
Pure and Applied Chemistry (IUPAC) for a compound consisting of alkyl group with
two carbon atoms (prefix “eth-”), having a single bond between them (infix “-an-”),
attached functional group −OH group (suffix “-ol”). With Chemical formula of
C2H6O or better be CH3-CH2-OH.
The physical and chemical properties of ethanol stem primarily from the presence
of its hydroxyl group and the shortness of its carbon chain.
This group imparts polarity to the molecule and gives rise to intermolecular
hydrogen bonding. These two properties account for the differences between the
physical behavior of lower molecular weight alcohols and that of hydrocarbons of
equivalent weight.
Figure 1-1 Structure of ethanol
1.1 Physical properties

Ethanol under ordinary conditions is a volatile, flammable, clear, colorless liquid.
Its odor is pleasant, familiar, and characteristic, as is its taste when suitably diluted
with water. The most amazing property of ethanol is the volume shrinkage that
occurs when it is mixed with water, or the volume expansion that occurs when it is
mixed with gasoline. It burns with a smokeless blue flame that is not always visible
in normal light. Ethanol's hydroxyl group is able to participate in hydrogen bonding,
rendering it more viscous and less volatile than less polar organic compounds of
similar molecular weight, such as propane.
Molar Mass 46.069 gm/mol
Density at 20 °C 789.3 kg/cm3
Boiling point at 1 Bar 78.32 °C
Viscosity at 20 °C 1.17 mPa.s
Heat combustion at 25 °C 29686.69 J/gc
Melting point −114.14 °C
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INTRODUCTION
1.2 Chemical properties

Reactions of dehydration, dehydrogenation, oxidation, and esterification.
The hydrogen atom of the hydroxyl group can be replaced by an active metal, such
as Sodium, to form a metal ethoxide (ethylate) with the evolution of hydrogen gas.
Barbiturates (Verona, Barbital, Luminal, Amytal), ethyl orthoformate, and other

chemicals are produced commercially from sodium ethoxide.
Aluminum and magnesium also react to form ethoxides, but the reaction must be
catalyzed by amalgamating the metal (adding a small amount of mercury).
1.3 Manufacture
Industrial ethyl alcohol can be produced synthetically from ethylene, as a by-
product of certain industrial operations, or by the fermentation. There are two main
processes for the synthesis of ethyl alcohol from ethylene. The earliest to be
developed was the indirect hydration process and the other is direct hydration
process.
1. Indirect hydration (Esterification–Hydrolysis) process
Preparation from ethylene by the use of sulfuric acid is a three-step
process:
1. Absorption of ethylene in concentrated sulfuric acid to form
monomethyl sulfate (ethyl hydrogen sulfate) and diethyl
sulfate
2CH2=CH2 + H2SO4 (CH3CH2O)2SO2
2. Hydrolysis of ethyl sulfates to ethanol:

(CH3CH2O)2SO2 + 2 H2O 2 CH3CH2OH + H2SO4
3. Re-concentration of the dilute sulfuric acid.
1. Direct hydration process

Hydration of ethylene to ethanol via a liquid-phase process catalyzed
by dilute sulfuric acid, the passage of an ethylene-steam mixture over
alumina at 300◦C was found to give a small yield of acetaldehyde, and
it was inferred that this was produced via ethanol. Then, several
industrial concerns have expressed interest in producing ethanol
synthetically from ethylene over solid catalysts.
There are two main process categories for the direct hydration of
ethylene to ethanol. Vapor-phase processes contact a solid or liquid
catalyst with gaseous reactants. Mixed-phase processes contact a
solid or liquid catalyst with liquid and gaseous reactants.
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INTRODUCTION
3. Fermentation
It is one of the oldest chemical processes known, it is used to make a variety
of products, including fuel, foods, flavorings, beverages, chemicals and
pharmaceuticals.
Fermentation processes was accounting for 83% of total production and by

2001 fermentation increased to 90%. Ethanol can be derived by
fermentation processes from any material that contains sugar or compounds
that can be converted to sugar mostly corn even though before World War II
molasses was the chief feedstock. Other agricultural products such as grains,
sugar cane and beets, fruit, whey, and sulfite waste liquor. Studies are
underway to ferment garbage to ethanol.
➢ Sugar Beet Molasses

Only the syrup left from the final crystallization stage is called
molasses. Beet molasses is 50% sugar by dry weight, predominantly
sucrose. Molasses is a microbiological energy source that helps in the
process of growing yeast and bacteria. Beet molasses is limited in
biotin for cell growth; hence, it may be supplemented with a biotin
source important for growth of bacteria and yeasts accelerating
fermentation for ethanol production.
Figure 1-2 Molasses
1.4 Uses of Ethanol

➢ Medical
✓ Antiseptic
Used as antibacterial, antiseptic for its bactericidal and anti-fungal
effects. Ethanol kills organisms by denaturing their proteins and
dissolving their lipids and is effective against most bacteria and fungi,
and many viruses but not bacterial spores. 70% ethanol is the most
effective concentration, particularly because of osmotic pressure.
Absolute ethanol may inactivate microbes without destroying them
because the alcohol is unable to fully permeate the cellular membrane.
Ethanol can also be used as a disinfectant and antiseptic because it
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INTRODUCTION
causes cell dehydration by disrupting the osmotic balance across cell

membrane, so water leaves the cell leading to cell death.
✓ Antidote
Used as an antidote to methanol and ethylene glycol poisoning.
✓ Medicinal solvent
Used in high concentrations to dissolve many water-insoluble
medications and related compounds.
✓ Medication
Used as main central nervous system depressant drug.
➢ As a fuel
✓ Engine fuel
The largest single use of ethanol is as an engine and fuel additive. In
Brazil gasoline sold contains at least 25% anhydrous ethanol while
hydrous ethanol can be used as fuel in more than 90% of new gasoline
fueled cars.
✓ Rocket fuel
Ethanol was commonly used as fuel in early bipropellant rocket (liquid
propelled) vehicles, in conjunction with an oxidizer such as liquid
oxygen.
✓ Fuel cells
Commercial fuel cells operate on reformed natural gas, hydrogen or
methanol. Ethanol is an attractive alternative due to its wide
availability, low cost, high purity and low toxicity.
✓ Household heating
Ethanol fireplaces can be used for home heating or for decoration.
➢ Feedstock
Ethanol is an important industrial ingredient. It has widespread use as a
precursor for other organic compounds such as ethyl halides, ethyl esters,
diethyl ether, acetic acid, and ethyl amines.
➢ Solvent
Ethanol is considered a universal solvent, as its molecular structure allows
for the dissolving of both polar, hydrophilic and nonpolar, hydrophobic
compounds allowing easy extraction of botanical oils.
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INTRODUCTION
As ethanol also has a low boiling point, it is easy to remove from a solution
that has been used to dissolve other compounds and also as a post-
processing solvent to remove oils, waxes, and chlorophyll from solution in a
process known as winterization. Ethanol is found in paints, tinctures,
markers, and personal care products such as mouthwashes, perfumes and
deodorants. However, polysaccharides precipitate from aqueous solution in
the presence of alcohol, and ethanol precipitation is used for this reason in
the purification of DNA and RNA.
➢ Low-temperature liquid
Because of its low melting point (−114.14 °C) and low toxicity, it is used in
laboratories as a cooling bath to keep vessels at temperatures below the
freezing point of water.
For the same reason, it is also used as the active fluid in alcohol
thermometers.
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CAPTER 2: FERMENTATION SECTION
2 CHAPTER 2: FERMENTATION SECTION

2.1 INTRODUCTION
Fermentation is a bio-chemical reaction where the substrate is converted into
desired product with the help of micro-organism which may be yeast, Mould or
bacteria and the enzyme present in the Microorganism actually acts in the reaction.
Reaction: C6 H12 O6 ------> 2 C2 H5 OH + 2 CO2

(sugar) (alcohol)
The yeast Saccharomyces cerevisiae that is used for the culture for Alcohol
fermentation is having two kinds of enzymes, one’s INVERTASE and other is
ZYMASE. Invertase converts sucrose to invert sugar and Zymase converts invert
sugar into Ethyl Alcohol. Fermentation is a dynamic process involving a series of
reactions. These are:
1. Enzymes added after cooling continuous to convert the gelatinized starch
to dextrin’s and fermentable sugars.
2. The yeast metabolizes sugar to acetaldehydes and then to ethanol. The cycle
is known as Glycolysis. The lactic acid bacteria produce small amounts of a
variety of products, some of which are volatile and contribute to the
congeners in the distillate.
Molasses is transported in the cells via specific carrier proteins called Permeases
where it is hydrolyzed into 2 molecules of glucose. The Permeases are substrate
and require metabolic energy for operation.
C6H12O6 --> 2 C2H5OH +2 CO2 + 2 ATP + heat
Two moles of ATP (Adenosine Triphosphate) are also produced which are used to
supply energy for cell maintenance and growth. Theoretically conversion of 1gm of
glucose via fermentation yields 0.511grms of ethanol. This theoretical value is
never obtained due to carbohydrate utilization for cell maintenance, growth and
formation of small amounts of glycerol's and higher alcohols.
Fermentation efficiency also depends upon factors such as yeast strain and
environmental parameters. In practice efficiency is 60-80%. An increase in temp
within a certain range increases activity. The condition in Fermentation vats are
such obtained so as to avoid bacterial action. During a normal Fermentation heat is
produced from active yeast growth and metabolism which causes a rise in temp.
Then this temp rise can drastically affect yeast metabolism and ethanol. An average
upper limit temp for growth is around 40’ C with an optimum temp of about 30’C.
Increased heat tolerances are obtained with media containing oleic acid. The
maximum concentration of ethanol that yeast can produce depends upon the yeast
strain used. In general, yeast cell growth is inhibited around 10 to 12% wt/vol.
ethanol while 20% ethanol will terminate cellular metabolism.
Page | 17
2.2 Ethanol Fermentation with Yeast

The organisms of primary interest to industrial operations in fermentation of
ethanol include Saccharomyces cerevisiae, S. uvarum, Schizosaccharomyces pombe,
and Kluyueromyces sp. Yeast, under anaerobic conditions, metabolize glucose to
ethanol primarily by way of the Embden-Meyerhof pathway. The overall net
reaction involves the production of 2 moles each of ethanol, but the yield attained
in practical fermentations however does not usually exceed 90 – 95% of theoretical.
This is partly due to the requirement for some nutrient to be utilized in the synthesis
of new biomass and other cell maintenance related reactions.
A small concentration of oxygen must be provided to the fermenting yeast as it is a

necessary component in the biosynthesis of polyunsaturated fats and lipids. Typical
amounts of O2 maintained in the broth are 0.05 – 0.10 mm Hg oxygen tension. The
relative requirements for nutrients not utilized in ethanol synthesis are in
proportion to the major components of the yeast cell. These include carbon oxygen,
nitrogen and hydrogen. To lesser extent quantities of phosphorus, sulfur,
potassium, and magnesium must also be provided for the synthesis of minor
components. Minerals (i.e. Mn, Co, Cu, Zn) and organic factors (amino acids, nucleic
acids, and vitamins) are required in trace amounts. Yeast are highly susceptible to
ethanol inhibition. Concentration of 1-2% (w/v) are sufficient to retard microbial
growth and at 10% (w/v) alcohol, the growth rate of the organism is nearly halted.
Fermentation at PDM is done through two ways:

1. Grain spirit plant (From wheat or rice flour).
2. Fermentation from Molasses.
PROCESS PARAMETERS
a. NUTRIENTS: Generally, di ammonium phosphate (DAP) and urea are
used as nutrients. These are used so as to form amino acid to give energy
and to carry out propagation faster.
b. TEMPERATURE: Temperature of the material in the fermenter is 32 to
34 °C.
c. PRESSURE: The process is carried out at Normal Pressure.
d. ANTIFOAM: 25% Silicon antifoam was prepared to control the foam
formation in the pre-fermenter and the fermenter.
2.3 What is a Fermentor?

A Fermentor can be defined as a vessel in which sterile nutrient media and pure
culture of micro-organism are mixed and fermentation process is carried out under
aseptic and optimum condition.
Fermentor provides a sterile environment and optimum condition that are

important for growth of micro-organisms and synthesis of desired product.
Page | 18
Figure 2-1 Fermentor
A fermentor should be constructed in such a way that it can make provisions for the
below activities:
▪ Sterilization.
▪ Temperature control.
▪ pH control.
▪ Foam control.
▪ Aeration and agitation.
▪ Sampling point.
▪ Inoculation points for micro-organisms, media and supplements.
▪ Drainage point for drainage of fermented media.
▪ Harvesting of product.
▪ Cleaning.
▪ Facility of providing hot, cold water and sterile compressed air.
Page | 19
Here one by one we will be studying major parts of fermentor and their function.
▪ Material used for fermentor
▪ Impellers
▪ Baffles
▪ Inoculation port
▪ Sparger
▪ Sampling point
▪ pH control device
▪ Temperature control system
▪ Foam control device
▪ Bottom drainage system
1. Material used for fermentor

The material used for designing of a fermentor should have some important
functions.
▪ It should not be corrosive
▪ It should not add any toxic substances to the fermentation media.
▪ It should tolerate steam sterilization process.
▪ It should be able to tolerate high pressure and resist pH changes.
The fermentor material used is also decided on type of fermentation process.
For example, in case of Beer, Wine, Lactic acid fermentation, the fermentor
tanks are made up of wooden material. Whereas material such as iron,
copper, glass and stainless steel can be used in some cases. Most of the time,
304 and 316 stainless steel is used for designing of a fermentor and these
fermentors are mostly coated with epoxy or glass lining.
A fermentor should provide the facility to control and monitor various

parameters for a successful fermentation process.
2. Impellers
▪ Impellers are an agitation device. They are mounted on the shaft and
introduced in the fermentor through its lid.
▪ They are made up of impeller blades and the position may vary
according to its need.
▪ These impellers or blades are attach to a motor on lid.
▪ The important function of an impeller is to mix micro-organisms,
media and oxygen uniformly.
▪ Impeller blades reduce the size of air bubbles and distributes these
air bubbles uniformly into the fermentation media.
▪ Impellers also helps in breaking foam bubbles in the head space of
fermentor. This foam formed during fermentation process can cause
contamination problem and this problem is avoided by the use of
impellers.
Page | 20
3. Baffles
▪ Baffles are mounted on the walls of a fermentor.
▪ The important function of baffles is to break the vortex formed during
agitation process by the impellers.
▪ If this vortex is not broken, the fermentation media may spill out of
fermentor and this may result in contamination as well as can lead to
different problems. So, it is important to break the vortex formed by
using a barrier.
▪ Baffles acts as a barrier which break the vortex.
4. Inoculation Port
▪ Inoculation port is a device from which fermentation media,
inoculum and substrate are added in the fermentation tank.
▪ Care should be taken that the port provides aseptic transfer.
▪ The inoculation port should be easy to sterilize.
5. Spargers
▪ A Sparger is an aeration system through which sterile air is
introduced in the fermentation tank.
▪ Spargers are located at the bottom of the fermentation tank.
▪ Glass wool filters are used in a sparger for sterilization of air and
other gases.
▪ The sparger pipes contain small holes of about 5-10 mm. Through
these small holes pressurized air is released in the aqueous
fermentation media.
▪ The air released is in the form of tiny air bubbles. These air bubbles
helps in mixing of media.
6. Sampling point
▪ Sampling point is used for time to time withdrawal of samples to
monitor fermentation process and quality control.
▪ This sampling point should provide aseptic withdrawal of sample.
7. pH Control device
▪ The pH controlling device checks the pH of media at specific intervals
of time and adjusts the pH to its optimum level by addition of acids or
alkalis.
▪ Maintaining pH to its optimum level is very important for growth of
micro-organism to obtain a desired product.
Page | 21
8. Temperature control
▪ Temperature control device generally contains a thermometer and
cooling coils or jackets around fermentor.
▪ During the fermentation process, various reactions take place in the
fermentor. Heat is generated and released in the fermentation media.
This increase in temperature is detrimental to the growth of micro-
organisms, which may slow down the fermentation process.
▪ So, it is necessary to control this rise in temperature. This is done by
passing cool water through the coils or jackets present around
fermentor.
9. Foam controlling device

▪ A Foam controlling device is placed on the top of fermentor with an
inlet into fermentor. This device contains a small tank containing
anti-foaming agent.
▪ Foam is generated during fermentation. It is necessary to remove or
neutralize this foam with the help of anti-foaming agents, lest the
media may spill out of fermentor and lead into contamination and a
mess.
10. Bottom drainage system

▪ It is an aseptic outlet present at the bottom of fermentor for removal
of fermented media and products formed.
2.4 Classification of Fermentation Processes

1. Batch process
2. Fed-batch process (semi-batch process)
3. Repeated fed-batch process (cyclic fed-batch process)
4. Repeated fed-batch process (semi-continuous process or cyclic batch
process)
5. Continuous process
The continuous operations are three types of operations. without feedback control,
the feed medium containing all the nutrients is continuously fed at a constant rate
(dilution rate) and the cultured broth is simultaneously removed from the
fermenter at the same rate. A. This type is quite useful in the optimization of media
fonnulation and to investigate the physiological state of the microorganism, with
feedback control is a continuous process to maintain the cell concentration at a
constant level by controlling the medium feeding rate, with feedback control is a
cultivation technique to maintain a nutrient concentration at a constant level, an
extended nutristat which maintains the pH value of the medium in the fermenter at
a preset value.
Page | 22
Figure 2-2 Multistage continuous separation: Multiple separate addition is

our case
Figure 2-4 single stage continuous system

Figure 2-3 level controller
Page | 23
2.5 The Main Fermenter Layout

For simplicity of piping, especially the utility piping, the fermenters are usually
placed in a straight line, sometimes two or more parallel lines . In this manner the
plant is easily expanded, and other tank layouts do not seem as convincing. It is
desirable to have the working platform extend completely around the
circumference of the top dish, and to have enough room between tanks for
maintenance carts (1 to 1.5 meters). Good lighting and ventilation on the working
platform should not be overlooked. Using water from hoses for cleaning is common
so care must be taken to have nonskid floors with adequate drains, especially at the
top of stairs. Open floor grating is not desirable.
All structural steel should be well primed to prevent corrosion from the very humid
atmosphere. Electronic instrumentation and computers must be placed in control
rooms which run at constant (HVAC) temperature. Most fermenter buildings are
between 40 and 100 feet high, making it possible to have one or more floors
between the ground floor and the main fermenter working platform. The
intermediate floors can be used for the utility and process piping, sterile air filters,
the sterile anti-foam system, instrumentation sensors (temperature, pH, DO, etc.),
heat exchangers, motor control center, laboratories and offices. Buildings 40 feet or
more high frequently have elevators installed.
Fermenters can be located outdoors in most countries of the world. The working
platforms usually are enclosed and heated in temperate zones, and only shaded in
more tropical zones. In more populated areas, open fermenter buildings make too
much noise for local residents. The environmental awareness, or the tolerance of
the public, could preclude open fermenter buildings in the future. Odor is also
offensive to the public. The environmental authorities are demanding that
equipment be installed to eliminate the offensive odor of the off gases. (Noise levels
inside a fermenter building will be greater than 90 dB if no preventive measures are
taken.) Harvest tanks can be justified as the responsibility of the fermentation or
recovery department. They are economical (carbon or stainless steel) and should
be insulated and equipped with cooling coils and agitator(s).
2.5.1 Nutrient Feed Tanks

Essential equipment to a productive fermentation department are sterilizable
tanks for nutrient feeds. Multiproduct plants usually require several different sizes
of feed tanks:
1. A small volume to be transferred once every 12 or 24 hours such as a
nitrogen source.
2. A large volume carbohydrate solution fed continuously, perhaps varying
with the fermenter volume.
3. A precursor feed fed in small amounts relative to assay data; (iv) anti-foam
(Some companies prefer a separate anti-foam feed system for each
fermenter.
4. Other tanks for acids, bases, salts, etc. Many companies prefer to batch
sterilize a known quantity and transfer the entire contents quickly.
Sometimes, the feeds require programming the addition rate to achieve
high productivity.
Page | 24
In this latter case, large volume tanks are used, and the contents are presterilized
(batch or continuous) or the feed is continuously sterilized between the feed tank
and the fermenter. Usually feed tanks are not designed as fermenters, even though
they are sterilizable, and there is no need for high volume air flow, but only
sufficient air pressure for the transfer. For solvable nutrients the agitator and anti-
foam system are not required. Since the air requirements are needed only to
transfer the feed, the air piping design is different, and the sterile air filter is
proportionately smaller. Instrumentation is usually limited to temperature,
pressure and volume. The HID ratio of the vessel can be near one for economy and
need not be designed for the aeration/agitation requirements of a fermenter.
2.5.2 Sterile Filters

Sterile air filtration is simple today with the commercial units readily available.
However, some companies still design their own to use a variety of filter media such
as carbon, cotton, glass staple, etc.
The essential method to obtain sterile air, whether packed-bed or cartridge filters
are used, is to reduce the humidity of the air after compression so that the filter
material always remains dry. The unsterilized compressed air must never reach
100% relative humidity. Larger plants install instrumentation with alarms set at
about 85% relative humidity. Careful selection of the cartridge design or the design
of packed-bed filters will result in units that can operate in excess of three years
without replacement of filter media. If a fiber material is used in a packed-bed type
filter, the finer the fiber diameter the shallower the bed depth needs to be for
efficient filtration. Other filter media are less common and tend to have special
problems and/or shorter life. The bed depth of filters is only 10 to 18 inches for
fibers of less than 10 microns. These filters run "clean" for 2 weeks or longer before
being resterilized.
Some plants have a separate filter for each sterile vessel. Others place filters in a
central group which feeds all the vessels. In this case, one filter, for example, might
be taken out of service. each day sterilized and put back into service. If there were
ten filters in the group, each one would be sterilized every tenth day. This system
has the advantage that the filter can be blown dry after sterilization with sterile air
before it is put into service again.
Figure 2-5 Domnick -hunter sterile air filter
Page | 25
2.5.3 Air Compressors

It is ideal to have oil-free compressed air. Centrifugal machines generally are
available up to 40,000 cfm. "Oil free" screw air compressors are available in smaller
sizes. Regarding oil-free screw type compressors, it is necessary to read the fine
print of the manufacturer. For example, one manufacturer uses no lubricant on the
screws and other claims to be oil free but does use a non-hydrocarbon liquid
lubricant. Carbon ring reciprocating compressors are available and used, but
maintenance is annoying. For small plants, non-lubricated screw compressors with
two-speed motors and constant pressure control will provide versatility. For large
plants, centrifugal air compressors, driven by non-condensing steam turbines with
50 psig steam extraction for process requirements, are suitable. In all cases, extra
considerations include locating the intake 20 feet or more above the ground level
and installing filters on the intake to the compressors to prevent dirt accumulation
on the sterile filters. Occasionally, the noise levels measured at the suction inlet
exceed OSHA regulations and bother the neighbors of the plant. The air from the
compressors requires heat exchangers to lower the air temperature below the dew
point, plus additional heat exchangers to reheat and control the air to have the
relative humidity at about 85%.
2.5.4 Valves
Most companies have tried gate, diaphragm, ball, and plug valves, to name a few.
Some have designed and patented special valves for the bottom or sample positions.
Some companies will disassemble all fermenter valves after an infected run. No
companies use threaded nipples or valves on a fermenter because the threads are a
site of potential infection. In general, valves are less of a sterility problem when a
continuous sterilizer is used for the substrate than fermenters which batch sterilize
the substrate. This is because, in the former case, the vessel is sterilized empty, and
all valves are opened and sterilized in an outward direction so that a steam plume
can be seen. The temperature of the valves during sterilization can be checked.
Batch sterilizing requires all valves below the liquid level to be sterilized with steam
passing through the valve into the substrate. This depends upon steam pressure and
how much the valve is opened (which might affect the PIT conditions of
sterilization). This is much more subject to human error and infection. Most plants
drill and tap the body of the valve near the valve seat in order to drain the
condensate away from all sections of pipe where a steam seal is required for
sterility. In general, diaphragm and ball valves require considerable maintenance,
but tend to be popular in batch sterilizing operations, while plug type valves are
more typical on fermenters where continuous sterilizers are used. Plug or
diaphragm valves are commonly used for inoculum transfer and sterile feed piping.
All the process valves and piping today are 316 SIS. Utility piping remains carbon
steel up to the first SIS valve on the fermenter. Valves used in non-process piping
are selected for the best type of service and/or control. Butterfly valves have been
used in applications where perfect closure is not essential, such as a vent valve. In
summary, the valves which maintain a sterile environment on one side and a non-
Page | 26
sterile environment on the other side are the essential valves. They must be devoid
of pockets, easily sterilized, maintained, and occasionally replaced.
2.5.5 Pumps
Apart from continuous sterilizers, pumps are a minor concern in the fermentation
department. A simple way to transfer inoculum from a large laboratory flask to a
fermenter, without removing the back pressure on the vessel, is to use a peristaltic
pump. Connect the sterile adapter (which is attached to the flask) to the fermenter
by sterile technique. Install the gum rubber tubing in the pump, open the hose clamp
and start the pump. Inoculum from sterile feeds are transferred to the fermenter by
air pressure. Centrifugal pumps (316 SIS) are used to pump non sterile raw
materials, slurries, harvested broth, etc. The centrifugal pumps and piping should
be cleaned immediately after a transfer has been completed. Occasionally a
specialty pump may be required.
2.5.6 Cooling Equipment

Cooling is required to cool media from sterilizing temperatures, to remove the
exothermic heat of fermentation, to cool broth before harvesting, and to cool the
compressed air. Some portion of the heat can be cleaned to produce hot water for
the preparation of new substrate, and for general cleaning of equipment, platforms
and floors, however, the excess heat must be disposed to the environment. Cooling
water is provided from cooling towers, but chilled water (5 15°C) is produced by
steam vacuum, or refrigeration units.
In any case, the fermentation department should always be concerned about its
cooling water supply, i.e., the temperature and chloride content. Chloride ions
above 150 ppm when stainless steel is above 80°C (while sterilizing) will cause
stress corrosion cracking of stainless steel.
A conductivity probe should be in the cooling water line. When the dissolved solids
(salts) get too high, it may indicate a process leak, or that the salt level is too high
and some water must be discharged and fresh water added. If cooling water is
discharged to a stream, river, etc., an NPDES permit may be needed and special
monitoring required. The chloride content should be determined analytically every
two weeks to control the chloride to less than 100 ppm. This is done by draining
water from the cooling tower and adding fresh water.
2.5.7 Environmental Control

Stack odors have to be avoided. Certain raw materials smell when sterilized. Each
fermentation process tends to have its own unique odor ranging from mild to strong
and from almost pleasant to absolutely foul. Due to the high volume of air
discharged from a large fermenter house, odor is neither easy nor cheap to
eliminate. Carbon adsorption is impractical.
Page | 27
Normally, more air is exhausted than required for steam production from the
boilers which eliminates that route of disposal. Wet scrubbing towers with sodium
hypochlorite are expensive ($1.50/yr. cfm), and discharge Na+ and Cl2 to the waste
system which may preclude this method. Ozone treatment can be effective. A very
tall exhaust stack for dilution of the off gas with the atmosphere before the odor
reaches the ground is possible in some cases but is not considered an acceptable
solution by U. S. Authorities.
The fermentation department should monitor and control the CODI BOD of its liquid
waste to the sewer. Procedures for cleaning up spills and reporting should be
Standard Operating Procedure. A primary aeration basin will reduce the COD to 80-
90 ppm. Secondary aeration lagoons will reduce the BOD to acceptable levels which
have no odor.
Noise levels are very difficult to reduce to Federal standards. Hearing protection for
employees is essential. The move towards greater automation has resulted in
operators having less exposure to noisy work areas.
2.5.8 General design data

Most companies produce more than one product by fermentation simultaneously.
It is not necessary to have separate fermenter buildings to isolate products. Well-
designed fermenters which are operated properly, not only keep infection out, but
prevent cross contamination of products. Over the years, most fermentation plants
have been enlarged by the addition of new fermenters despite major yield
improvements. Therefore, as plants grow, the engineer must always keep in mind
there will be a need for further expansions. The layout of labs, fermenter buildings,
the media preparation area and warehousing must be able to be expanded. Utilities
and utility piping must also be installed with spare capacity to handle average and
peak loads as well as future growth.
The fermentation department can consume up to 2/3 of the total plant electrical
requirements (depending upon the recovery process), which includes mechanical
agitation (usually 15 HP/l000 gal) and electrically driven air compressors.
There is no relationship between the cubic feet of compressed air for large
fermenters and their installed capacity. The compressed air required for fermenters
is calculated by linear velocity through the fermenter and the square feet of cross-
sectional area of a vessel, not its volume. Therefore, if volume is constant, short
squat vessels require more compressed air than tall slender vessels.
2.6 Fermentation section

The molasses from molasses storage is mixed with sucrose and Di ammonium
phosphate and Sodium hypochlorite. The temperature of the combined stream is
96 ºC and is to be cooled to fermentation temperature. The cooling of the broth is
carried through in two stages: the hot broth is passed through an heat exchanger
(E-1) in countercurrent with the cold mixing broth, where the mixing broth is
warmed and the broth for distillery is cooled.
Page | 28
Final cooling, approximately 30 Cº, is carried out in the fermenter (BR-1) During the
fermentation, sugar is converted to ethanol with 0.92 of the theoretical yield which
corresponds to 0.46-0.47 g ethanol/g sugar. The remaining substrate is utilized by
the microorganisms for maintenance, cell growth and production of by products
such as succinic acid, glycerol, acetic acid, higher alcohols and acetaldehyde. Also,
0.44-0.48 g CO2 / g sugar is produced during the ethanol fermentation.
Saccharomyces species is used as the ethanol fermenting microorganism. The
fermentation is carried out anaerobically to decrease cell growth and increase the
ethanol productivity.
The fermentation is carried out in 10 vessels to maintain a continuous operation

and to prevent requirement of extra storage tanks for broth and recycle biomass.
The biomass is recycled to maintain high cell concentrations in the fermenters. The
biomass is separated from the broth using continuous disc type centrifuges (S-1)
and sent to biomass sterilization vessel (V-1), which are stirred vessels to blend the
biomass with pH 2 acid solution (sulfuric acid). The residence time in the vessels
are set to 15 minutes. After the sterilization vessel, the biomass is separated from
the acid solutions using centrifuge (S-2). The sulfuric acid is taken outside the
battery limit without treatment, but the cost of waste treatment is included in the
cash flows.
The sulfuric acid requirement for this step is approximately 0.013 kg per kg ethanol
produced. Since, yeast functions at low pH values they are not affected by the pH
treatment. The biomass is recycled to fermenters. By recycling the cells, the long lag
growth phase is eliminated, and high cell concentrations are obtained in fermenters.
Very short fermentation times (6-10 h) allows yeast to be recycled up to three times
a day.
The carbon dioxide rich gas from the fermenters are passed through the ethanol
scrubber column (C-1) to absorb the ethanol in the gas to lower the volatile organic
emissions to atmosphere and to recover the lost ethanol. This column is not only
feed with the gas from the fermenter, but, also with the carbon dioxide rich vapor
distillate from the beer column. The absorption water is recycling water form the
evaporators and boiling pans. The water and ethanol content of the vent gas is 1-2
w/w %. Carbon dioxide can be sold either to beverage and food industries or to dry
ice production facilities.
The water scrubber can remove 99.5% of ethanol in carbon dioxide stream. The
environmental legislations set the upper limit of total volatile components to the
atmosphere as 36.3 T/year. Therefore, the total ethanol released will be set
accordingly.
Page | 29
2.6.1 Process Control

1. Flow Controllers (FC)
▪ Raw materials: sulfuric acid, di ammonium phosphate and sodium
hypochlorite should be weighted to maintain the process
specifications before being send to system.
▪ Air Stream: to prevent heat losses by excess air or incomplete
combustion with less air flow, the air streams flowing into the
furnace and dryer are to be controlled with flow controller to
maintain the required air.
▪ Distillate: bottoms and side products of the distillation columns.
2. Level Controllers (LC)

All the vessels with continuous inflow require a level controller to prevent
any flooding in case of any problem with pumping in/out. The level
controllers are operated based on the liquid height in the vessel and the
manipulated variable is the output flow from the vessel. The controller type
is to be “fail-on” to prevent the overflow of the vessels in case of controller
failure.
3. Ratio Controllers (RC)

The ratio controllers are necessary when the stream split into two or more
streams.
4. Temperature Controllers (TC)

The equipment involving heat transfer are to be supplied with temperature
controller to maintain constant operation conditions. The equipment and
streams that require temperature controller are listed below.
▪ Evaporators and boiling pans.
▪ reactors: The temperature is manipulated by steam input of the
pretreatment. The controller should be fail-close control valve to
prevent steam inflow in case of controller failure.
▪ All Heat exchangers
▪ Re boilers and condensers.
▪ Molecular sieve column.
5. Pressure Controllers (PC)

The equipment that requires a certain operation pressure other than
atmospheric requires pressure controller.
6. pH Controller (pHC)
The pH of the cellulose hydrolysis and fermentation bio reactors should be
monitored to maintain the pH in optimal value.
Page | 30
2.7 Fermentation process

2.7.1 Fermentors
In continuous fermenters, sucrose in juice is hydrolyzed to glucose and
glucose is fermented to microbial biomass, ethanol, carbon dioxide and
fermentation by-products. The fermentation by-products are assumed as
acetic acid, Iso amyl alcohol, glycerol and succinic acid. There are several by-
products of fermentation, but for simplicity only the dominating
components are considered. Fusel oil which is a side product of ethanol
distilleries composes of various organics such as, methanol, ethyl acetate, n-
propanol, iso-butanol, ethyl butyrate, 2-butanol, iso-amyl alcohol, n butanol,
n-propanol and isopropanol. Iso-amyl alcohol is reported as the dominant
component for fusel oil. The growth conditions in the vessel are 30ºC
temperature and pH 4.5.
Fermenter Cooling
When designing a fermenter, one primary consideration is the removal Of
heat. There is a practical limit to the square feet of cooling surface that can
be achieved from a tank jacket and the number of coils that can be placed
inside the tank. The three sources of heat to be removed are from the cooling
of media after batch sterilization, from the exothermic fermentation process,
and the mechanical agitation.
The preceding topic about the design of a continuous sterilizer emphasized

reduced turnaround time, easier media sterilization, higher yields and one
speed agitator motors. The reduced turnaround time is realized because the
heat removal after broth sterilization is two to four times faster in a
continuous sterilizer than from a fermenter after batch sterilization. The
cooling section of a continuous sterilizer is a true countercurrent design.
Cooling a fermenter after batch sterilization is more similar to a co-current

heat exchanger. Assuming that all modem large scale industrial fermentation
plants sterilize media through a continuous sterilizer, the heat transfer
design of the fermenter is only concerned with the removal of heat caused
by the mechanical agitator (if there is one) and the heat of fermentation.
These data can be obtained while running a full-scale fermenter. The steps
are as follows:
1. Heat Loss by Convection and Radiation

a. u = 1.8 Btu/hr/F/ft2
(No insulation; if tank is insulated determine proper constant.)
b. Calculate tank surface area = A
c. Temp. of Broth = T1
d. Ambient Air Temp. = T2
Ql = UA (T1 – T2) = Btu/hr
Page | 31
Convection and radiation depend upon whether the tanks are

insulated or not, and the ambient air temperature, especially during
the winter. Measurements of convection and radiation heat losses
are, on average, 5% or less of total heat of fermentation (winter and
uninsulated tanks).
2. Heat Loss by Evaporation

a. If fermenters have level indicators, the average evaporation per
hour is easily determined.
b. Calculate pounds of water/hour evaporated from psychometric
charts based on the inlet volume and humidity of air used, and at
the broth temperature. The exhaust air will be saturated. Determine
heat of vaporization from steam tables at the temperature of the
broth = HEV = Btu/lb.
Q2 =HEV x (lb water evap/hr) = Btu/hr
Evaporation depends upon the relative humidity of the compressed
air, temperature of the fermentation broth and the aeration rate. It
is not uncommon that the loss of heat by evaporation is 15 to 25%
of the heat of fermentation. Modem plants first cool the compressed
air then reheat it to 70-80% relative humidity based on summertime
air intake conditions. Consequently, in winter the air temperature
and absolute humidity of raw air are very low and the sterile air
supply will be much lower in relative humidity than summer
conditions. Therefore, in the winter more water is evaporated from
the fermenters than in the summer. (Water can be added to the
fermenter or feeds can be made more dilute to keep the running
volume equal to summer conditions and productivity in summer and
winter equal).
3. Heat Removed by Refrigerant

a. This is determined by cooling the broth as rapidly as possible 5°F
below the normal running temperature and then shutting of fall
cooling. The time interval is then very carefully measured for the
broth to heat up to running temperature (AT and time).
b. Assume specific heat of broth = 1.0 Btu/lb-°F.
c. Volume of broth by level indicator (or best estimate) =gal
Q3 = Sp.Ht. x broth vol. x 8.345 x ΔT ÷ time (hr)
4. Heat Added by Mechanical Agitation

a. Determine or assume motor and gear box efficiency (about 0.92).
b. Measure kW of motor.
Q4 = kW x 3415 x efficiency = Btu/hr
5. Heat of Fermentation = ΔHF
Q1 + Q2 + Q3 - Q4 = ΔHF
Page | 32
The heat of fermentation is not constant during the course of the fermentation.
Peaks occur simultaneously with high metabolic activity. Commercial fermentation
is not constant during the course of the fermentation. Commercial fermentations
with a carbohydrate substrate may have peak loads of 120 Btu/hr/gal. The average
ΔHf for typical commercial fermentations is about 60 Btu/hr/gal. The average loss
of heat due to evaporation from aeration is in the range of 10 to 25 Btu/hr/gal.
Fermentations with a hydrocarbon substrate usually have a much higher ΔHf than
carbohydrate fermentations. Naturally, most companies determine the ΔHf for each
product, especially after each major medium revision. (Typically, data are collected
every eight hours throughout a run to observe the growth phase and production
phase. Three batches can be averaged for a reliable ΔHf.) In this manner, the
production department can give reliable data to the engineering department for
plant expansions.
If mechanical agitation is used and a jacket is desired, then additional internal coils
are required. The internal coils can be vertical, like baffles, or helical. Agitation
experts state that helical coils can be used with radial turbines if the spaces between
the coil loops are 1 to 1.5 pipe diameters. Once helical coils are accepted, Why use a
jacket at all? Reasons in favor of coils (in addition to the better heat transfer
coefficient) are:
1. Should stress corrosion cracking occur (due to chlorides in the cooling
water), the replacement of coils is cheaper than the tank wall and jacket.
2. The cost of a fermenter with helical coils is cheaper than a jacketed tank with
internal coils.
3. Structurally, internal coils present no problems with continuous
sterilization. However, if batch sterilization is insisted upon, vertical coils are
one solution to avoiding the stress between the coil supports and tank wall
created when cooling water enters the coils while the broth and tank wall
are at 120°C. Notice that the method of media sterilization, batch or
continuous, is related to the fermenter design and the capital cost.
2.8 Centrifugation
The solids-liquid separation process can be accomplished by filtration or
centrifugation. Centrifuges magnify the force of gravity to separate phases, solids
from liquids or one liquid from another. There are two general types of centrifuges
1. Sedimentation Centrifuges-where a heavy phase settles out from a lighter
phase, therefore requiring a density difference.
2. Filtering Centrifuges-where the solid phase is retained by a medium like a
filter cloth, for example, that allows the liquid phase to pass through.
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Figure 2-6 Disk-bowl centrifuge

Theory
Centrifuges operate on the principle that a mass spinning about a central axis at a
fixed distance is acted upon by a force. The force exerted on any mass is equivalent
to the, weight of the mass times its acceleration rate in the direction of the force.
Figure 2-7 Theory of centrifugation
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2.8.1 Biomass Separation (centrifuges) (F-011, F-012)

The fermentation broth from the fermenters is sent to centrifuge (S-1) to separate
the biomass from broth to be recycled to fermenters. The centrifuge S-2 is utilized
to remove the biomass from acid solution before being sent to fermentation.
Sedimentation type disc bowl centrifuges are widely used in industry for this
purpose.
The performance of the sedimentation centrifuges are described by sigma factor (Σ)
which is equal to the cross-sectional area of sedimentation tank giving the same
clarification. the disc type centrifuges proved to be more suitable for this operation.
2.8.2 Yeast sterilization Tank (A-011)

The cell culture should be kept at low pH conditions, to prevent any microbial
contamination in yeast culture during the recycling process. For this purpose, cells
are separated from the fermentation broth by means of continuous centrifugation,
transferred into stirred vessels and sulfuric acid solution is added into vessel to
lower the pH to 2. Approximately 13 g or sulfuric acid is required per kg of ethanol
produced. The cell flow rate is 172 m3/h. The ethanol flow out of the fermenter is
39.4 Mt/h therefore the required sulfuric acid is 512 kg/h. The required acid will
be 694 m3/h. using the residence time of 15 minutes the required vessel volume is
calculated as 190 m3 including 10% safety.
2.8.3 Ethanol Purification

Ethanol Scrubber (S-012)
The ethanol scrubber is utilized to absorb the evaporated ethanol from the carbon
dioxide effluent of the fermentation and top product of beer column. The
environmental regulations limit the emission of volatile organics to atmosphere
with total of 36.4 ton/year. This is why the ethanol scrubber is designed
accordingly.
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CHAPTER 3: DISTILLATION AND DEHYDRATION
3 CHAPTER 3: DISTILLATION AND DEHYDRATION
3.1 INTRODUCTION
The separation of liquid mixtures into their various components is one of the major
operations in the process industries, and distillation, the most widely used method
of achieving this end, is the key operation in any oil refinery. In processing, the
demand for purer products, coupled with the need for greater efficiency, has
promoted continued research into the techniques of distillation. In engineering
terms, distillation columns have to be designed with a larger range in capacity than
any other types of processing equipment, with single columns 0.3–10 m in diameter
and 3–75 m in height. Designers are required to achieve the desired product quality
at minimum cost and also to provide constant purity of product even though there
may be variations in feed composition. A distillation unit should be considered
together with its associated control system, and it is often operated in association
with several other separate units. The vertical cylindrical column provides, in a
compact form and with the minimum of ground requirements, a large number of
separate stages of vaporization and condensation. In this chapter the basic
problems of design are considered, and it may be seen that not only the physical and
chemical properties, but also the fluid dynamics inside the unit, determine the
number of stages required and the overall layout of the unit.
Figure 3-1 Distillation unit
The separation of ethanol from a mixture with water, for example, requires only a
simple single unit, and virtually pure products may be obtained. A more complex
arrangement where the columns for the purification of crude styrene formed by the
dehydrogenation of ethyl benzene are. It may be seen that, in this case, several
columns are required and that it is necessary to recycle some of the streams to the
reactor.
In this chapter consideration is given to the theory of the process, methods of

distillation and calculation of the number of stages required for both binary system,
and discussion on design methods is included for plate and packed columns
incorporating a variety of column internals.
Page | 36
3.2 Distillation terminology

To provide a better understanding of the distillation process, the following briefly
explains the terminology most often encountered.
SOLVENT RECOVERY
The term “solvent recovery” often has been a somewhat vague label applied
to the many different ways in which solvents can be reclaimed by industry.
One approach employed in the printing and coatings industries is merely to
take impure solvents containing both soluble and insoluble particles and
evaporate the solvent from the solids. For a duty of this type, APV offers the
Para flash evaporator, a compact unit which combines a Para flow plate heat
exchanger and a small separator. As the solvent laden liquid is recirculated
through the heat exchanger, it is evaporated, and the vapor and liquid are
separated. This will recover a solvent, but it will not separate solvents if two
or more are present.
Another technique is available to handle an air stream that carries solvents.

By chilling the air by means of vent condensers or refrigeration equipment,
the solvents can be removed from the air stream.
Solvents also can be recovered by using extraction, adsorption, absorption

and distillation methods.
SOLVENT EXTRACTION
Essentially a liquid/liquid process where one liquid is used to extract
another from a secondary stream, solvent extraction generally is performed
in a column somewhat similar to a normal distillation column. The primary
difference is that the process involves the mass transfer between two liquids
instead of a liquid and a vapor. During the process, the lighter (i.e., less
dense) liquid is charged to the base of the column and rises through packing
or trays while the denser liquid descends.
Mass transfer occurs and one or more components is extracted from one
stream and passed to the other.
Liquid/liquid extraction sometimes is used when the breaking of an

azeotrope is difficult or impossible by distillation techniques.
CARBON ADSORPTION
The carbon adsorption technique is used primarily to recover solvents from
dilute air or gas streams. In principle, a solvent laden air stream is passed
over activated carbon and the solvent is adsorbed into the carbon bed. When
the bed becomes saturated, steam is used to desorb the solvent and carry it
Page | 37
to a condenser. In such cases as toluene, for example, recovery of the solvent

can be achieved simply by decanting the water/solvent two phase mixture
which forms in the condensate.
Carbon adsorption beds normally are used in pairs so that the air flow can
be diverted to the secondary bed when required.
On occasion, the condensate is in the form of a moderately dilute miscible

mixture. In this case, the solvent must be recovered by distillation. This
would apply especially to water miscible solvents such as acetone.
ABSORPTION
When carbon adsorption cannot be used because certain solvents either
poison the activated carbon bed or create so much heat that the bed can
ignite, absorption offers an alternate technique. Solvent is recovered by
pumping the solvent laden air stream through a column counter currently
to a water stream, which absorbs the solvent. The air from the top of the
column essentially is solvent free, while the dilute water/solvent stream
discharged from the column bottom usually is concentrated in a distillation
column. Absorption also can be applied in cases where an oil rather than
water is used to absorb certain organic solvents from the air stream.
AZEOTROPES
During distillation, some components form an azeotrope at a certain stage of
the fractionation, requiring a third component to break the azeotrope and
achieve a higher percentage of concentration. In the case of ethyl alcohol and
water, for example, a boiling mixture containing less than 96% by weight
ethyl alcohol produces a vapor richer in alcohol than in water and is readily
distilled. At the 96% by weight point, however, the ethyl alcohol composition
in the vapor remains constant (i.e., the same composition as the boiling
liquid). This is known as the azeotrope composition and further
concentration requires use of a process known as azeotropic distillation.
Other common fluid mixtures which for azeotropes are formic acid/water,
isopropyl alcohol/water, and iso butanol/water.
AZEOTROPIC DISTILLATION
In a typical azeotropic distillation procedure, a third component, such as
benzene, isopropyl ether or cyclohexane, is added to an azeotropic mixture,
such as ethyl alcohol/water, to form a ternary azeotrope. Since the ternary
azeotrope is richer in water than the binary ethyl alcohol/water azeotrope,
water is carried over the top of the column. The ternary azeotrope, when
condensed, forms two phases. The organic phase is refluxed to the column
while the aqueous phase is discharged to a third column for recovery of the
Page | 38
entraining agent. Certain azeotropes such as the n-butanol/water mixture

can be separated in a two-column system without the use of a third
component. When condensed and decanted, this type of azeotrope forms
two phases. The organic phase is fed back to the primary column and the
butanol is recovered from the bottom of the still. The aqueous phase,
meanwhile, is charged to the second column with the water being taken from
the column bottom. The vapor streams from the top of both columns are
condensed and the condensates run to a common decanter.
EXTRACTIVE DISTILLATION
This technique is somewhat similar to azeotropic distillation in that it is
designed to perform the same type of task. In azeotropic distillation, the
azeotrope is broken by carrying over a ternary azeotrope at the top of the
column. In extractive distillation, a higher boiling compound is added and
the solvent to be recovered is pulled down the column and removed as the
bottom product. A further distillation step is then required to separate the
solvent from the entraining agent.
STRIPPING
In distillation terminology, stripping refers to the removal of a volatile
component from a less volatile substance. Again, referring to the ethyl
alcohol/water system, stripping is done in the column below the feed point,
where the alcohol enters at about 10% by weight and the resulting liquid
from the column base contains less than 0.02% alcohol by weight. This is
known as the stripping section of the column. This technique does not
increase the concentration of the more volatile component, but rather
decreases its concentration in the less volatile component.
A stripping column also can be used when a liquid such as water

contaminated by toluene cannot be discharged to sewer. For this pure
stripping duty, the toluene is removed within the column, while vapor from
the top is decanted for residual toluene recovery and refluxing of the
aqueous phase.
RECTIFICATION
For rectification or concentration of the more volatile component, the top
section of a column above the feed point is required. By means of a series of
trays and with reflux back to the top of the column, a solvent such as ethyl
alcohol can be concentrated to over 95% by weight.
Page | 39
BATCH DISTILLATION
When particularly complex or small operations require recovery of the
more volatile component, APV can offer batch distillation systems of various
capacities.
Essentially a rectification type process, batch distillation involves pumping

a batch of liquid feed into a tank where boiling occurs. Vapor rising through
a column above the tank combines with reflux coming down the column to
effect concentration. This approach is not too effective for purifying the less
volatile component since there is only the equivalent of one stripping stage.
For many applications, batch distillation requires considerable operator

intervention or alternatively, a significant amount of control
instrumentation. While a batch system is more energy intensive than a
continuous system, steam costs generally are less significant on a small
operation. Furthermore, it is highly flexible, and a single batch column can
be used to recover many different solvents.
CONTINUOUS DISTILLATION
The most common form of distillation used by the chemical, petroleum and
petrochemical industries is the continuous mode system. In continuous
distillation, feed constantly is charged to the column at a point between the
top and bottom sections. The section above the feed point rectifies or
purifies the more volatile component while the column section below the
feed point strips out the more volatile from the less volatile component. In
order to separate N components with continuous distillation, a minimum of
N-1 distillation columns is required.
Side draws can be taken to remove extra streams from the column but only
when high purity of individual components is not required.
TURNDOWN
The turndown ratio of a column is an indication of the operating flexibility.
If a column, for example, has a turndown ratio of 3, it means that the column
can be operated efficiently at 33% of the maximum design throughput.
STEAM STRIPPING
The term steam stripping can be applied to any system where rising steam
vapors in a column strip out the volatile components in the liquid. In
particular, the term is applied to systems where steam is used to strip out
partially miscible organic chemicals, even though the organic chemicals have
boiling points above water.
Page | 40
3.3 Types of Distillation

3.3.1 Simple Distillation
▪ Simple distillation involves heating the liquid mixture to the boiling point
and immediately condensing the resulting vapors.
▪ This method is only effective for mixtures wherein the boiling points of the
liquids are considerably different (a minimum difference of 25oC).
▪ The purity of the distillate (the purified liquid) is governed by Raoult’s law.
3.3.2 Fractional Distillation

Fractional distillation is often used to separate mixtures of liquids that have similar
boiling points. It involves several vaporization-condensation steps (which takes
place in a fractioning column). This process is also known as rectification. The
apparatus required to perform a fractional distillation on a mixture is listed below.
▪ Round-bottom flask or distilling flask.

▪ A source of heat, which can be a fire or
a hot bath.
▪ Receiving flask to collect the
condensed vapors.
▪ Fractioning column.
▪ Thermometer to measure the
temperature in the distilling flask.
▪ Condenser.
▪ Standard Glassware.
When heated, the liquid mixture is converted

into vapors that rise into the fractioning
column. The vapors now cool and condense on
the walls of the condenser. The hot vapors Figure 3-2 Fractional column
emanating from the distilling flask now heat the

condensed vapor, creating new vapors.
Many such vaporization-condensation cycles take place and the purity of the
distillate improves with every cycle. An illustration depicting a fractional distillation
setup is provided below.
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3.3.3 Steam Distillation

▪ Steam distillation is often used to separate heat-sensitive components in a
mixture.
▪ This is done by passing steam through the mixture (which is slightly
heated) to vaporize some of it. The process establishes a high heat-transfer
rate without the need for high temperatures.
▪ The resulting vapor is condensed to afford the required distillate.
▪ The process of steam distillation is used to obtain essential oils and herbal
distillates from several aromatic flowers/herbs.
Figure 3-3 Steam distillation
3.3.4 Vacuum Distillation

▪ Vacuum distillation is ideal for separating mixtures of liquids with very
high boiling points.
▪ In order to boil these compounds, heating to high temperatures is an
inefficient method. Therefore, the pressure of the surroundings is lowered
instead.
▪ The lowering of the pressure enables the component to boil at lower
temperatures. Once the vapor pressure of the component is equal to the
surrounding pressure, it is converted into a vapor.
▪ These vapors are then condensed and collected as the distillate. The
vacuum distillation method is also used to obtain high-purity samples of
compounds that decompose at high temperatures.
Page | 42
Figure 3-4 Schematic drawing of vacuum distillation
3.3.5 Azeotropic Distillation

The separation of a mixture of components can be based on several routes and
realized in different technical applications. Among them, the unit operation
“distillation” is the most common one. The separation is achieved by different
vapor pressures of the pure compounds and/or their activity coefficients. This
information is condensed in the separation factor. The driving force of the process
is the conversion of exergy to energy (i.e., the energy delivered at the sump of the
distillation column is always at a higher level than the energy retrieved at the top of
the distillation column). For narrow-boiling or even azeotropic systems, the
purification is hardly or even not possible. In such a case, three well-established
methods for modifying the equilibrium to allow obtaining pure products are
considered first: (1) varying the pressure between two columns (pressure swing
distillation), (2) adding an additional compound to influence the activity
coefficients, or (3) forming a better suited multicomponent azeotropic point
(azeotropic distillation). Another choice would be to use so-called hybrid processes,
which are arranged by combining distillation with other separation methods
capable of breaking the azeotrope, like adsorption (distillation and molecular
sieves) or pervaporation (distillation and membranes).
Page | 43
Many binary mixtures exhibit azeotropic behavior. That is, at a certain composition
known as the azeotrope point, the vapor composition over the boiling liquid is
exactly the same as the liquid. In other words, the azeotropic mixture of two or more
components behaves, during the distillation process, the same as a pure component.
As a result, simple distillation will not separate the components. A typical azeotrope
is a 96% w/w mixture of ethanol in water. To separate an azeotrope, it is necessary
to change some conditions that will affect either relative volatilities or
compositions. At APV, three different distillation techniques have been used to
break azeotropic systems. Azeotropes also can be broken with membrane systems
as well as molecular sieves. Membranes operating as pervaporation systems have
found a limited number of applications for the removal of water from isopropyl
alcohol, while molecular sieves have been used for the removal of water from
ethanol/water mixtures.
Azeotropic Distillation with an Entraining Agent

The most common form of azeotropic distillation is adding a third
component to the azeotropic mixture in a distillation column. This third
component essentially changes the vapor/liquid relationship between the
two components and allows separation. Using ethanol/water as the
example, the column is usually operated with a continuous feed of the
azeotrope into the column, which contains the third component. This causes
a ternary azeotrope to form in the vapor at the top of the column. When this
Figure 3-5 Azeotropic distillation for the separation of ethanol from water using benzene as entrainer.
Page | 44
vapor is condensed, the condensate splits into two liquid phases. The organic
layer is pumped back to the top of the column as reflux. The aqueous layer is
pumped to a smaller third column where the entertainer is recovered and
pumped back to the dehydration column. Thus, the entertainer is
continuously recycled, and losses are low. In the base of the dehydration
column, the entertainer is removed from the ethanol to give high purity
ethanol as the base product. The process for the removal of water from the
isopropyl alcohol/water azeotrope is essentially the same.
Many ethyl alcohol systems involve processing a feed of about 10% w/w
ethyl alcohol. This is concentrated to 93% w/w in a binary column, followed
by a concentration step to over 99% w/w in the azeotropic column. A flow
sheet for a typical system is shown in Figure 3-5.
On these systems, the two larger columns are often operated at different
pressures so that the vapor from one column can be used as the heating
medium for the reboiler of the second column, which operates at a lower
pressure.
Azeotropic Distillation Without an Entraining Agent

Certain binary systems form vapor azeotropes that, when condensed, form
a two-phase liquid without the presence of a third component. The
separation is achieved with the combination of an organic column and an
aqueous column coupled with a decanter. This is shown schematically in
Figure 3-6.
Figure 3-6 Azeotropic Distillation Without an Entraining Agent
Page | 45
The vapors from each column are condensed, and the resulting two-phase
liquids are combined and decanted in a single vessel. The organic phase is
returned as reflux to the organic column and the aqueous phase is returned
as reflux to the aqueous column. The feed should enter the columns at a point
that corresponds most closely to its composition. If the feed is at or close to
the azeotrope, the feed point can be the decanter. In this process, the high
purity products, which are usually water and organic, are removed from the
base of the two columns. APV has supplied this type of design for the
dehydration of butyl alcohol and cyclohexanone.
Azeotropic Distillation Using Pressure Swings

Some azeotropic mixtures can be separated by changing the operating
pressure of the column. This applies to those systems where the azeotropic
composition is significantly affected by the operating pressure. APV has used
this technique to separate the methyl ethyl ketone (MEK)/water system. In
the process, the product is processed in the first column at atmospheric
pressure to remove the azeotrope as a distillate. The azeotrope at 89% w/w
is then pumped to a second column which operates at 74 psia (5 bar a). At
this pressure, the azeotropic composition is at about 83% w/w, which is
substantially lower than the feed composition. Therefore, it is possible to
remove dehydrated MEK from the column bottom and take an azeotrope
distillate at about 83% w/w from the top. This azeotrope is then recycled
back to the first column. Since the columns are operated at different
pressures and temperatures, it is possible to economize on energy by using
vapor from the higher-pressure column as the heat source for the lower
pressure reboiler.
Figure 3-7 Azeotropic Distillation Using Pressure

Swings
Page | 46
3.4 System components

The following descriptions briefly define the many components required for a
distillation system, as well as the many variations in components that are available
to meet different process conditions.
3.4.1 Column shells

A distillation column shell can be designed for use as a free-standing module or for
installation within a supporting steel structure. Generally speaking, a self-
supporting column is more economical at diameters of 4 ft (1.2m) or larger.
This holds true even under extreme seismic-3 conditions. APV has built distillation
columns in carbon steel, 304 stainless steel, 316 stainless steel, Monel, titanium,
Hastelloy C and Incoloy 825. Usually, it is more economical to fabricate columns in
a single piece without shell flanges.
This technique not only simplifies installation but also reduces the danger of
leakage during operation. Columns over 80 ft (24m) in length have been shipped by
road without transit problems.
While columns of over 3 ft (0.9m) in diameter normally have been transported

without trays to prevent dislodgment and possible damage, recent and more
economical techniques have been devised for factory installation of trays with the
tray manways omitted. After the column has been erected, manways are added and,
at the same time, the fitter inspects each tray.
With packed columns of 24 inch (600 mm) diameter or less which may use high
efficiency sheet metal or mesh packing, the packing can be installed prior to
shipment. Job site packing installation, however, is the norm for larger columns.
This prevents the packing from bedding down during transit and leaving voids that
would reduce operating efficiency.
Random packing always is installed after delivery, except for those rare occasions
when a column can be shipped in a vertical position.
Access platforms and interconnecting ladders designed to OSHA standards also are
supplied for on site attachment to free-standing columns.
Installation usually is quite simple since columns are fitted with lifting lugs. At the
fabrication stage, a template is drilled to match support holes in the column base
ring. With these exact template dimensions, supporting bolts can be preset for quick
and accurate coupling as the column is lowered into place.
Page | 47
3.4.2 Column internals

During recent years, the development of sophisticated computer programs and new
materials has led to many innovations in the design of trays and packings for more
efficient operation of distillation columns. In designing systems for chemical,
petroleum and petrochemical use, APV specialists take full advantage of available
internals to assure optimum distillation performance.
Tray devices
While there are perhaps five basic distillation trays suitable for industrial use, there
are many design variations of differing degrees of importance and a confusing array
of trade names applied to their products by tray manufacturers. The most modern
and commonly used devices include sieve, valve, bubble cap, dual flow, and baffle
trays – each with its advantages and preferred usage. Of these, the sieve and valve
type trays currently are most often specified. For a better understanding of tray
design, Figure 3-8 defines and locates typical tray components. The material of
construction usually is 14 gauge with modern trays adopting the integral truss
design which simplifies fabrication. A typical truss tray is shown in Figure 3-9. For
columns less than 3 ft (0.9m) in diameter, it is not possible to assemble the truss
trays in the column; therefore, trays must be preassembled on rods into a cartridge
section for loading into the column. Figure 3-10 shows this arrangement in scale
model size. The hydraulic design of a tray is a very important factor. The upper
operating limit generally is governed by the flood point, although in some cases,
entrainment also can restrict performance before the onset of flooding. Flooding is
usually caused by either massive entrainment, termed jet flooding, or by
downcomer back-up.
Figure 3-9 Sieve tray
Figure 3-8 Tray column Figure 3-10 Tray column
Page | 48
Down comer back-up occurs when a tray design provides insufficient down comer
area to allow for the liquid flow or when the pressure drop across the tray is high,
which forces liquid to back up in the down comer. When the down comer is unable
to handle all the liquid involved, the trays start to fill and pressure drop across the
column increases. This also can occur when a highly foaming liquid is involved.
Flooding associated with high tray pressure drops and small tray spacing takes
place when the required liquid seal is higher than the tray spacing. Down comer
design also is particularly important at high operating pressure due to a reduction
in the difference between vapor and liquid densities.
The lower limit of tray operation, meanwhile, is influenced by the amount of liquid
weeping from one tray to the next. Unlike the upward force of entrainment, weeping
liquid flows in the normal direction and considerable amounts can be tolerated
before column efficiency is significantly affected. As the vapor rate decreases,
however, a point eventually is reached when all the liquid is weeping and there is
no liquid seal on the tray. This is known as the dump point, below which there is a
severe drop in efficiency.
SIEVE TRAY
The sieve tray is a low-cost device which consists of a perforated plate that
usually has holes of 3/16 inch to 1 inch (5 to 25mm) diameter, a down comer,
and an outlet weir. Although inexpensive, a correctly designed sieve tray can
be comparable to other styles in vapor and liquid capacities, pressure drop
and efficiency. For flexibility, however, it is inferior to valve and bubble cap
trays. It is also sometimes unacceptable for low liquid loads when weeping
has to be minimized.
Depending on process conditions, tray spacing, and allowable pressure drop,

the turndown ratio of a sieve tray can vary from 1.5 to 2, and occasionally
higher. For many applications, a turndown of 1.5 is acceptable. It also is
possible to increase the flexibility of a sieve tray for occasional low
throughput operation by maintaining a high vapor boil up and increasing the
reflux ratio. This may be economically desirable when the low throughput
occurs for a small fraction of the operating time. Flexibility, likewise, can be
increased by the use of blanking plates to reduce the hole area. This is
particularly useful for initial operation when it is proposed to increase the
plant capacity after a few years. There is no evidence to suggest that blanked-
off plates have inferior performance to unbanked plates of similar hole area.
Page | 49
Dual flow tray

The dual flow tray is a high hole area sieve tray without a down comer. The
liquid passes down the same holes through which the vapor rises. Since no
down comer is used, the cost of the tray is lower than that of a conventional
sieve tray. In addition, the less complex design allows for easier cleaning. In
recent years, use of the dual flow tray has declined somewhat because of
difficulties experienced with partial liquid/vapor bypassing of the two
phases, particularly in larger diameter columns. The dual flow column also
has a very restricted operating range and a reduced efficiency because there
is no crossflow of liquid.
Figure 3-11 Dual flow tray
Valve tray
While the valve tray dates back to the rivet type first used in 1922, many
design improvements and innumerable valve types have been introduced in
recent years. Two types of valves are illustrated in Figure 3-11. These valves
provide the following advantages:
1. Throughputs and efficiencies can be as high as sieve or bubble cap
trays.
2. Very high flexibility can be achieved and turndown ratios of 4 to 1 can
be obtained without having to resort to large pressure drops at the
high end of the operating range.
3. Special valve designs with venturi shaped orifices are available for
duties involving low pressure drops.
4. Although slightly more expensive than sieve trays, the valve tray is
economical in view of its numerous advantages.
5. Since an operating valve is continuously in movement, the valve tray
can be used for light to moderate fouling duties.
APV has successfully used valve trays on brewery effluent containing waste
beer, yeast and other materials with fouling tendencies.
Page | 50
Figure 3-12 Valve tray
Bubble cap tray

Although many bubble cap columns still are in operation, bubble cap trays
rarely are specified today because of high cost factors and the excellent
performance o the modern valve tray. The bubble cap, however, does have a
good turndown ratio and is good for low liquid loads.
Figure 3-13 Bubble cap tray
BAFFLE TRAY
Baffle trays are arranged in a tower in such a manner that the liquid flows
down the column by splashing from one baffle to the next tower baffle. The
ascending gas or vapor, meanwhile, passes through this “curtain” of liquid
spray. Although the baffle tray has a low efficiency, it can be useful in
applications when the liquid contains a high fraction of solids.
Page | 51
Packings
For many types of duties, particularly those involving small diameter columns,
packing is the most economical tower internal. One advantage is that most packing
can be purchased from stock on a volumetric basis. In addition, the mechanical
design and fabrication of a packed column is quite simple. Disadvantages of packing
include its unsuitability for fouling duties, breakage of ceramic packing, and in APV
experience, less predictive performance, particularly at low liquid loads or high
column diameters. The most widely used packing is the random packing, usually
Raschig Rings, Pall Rings and ceramic saddles. These are available in various
plastics, a number of different metals and, with the exception of Pall Rings, in
ceramic materials. While packings in plastic have the advantage of corrosion
resistance, the self-wetting ability of some plastic packing such as fluorocarbon
polymers sometimes is poor, particularly in aqueous systems. This considerably
increases the HETP when compared with equivalent ceramic rings. Structured high
efficiency packings have become more available in the last 20 years. These packings,
which are usually made of corrugated gauze or sheet metal, can provide better
efficiency than random packing, but at a higher cost. The gauze packings can
provide an HETP of 8 to 10 in (200 to 250mm) for organic systems.
A sample of gauze packing is shown in Figure 3-14. The sheet metal packings
usually have an HETP in the range of 18 to 22 in (450mm to 550mm) but are far
less expensive than the gauze. These types of packing are good at maintaining
distribution of the liquid. With both random and, in particular, high efficiency
packing, considerable attention must be given to correct liquid and vapor
distribution. Positioning of the vapor inlets and the design of liquid distributors and
redistributors are important factors that should be designed only by experts.
Figure 3-14 Packings
Page | 52
Table 3-2 Comparison of performance characteristics of common tray type, random and structured packing
Table 3-1 Comparison of three types of cross flow tray
3.4.3 Auxiliary equipment

In any distillation system, the design of auxiliary equipment such as the reboiler,
condenser, preheaters and product coolers is as important as the design of the
column itself.
REBOILER
Although there are many types of reboilers, the shell and tube thermosyphon
reboiler is used most frequently. Boiling within the vertical tubes of the
exchanger produces liquid circulation and eliminates the need for a pump. A
typical arrangement is shown in Figure 3-15.
For certain duties, particularly when the bottoms liquid has a tendency to
foul heat transfer surfaces, it is desirable to pump the liquid through a forced
circulation reboiler. Since boiling can be suppressed by use of an orifice plate
at the outlet of the unit, fouling is reduced. The liquid being pumped is heated
under pressure and then is flashed into the base of the column where vapor
is generated.
Page | 53
An alternate approach is the use of a plate heat exchanger as a forced

circulation reboiler.
With this technique, the very high liquid turbulent flow which is induced
within the heat exchanger through the use of multiple corrugated plates
holds fouling to a minimum. Meanwhile, the superior rates of heat transfer
that are achieved reduces the surface area required for the reboiler.
Figure 3-16 Kettle type reboiler
Figure 3-15 Vertical reboiler
Figure 3-17 Internal reboiler

CONDENSERS
Since most distillation column condensers are of shell and tube design, the
processor has the option of condensing on either the shell or tube side. From
the process point of view, condensation on the shell side is preferred since
there is less subcooling of condensate and a lower pressure drop is required.
These are important factors in vacuum duties. Furthermore, with cooling
water on the shell side, any fouling can be removed more easily. Tube side
condensation, on the other hand, can be more advantageous whenever
process fluid characteristics dictate the use of more expensive, exotic
materials. Capital cost of the unit can be reduced by using a carbon steel
shell.
PREHEATERS/COOLERS
The degree to which fluids are aggressive to metals and gasketing materials
generally determines the selection of plate or shell and tube preheaters and
product coolers. If fluids are not overly aggressive toward gasket materials,
a plate heat exchanger is an extremely efficient preheater since a very close
temperature approach may be achieved. Added economy is realized by using
heat from the top and bottoms product for all necessary preheating.
Page | 54
While plate type units can be supplied with fluorocarbon gaskets, very
aggressive duties normally are handled in a number of tubular exchangers
arranged in series to generate a good mean temperature difference. The use
of multiple tubular units is more expensive than a single plate heat
exchanger but is unavoidable for certain solutions such as aromatic
compounds.
One technique that makes use of the plate heat exchanger with gasket
aggressive fluids is a welded plate pair. In this case, one of the fluids is
contained between a pair of plates that are laser welded. Since the ‘O’ ring
gaskets around the ports on the non-welded plates can be supplied in PTFE,
it is possible to handle the aggressive fluid. However, this is only possible on
one side of the exchanger, so the second fluid must be free of aggressive
fluids. This is often the type of duty that is required for a waste water steam
stripper where the organics are stripped out of the contaminated feed, and
are no longer present in the hot bottoms product.
VENT CONDENSERS
It is normal practice on distillation systems to use a vent condenser after
the main condenser to minimize the amount of volatiles being driven off
into the atmosphere.
Usually of the shell and tube type, the vent condenser will have about one-
tenth the area of the main unit. The vent condenser will utilize a colder
cooling medium than that of the main condenser to cool the non-
condensable gases to about 50°F (10°C).
Figure 3-18 Vent condenser
PUMPS
Since most distillation duties involve fluids that are highly flammable and
have a low flash point, it is often essential that explosion-proof (Class 1,
Group D, Division 1) pump motors be supplied. Centrifugal pumps generally
are specified since they are reliable and can provide the necessary head and
volumetric capacity at moderate costs.
For environmental purposes, it is often necessary to supply a pressurized oil

seal pot with the oil recirculated around the pump, as well as a pumping ring
inside the seal itself to minimize the leaking of the process fluid into the
environment. These are extremely expensive, but often necessary, seals.
Page | 55
3.5 The fractionating column design

3.5.1 The fractionating process
The operation of a typical fractionating column may be followed by reference to
Figure 3-19. The column consists of a cylindrical structure divided into sections by
a series of perforated trays which permit the upward flow of vapour. The liquid
reflux flows across each tray, over a weir and down a down comer to the tray below.
The vapour rising from the top tray passes to a condenser and then through an
accumulator or reflux drum and a reflux divider, where part is withdrawn as the
overhead product D, and the remainder is returned to the top tray as reflux R.
The liquid in the base of the column is frequently heated, either by condensing
steam or by a hot oil stream, and the vapour rises through the perforations to the
bottom tray.
Figure 3-19 Fractional distillation column
A more commonly used arrangement with an external reboiler is shown in Figure

3-19 where the liquid from the still passes into the reboiler where it flows over the
tubes and weir and leaves as the bottom product by way of a bottom’s cooler, which
preheats the incoming feed. The vapour generated in the reboiler is returned to the
bottom of the column with a composition ys , and enters the bottom tray where it is
partially condensed and then revalorized to give vapor of composition y1.
Page | 56
This operation of partial condensation of the rising vapour and partial vaporisation
of the reflux liquid is repeated on each tray. Vapour of composition yt from the top
tray is condensed to give the top product D and the reflux R, both of the same
composition yt . The feed stream is introduced on some intermediate tray where
the liquid has approximately the same composition as the feed. The part of the
column above the feed point is known as the rectifying section and the lower
portion is known as the stripping section. The vapour rising from an ideal tray will
be in equilibrium with the liquid leaving, although in practice a smaller degree of
enrichment will occur.
In analyzing the operation on each tray, it is important to note that the vapour rising
to it, and the reflux flowing down to it, are not in equilibrium, and adequate rates of
mass and heat transfer are essential for the proper functioning of the tray.
The tray as described is known as a sieve tray and it has perforations of up to about
12 mm diameter, although there are several alternative arrangements for
promoting mass transfer on the tray, such as valve units, bubble caps. In all cases
the aim is to promote good mixing of vapour and liquid with
a low drop in pressure across the tray.
On each tray the system tends to reach equilibrium because:

a. Some of the less volatile component condenses from the rising
vapour into the liquid thus increasing the concentration of the more
volatile component (MVC) in the vapor.
b. Some of the MVC is vaporized from the liquid on the tray thus
decreasing the concentration of the MVC in the liquid.
The number of molecules passing in each direction from vapour to liquid and in
reverse is approximately the same since the heat given out by one mole of the
vapour on condensing is approximately equal to the heat required to vaporize one
mole of the liquid. The problem is thus one of equimolecular counter diffusion. If
the molar heats of vaporization are approximately constant, the flows of liquid and
vapour in each part of the column will not vary from tray to tray. This is the concept
of constant molar overflow which is discussed under the heat balance. Conditions
of varying molar overflow, arising from unequal molar latent heats of the
components.
In the arrangement discussed, the feed is introduced continuously to the column

and two product streams are obtained, one at the top much richer than the feed in
the MVC and the second from the base of the column weaker in the MVC. For the
separation of small quantities of mixtures, a batch still may be used. Here the
column rises directly from a large drum which acts as the still and reboiler and holds
the charge of feed. The trays in the column form a rectifying column and distillation
is continued until it is no longer possible to obtain the desired product quality from
the column. The concentration of the MVC steadily falls in the liquid remaining in
the still so that enrichment to the desired level of the MVC is not possible.
Page | 57
A complete unit will normally consist of a feed tank, a feed heater, a column with
boiler, a condenser, an arrangement for returning part of the condensed liquid as
reflux, and coolers to cool the two products before passing them to storage. The
reflux liquor may be allowed to flow back by gravity to the top plate of the column
or, as in larger units, it is run back to a drum from which it is pumped to the top of
the column. The control of the reflux on very small units is conveniently affected by
hand-operated valves, and with the larger units by adjusting the delivery from a
pump. In many cases the reflux is divided by means of an electromagnetically
operated device which diverts the top product either to the product line or to the
reflux line for controlled time intervals.
3.5.2 Number of plates required in a distillation column

In order to develop a method for the design of distillation units to give the desired
fractionation, it is necessary, in the first instance, to develop an analytical approach
which enables the necessary number of trays to be calculated. First the heat and
material flows over the trays, the condenser, and the reboiler must be established.
Thermodynamic data are required to establish how much mass transfer is needed
to establish equilibrium between the streams leaving each tray. The required
diameter of the column will be dictated by the necessity to accommodate the
desired flowrates, to operate within the available drop in pressure, while at the
same time effecting the desired degree of mixing of the streams on each tray.
Four streams are involved in the transfer of heat and material across a plate, as
shown in Figure in which plate n receives liquid Ln+1 from plate n + 1 above, and
vapour Vn−1 from plate n − 1 below. Plate n supplies liquid Ln to plate n − 1, and
vapour Vn to plate n + 1. The action of the plate is to bring about mixing so that the
vapour Vn, of composition yn, approaches equilibrium with the liquid Ln, of
composition xn. The streams Ln+1 and Vn−1 cannot be in equilibrium and, during the
interchange process on the plate, some of the more volatile component is vaporised
from the liquid Ln+1, decreasing its concentration to xn, and some of the less volatile
component is condensed from Vn−1, increasing the vapour concentration to yn. The
heat required to vaporise the more volatile component from the liquid is supplied
by partial condensation of the vapour Vn−1. Thus, the resulting effect is that the more
volatile component is passed from the liquid running down the column to the
vapour rising up, whilst the less volatile component is transferred in the opposite
direction.
Page | 58
Heat balance over a plate

A heat balance across plate n may be written as:
L(n+1) * HL(n+1) + HV(n−1) * HV(n−1) = V(n) * HV(n) + L(n) * HL(n) + losses + heat of mixing
where: HL(n) is the enthalpy per mole of the liquid on plate n, and HV(n) is the enthalpy
per mole of the vapour rising from plate n. This equation is difficult to handle for
the majority of mixtures, and some simplifying assumptions are usually made. Thus,
with good lagging, the heat losses will be small and may be neglected, and for an
ideal system the heat of mixing is zero. For such mixtures, the molar heat of
vaporization may be taken as constant and independent of the composition. Thus,
one mole of vapour V(n−1) on condensing releases sufficient heat to liberate one mole
of vapour V(n). It follows that V(n) = V(n−1), so that the molar vapour flow is constant
up the column unless material enters or is withdrawn from the section. The
temperature changes from one plate to the next will be small, and HL(n) may be taken
as equal to HL(n+1).
Applying these simplifications to equation, it is seen that L(n) = L(n+1) so that the
moles of liquid reflux are also constant in this section of the column. Thus V(n) and
L(n) are constant over the rectifying section, and V(m) and L(m) are constant over the
stripping section.
For these conditions there are two basic methods for determining the number of
plates required. The first is due to SOREL and later modified by LEWIS
Page | 59
Operating line using the Lewis–Sorel method (Analytical)

If a unit is operating as shown in Figure 3-20 so that a binary feed F is distilled to
give a top product D and a bottom product W, with xf , xd, and xw as the
corresponding mole fractions of the more volatile component, and the vapour Vt
rising from the top plate is condensed, and part is run back as liquid at its boiling
point to the column as reflux, the remainder being withdrawn as product, then a
material balance above plate n, indicated by the loop I in Figure gives:
V(n) = L(n+1) + D
Figure 3-20 Mass balance a cross distillation column
Figure Material balances at top and bottom of column Expressing this balance for
the more volatile component gives:
y(n) * V(n) = L(n+1) * x(n+1) + D * xd

Thus: y(n) = L(n+1) * x(n+1) / V(n) + D * xd / V(n)
This equation relates the composition of the vapour rising to the plate to the
composition of the liquid on any plate above the feed plate. Since the molar liquid
overflow is constant, L(n) may be replaced by L(n+1) and:
y(n) = L(n) * x(n+1) / V(n) + D * xd / V(n) equation(1)
Similarly, taking a material balance for the total streams and for the more volatile
component from the bottom to above plate m, as indicated by the loop II in Figure
and noting that L(m) = L(m+1) gives:
y(m) = L(m) * x(m+1) / V(m) - W * xw / V(m) equation(2)
This equation, which is similar to equation 1, gives the corresponding relation

between the compositions of the vapour rising to a plate and the liquid on the plate,
for the section below the feed plate. These two equations are the equations of the
operating lines.
Page | 60
In order to calculate the change in composition from one plate to the next, the
equilibrium data are used to find the composition of the vapour above the liquid,
and the enrichment line to calculate the composition of the liquid on the next plate.
This method may then be repeated up the column, using equation 2 for sections
below the feed point, and equation 1 for sections above the feed point.
Operating line using the Lewis–Sorel method (Graphical)
Operating Line for the Rectification Section

The operating line for the rectification section is constructed as follows. First the
desired top product composition is located on the VLE diagram, and a vertical line
produced until it intersects the diagonal line that splits the VLE plot in half. A line
with slope R/(R+1) is then drawn from this intersection point as shown in the
diagram below.
Figure 3-21 Operating line for the rectification section
R is the ratio of reflux flow (L) to distillate flow (D) and is called the reflux ratio and
is a measure of how much of the material going up the top of the column is returned
back to the column as reflux.
Operating Line for the Stripping Section

The operating line for the stripping section is constructed in a similar manner.
However, the starting point is the desired bottom product composition. A vertical
line is drawn from this point to the diagonal line, and a line of slope Ls/Vs is drawn
as illustrated in the diagram below.
Ls is the liquid rate down the stripping section of the column, while Vs is the vapour
rate up the stripping section of the column. Thus the slope of the operating line for
the stripping section is a ratio between the liquid and vapour flows in that part of
the column.
Page | 61
Figure 3-22 Operating Line for the Stripping Section
Equilibrium and Operating Lines

The McCabe-Thiele method assumes that the liquid on a tray and the vapour above
it are in equilibrium. How this is related to the VLE plot and the operating lines is
depicted graphically in the diagram on the right.
Figure 3-23
A magnified section of the operating line for the stripping section is shown in
relation to the corresponding n'th stage in the column. L's are the liquid flows while
V's are the vapour flows. x and y denote liquid and vapour compositions and the
subscripts denote the origin of the flows or compositions. That is 'n-1' will mean
from the stage below stage 'n' while 'n+1' will mean from the stage above stage 'n'.
Page | 62
The liquid in stage 'n' and the vapour above it are in equilibrium, therefore, xn and
yn lie on the equilibrium line. Since the vapour is carried to the tray above without
changing composition, this is depicted as a horizontal line on the VLE plot. Its
intersection with the operating line will give the composition of the liquid on tray
'n+1' as the operating line defines the material balance on the trays. The
composition of the vapour above the 'n+1' tray is obtained from the intersection of
the vertical line from this point to the equilibrium line.
Number of Stages and Trays

Doing the graphical construction repeatedly will give rise to a number of 'corner'
sections, and each section will be equivalent to a stage of the distillation. This is the
basis of sizing distillation columns using the McCabe-Thiele graphical design
methodology as shown in the following example.
Given the operating lines for both stripping and rectification sections, the graphical
construction described above was applied. This particular example shows that 7
theoretical stages are required to achieve the desired separation. The required
number of trays (as opposed to stages) is one less than the number of stages since
the graphical construction includes the contribution of the reboiler in carrying out
the separation.
Figure 3-24 tray number using graphical solution
The actual number of trays required is given by the formula:

(number of theoretical trays)/(tray efficiency)
Typical values for tray efficiency ranges from 0.5 to 0.7 and depends on a number
of factors, such as the type of trays being used, and internal liquid and vapour flow
conditions. Sometimes, additional trays are added (up to 10%) to accomodate the
possibility that the column may be under-designed.
Page | 63
The Feed Line (q-line)

The diagram above also shows that the binary feed should be introduced at the 4'th
stage. However, if the feed composition is such that it does not coincide with the
intersection of the operating lines, this means that the feed is not a saturated liquid.
The condition of the feed can be deduced by the slope of the feed line or q-line. The
q-line is that drawn between the intersection of the operating lines, and where the
feed composition lies on the diagonal line.
Figure 3-25 Feed line
Depending on the state of the feed, the feed lines will have different slopes. For
example,
q = 0 (saturated vapour)
q = 1 (saturated liquid)
0 < q < 1 (mix of liquid and vapour)
q > 1 (subcooled liquid)
q < 0 (superheated vapour)
The q-lines for the various feed conditions are shown in the diagram on the left.
Using Operating Lines and the Feed Line in McCabe-Thiele Design

If we have information about the condition of the feed mixture, then we can
construct the q-line and use it in the McCabe-Thiele design. However, excluding the
equilibrium line, only two other pairs of lines can be used in the McCabe-Thiele
procedure. These are:
▪ feed-line and rectification section operating line
▪ feed-line and stripping section operating line
▪ stripping and rectification operating lines
This is because these pairs of lines determine the third.
Page | 64
OVERALL COLUMN DESIGN

Determining the number of stages required for the desired degree of separation and
the location of the feed tray is merely the first steps in producing an overall
distillation column design. Other things that need to be considered are tray
spacings; column diameter; internal configurations; heating and cooling duties. All
of these can lead to conflicting design parameters. Thus, distillation column design
is often an iterative procedure. If the conflicts are not resolved at the design stage,
then the column will not perform well in practice. The next set of notes will discuss
the factors that can affect distillation column performance.
3.5.3 Factors affecting distillation column operation

The performance of a distillation column is determined by many factors, for
example:
▪ feed conditions
✓ state of feed
✓ composition of feed
✓ trace elements that can severely affect the VLE of liquid mixtures
▪ internal liquid and fluid flow conditions

▪ state of trays (packings)
▪ weather conditions
Some of these will be discussed below to give an idea of the complexity of the
distillation process.
Feed Conditions
The state of the feed mixture and feed composition affects the operating lines and
hence the number of stages required for separation. It also affects the location of
feed tray. During operation, if the deviations from design specifications are
excessive, then the column may no longer be able handle the separation task. To
overcome the problems associated with the feed, some column are designed to have
multiple feed points when the feed is expected to containing varying amounts of
components.
Reflux Conditions
Page | 65
As the reflux ratio is increased, the gradient of operating line for the rectification
section moves towards a maximum value of 1. Physically, what this means is that
more and more liquid that is rich in the more volatile components are being
recycled back into the column. Separation then becomes better and thus less trays
are needed to achieve the same degree of separation. Minimum trays are required
under total reflux conditions, i.e. there is no withdrawal of distillate.
On the other hand, as reflux is decreased, the operating line for the rectification
section moves towards the equilibrium line. The ‘pinch’ between operating and
equilibrium lines becomes more pronounced and more and more trays are
required. This is easy to verify using the McCabe-Thiele method.
The limiting condition occurs at minimum reflux ration, when an infinite number
of trays will be required to effect separation. Most columns are designed to
operate between 1.2 to 1.5 times the minimum reflux ratio because this is
approximately the region of minimum operating costs (more reflux means higher
reboiler duty).
Vapour Flow Conditions

Adverse vapour flow conditions can cause
▪ foaming
▪ entrainment
▪ weeping/dumping
▪ flooding
Foaming
Foaming refers to the expansion of liquid due to passage of vapour or gas. Although
it provides high interfacial liquid-vapour 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 vapour up to the tray above and is again
caused by high vapour 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 vapour flow. The pressure exerted by the vapour
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.
Page | 66
The minimum vapor velocity (𝑈min) at the weep point:
𝐾2 − .9 ∗ (25.4 − 𝑑ℎ )
𝑈𝑚𝑖𝑛 =
𝜌𝑣 .5
Where, 𝑑ℎ= hole diameter, mm,
𝜌𝑣 = vapor density, kg/m3 (maximum value of vapor density)
𝐾𝟐 = constant (𝐾2) of weep-point correlation depends on the depth of clear liquid
(weir crest + weir height) on the plate.
Weir crest (ℎ𝑤𝑐) can be determined using the Francis’ weir correlation:
𝑙𝑤𝑐 2/3
ℎ𝑤𝑐 = 750( )
𝑙𝑤 𝜌𝑙
𝐿𝑊𝐶=weir length, m
𝐿𝑊=liquid flow rate over the crest, kg/s
𝜌𝑙 = liquid density, kg/m3
Actual operating minimum vapor velocity: 𝑈𝑚𝑖𝑛, 𝑜𝑝=minimum vapor flow ratehole
area[m/s].
To avoid weeping: 𝑈𝑚𝑖𝑛, 𝑜𝑝>𝑈min.
Flooding
Flooding is brought about by excessive vapour flow, causing liquid to be entrained
in the vapour up the column. The increased pressure from excessive vapour 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.
𝜎 𝜌𝑙 − 𝜌𝑉 .5
𝑈𝑛𝑓 = 𝐶𝑠𝑏𝑓 ∗ ( ).2 ∗ ( )
20 𝜌𝑉
𝜌𝑣 = vapor density, kg/m3
𝜌𝑙 = liquid density, kg/m3
σ = liquid surface tension, mN/m (dyn/cm).
𝐶𝑠𝑏𝑓= capacity parameter (m/s) can be calculated in terms of plate spacing and
flow parameter
𝐿=liquid flow rate, kg/s
𝑉=vapor flow rate, kg/s
The design gas velocities (𝑈𝑛) is generally 80-85% of 𝑈𝑛𝑓 for non-foaming liquids
and 75% or less for foaming liquids subject to acceptable entrainment and plate
pressure drop.
Column Diameter
Most of the above factors that affect column operation is due to vapour flow
conditions: either excessive or too low. Vapour flow velocity is dependent on
column diameter. Weeping determines the minimum vapour flow required while
flooding determines the maximum vapour flow allowed, hence column capacity.
Thus, if the column diameter is not sized properly, the column will not perform well.
Not only will operational problems occur, the desired separation duties may not be
achieved.
Page | 67
State of Trays and Packings

Remember that the actual number of trays required for a particular separation duty
is determined by the efficiency of the plate, and the packings if packings are used.
Thus, any factors that cause a decrease in tray efficiency will also change the
performance of the column. Tray efficiencies are affected by fouling, wear and tear
and corrosion, and the rates at which these occur depends on the properties of the
liquids being processed. Thus, appropriate materials should be specified for tray
construction.
Weather Conditions
Most distillation columns are open to the atmosphere. Although many of the
columns are insulated, changing weather conditions can still affect column
operation. Thus, the reboiler must be appropriately sized to ensure that enough
vapour can be generated during cold and windy spells and that it can be turned
down sufficiently during hot seasons. The same applies to condensers.
These are some of the more important factors that can cause poor distillation
column performance. Other factors include changing operating conditions and
throughputs, brought about by changes in upstream conditions and changes in the
demand for the products. All these factors, including the associated control system,
should be considered at the design stages because once a column is built and
installed, nothing much can be done to rectify the situation without incurring
significant costs. The control of distillation columns is a field in its own right, but
that's another story.
3.5.4 Total plate pressure drop

All gas pressure drops (ℎ𝑡) are expressed as heads of the clear liquid and ℎ𝑡is
given by:
ℎ𝑡=ℎ𝑑+ ℎ𝑤𝑐+ℎ𝑤 +ℎ𝑟
Where, ℎ𝑑=dry plate pressure drop, mm
ℎ𝑤𝑐=height of liquid over weir (weir crest), mm
ℎ𝑤=weir height, mm
ℎ𝑟=residual head, mm
Dry plate pressure drop (hd):

Dry plate pressure drop occurs due to friction within dry short holes. ℎ𝑑 can be
calculated using following expression derived for flow through orifices.
𝑈𝑚𝑎𝑥 2 𝜌𝑣
ℎ𝑑 = 51( ) ∗
𝐶0 𝜌𝑙
Maximum vapor velocity:
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒

𝑈𝑚𝑎𝑥 =
𝐴𝐻
The orifice coefficient, 𝐶0 can be determined in terms of 𝐴𝐻/𝐴𝑃 and plate thickness
/hole diameter.
Page | 68
Residual gas pressure head (𝒉𝒓):

The residual pressure drop results mainly from the surface tension as the gas
releases from a perforation. The following simple equation can be used to estimate
ℎ𝑟with reasonable accuracy.
12.5 ∗ 103
ℎ𝑟 =
𝜌𝑙
Down comer backup (hb) and down comer residence time:

The liquid level and froth in the down comer should be well below the top of the
outlet weir on the tray above to avoid flooding.
ℎ𝑏= ℎ𝑤𝑐+ℎ𝑤 +ℎ𝑡+ℎ𝑑𝑐
Head loss in down comer:

𝑙𝑤𝑑 2
ℎ𝑑𝑐 = 166 ∗ ( )
𝜌𝑙 ∗ 𝐴𝑚
𝐿𝑤𝑑 = Down comer liquid flow rate, kg/s
𝐴𝑚=Smaller of clearance area under the down comer apron (𝐴𝑎𝑝) and down comer
area(𝐴𝐷)
The average density of aerated liquid in the down comer can be assumed as 1/2 of
the clear liquid density Therefore, half of the sum of the plate spacing, and weir
height should be greater than the down comer backup.
𝟏/𝟐 (𝐩𝐥𝐚𝐭𝐞 𝐬𝐩𝐚𝐜𝐢𝐧𝐠+𝐰𝐞𝐢𝐫 𝐡𝐞𝐢𝐠𝐡𝐭) >𝒉𝒅
Down comer residence time (𝑡𝑑𝑟𝑡) should be sufficient for the disengagement of
liquid and vapor in the down comer to minimize entrained vapor. The value of
𝑡𝑑𝑟𝑡>3 s is suggested. Down comer residence times given by:
𝐴𝐷 ∗ ℎ𝑏𝑐 ∗ 𝜌𝑙
𝑡𝑑𝑟𝑡 =
𝑙𝑤𝑑
ℎ𝑏𝑐=clear liquid back up, mm
3.6 Dehydration
There has been a gaining interest in the use of fuel ethanol from fermentation
process. A main challenge in producing the ethanol concerned the production cost
which was largely contributed by the process of water removal. Distillation could
remove water to a certain level but due to ethanol water azeotrope an extra process
was needed before ethanol could be blended with gasoline. Problem statement:
Pressure Swing Adsorption (PSA) process was attractive for final separation since
it required less energy and lower setup cost. Despite many researches on simulation
and experimental works on adsorption of water on 3A zeolite in a fixed bed, none
have studied a process with the actual PSA system.
Page | 69
The use of ethanol has gained a wide popularity because of the fact that the raw
material is renewable. A significant cost involved in the ethanol production process
is the energy required for the product purification. The ethanol content of a
fermentation broth is usually about 6-10 wt %. By simple distillation, the ethanol-
water mixture can be enriched up to a maximum of 95 wt %. Further enrichment of
ethanol must obviate the azeotropic point in order to deliver a fuel grade ethanol
(g99.5 wt %). Conventionally, the final purification was done by azeotropic
distillation.
With the development of adsorption processes and invention of molecular sieves,

pressure swing adsorption (PSA) replaced the azeotropic distillation process in the
late 1980s.2 The large-scale process utilizes a 3A zeolite that preferentially adsorbs
water while ethanol molecules are excluded. The PSA process is attractive due to
the low energy consumption, its capability of producing very dry product, and its
proven technical record.
In spite of the widespread application of this technology, a detailed numerical study

on the operation and performance of this PSA process is not available. The quality
of a PSA model largely depends on the accuracy of sub models used for the
description of adsorption equilibrium, heat of adsorption, kinetics, and heat
transfer dynamics. The coupling of these effects can be quite complicated in a real
PSA process due to the fact that the operation is inherently transient.
The objective of this work was to study the adsorption/ desorption kinetics of water
and ethanol on a 3A zeolite in the range of operating conditions corresponding to
the industrial ethanol dehydration PSA process. Dynamic breakthrough
measurements in nonadiabatic fixed beds are a proven technique to assess the
kinetic parameters for adsorption and desorption processes. Adsorption
breakthrough and desorption curves were measured at different operating
conditions by varying the temperature, pressure, bed velocity, inlet concentration,
and particle size. The effects of operating parameters were considered to formulate
the adsorption/desorption kinetic model for the diffusion in a 3A zeolite pellet. The
unknown parameters were estimated by fitting experimental data to the postulated
kinetic model. It was found that both macropore and micropore diffusion
mechanisms are the controlling diffusion mechanisms.
3.6.1 Theory of adsorption

Commercial zeolite adsorbents are made by compressing zeolite crystals (∼1 μm in
diameter) into pellets (a few millimeters in diameter) with the aid of a binder. In
general, the pellet uptake can be controlled by up to four distinct mass transfer
resistances:
Page | 70
1. An adsorbent particle is always enclosed by a laminar film separating the

particle from the bulk fluid.
2. Macropores (voids in the pellet) act as a conduit to transport the gas
molecules from the pellet surface to the particle interior.
3. Molecules are adsorbed on the surface of zeolite crystals (pore mouth), also
known as the surface barrier resistance.
4. Eventually molecules diffuse within the zeolite crystal by a mechanism
known as activated micropore diffusion.
A combination of two diffusion mechanisms, Knudsen diffusion and the molecular
(bulk) diffusion, is possible in the macropore region depending on the size of the
pore and diffusing molecule. Each of the above resistances exhibits a unique
dependence on the operating conditions, and thus a carefully planned experiment
can provide information on the rate-controlling mechanism.
There are only several citations in the open literature on the adsorption kinetics of
water and ethanol on a 3A zeolite relevant to the ethanol-water PSA process.
Several purely experimental studies have demonstrated the ability of a 3A zeolite
to produce fuel grade ethanol in either liquid6 or gaseous phase. It was also
concluded that the extent of the ethanol coadsorption is minimal; however, this
claim was not supported quantitatively. Sowerby and Crittenden developed a
kinetic model for ethanol drying in small columns for the purpose of a temperature
swing adsorption (TSA) process design.8 In their work, an ethanol-water vapor feed
was used in dynamic no isothermal breakthrough measurements. External fluid and
solid film were considered as the relevant mass transfer resistances in the kinetic
model. The range of experimental conditions was quite narrow, especially in terms
of temperatures (105-120 °C), and the effect of pressure was not considered at all.
The solid film coefficient, used to lump the adsorption rate inside the pellet,
indicated the importance of activated micropore diffusion since the system showed
a strong temperature and concentration dependence. However, no comment on the
actual mass transfer mechanism was made. An isothermal breakthrough study for
the ethanol-water mixture was performed by Kupiec et al.7 Micropore diffusion was
assumed to be the rate-limiting step; unfortunately, diffusion coefficients were
reported only at 100 °C. Studies of Sowerby and Kupiec used zeolite pellets of
several millimeters in diameter.
Tian et al.9 performed gravimetric temperature programmed desorption
experiments with 3A zeolite particles smaller than 0.1 mm in diameter. It was
assumed that the macropore and external film resistances were negligible for such
small pellets. Micropore diffusion was considered as the sole mass transfer
phenomenon governing the particle uptake. Data confirmed that the concentration
and temperature dependences of the crystal diffusion coefficient conform to the
Darken equation.
The Eigenberger group studied the breakthrough curves for water on W. R. Grace
4A zeolite.10 They concluded that the macropore diffusion was the controlling
mechanism. Experiments were conducted for temperatures from 25 to 80 °C and
pressures from 2 to 5 bar. Both 3A and 4A pellets should be very similar in terms of
Page | 71
their macropore structure; i.e., the same macropore diffusion mechanism should
apply for both materials. However, it was not reported or observed experimentally
that the macropore diffusion mechanism was relevant for adsorption uptake on a
3A zeolite.
Figure 3-26 Dehydration section
3.7 Calculations of distillation unit
Page | 72
Heat balance over a plate

A heat balance across plate n may be written as:
L(n+1) * HL(n+1) + HV(n−1) * HV(n−1) = V(n) * HV(n) + L(n) * HL(n) + losses + heat of mixing
where: HL(n) is the enthalpy per mole of the liquid on plate n, and HV(n) is the enthalpy
per mole of the vapour rising from plate n. This equation is difficult to handle for
the majority of mixtures, and some simplifying assumptions are usually made. Thus,
with good lagging, the heat losses will be small and may be neglected, and for an
ideal system the heat of mixing is zero. For such mixtures, the molar heat of
vaporization may be taken as constant and independent of the composition. Thus,
one mole of vapour V(n−1) on condensing releases sufficient heat to liberate one mole
of vapour V(n). It follows that V(n) = V(n−1), so that the molar vapour flow is constant
up the column unless material enters or is withdrawn from the section. The
temperature changes from one plate to the next will be small, and HL(n) may be taken
as equal to HL(n+1)
Applying these simplifications to equation, it is seen that L(n) = L(n+1) so that the
moles of liquid reflux are also constant in this section of the column. Thus V(n) and
L(n) are constant over the rectifying section, and V(m) and L(m) are constant over the
stripping section.
For these conditions there are two basic methods for determining the number of
plates required. The first is due to SOREL and later modified by LEWIS
Calculation of number of plates using the Lewis–Sorel method

If a unit is operating as shown in Figure so that a binary feed F is distilled to give a
top product D and a bottom product W, with xf , xd, and xw as the corresponding
mole fractions of the more volatile component, and the vapour Vt rising from the
top plate is condensed, and part is run back as liquid at its boiling point to the
column as reflux, the remainder being withdrawn as product, then a material
balance above plate n, indicated by the loop I in Figure gives:
V(n) = L(n+1) + D
Page | 73
Figure Material balances at top and bottom of column Expressing this balance for
the more volatile component gives:
y(n) * V(n) = L(n+1) * x(n+1) + D * xd
Thus: y(n) = L(n+1) * x(n+1) / V(n) + D * xd / V(n)
This equation relates the composition of the vapour rising to the plate to the
composition of the liquid on any plate above the feed plate. Since the molar liquid
overflow is constant, L(n) may be replaced by L(n+1) and:
y(n) = L(n) * x(n+1) / V(n) + D * xd / V(n) equation(1)
Similarly, taking a material balance for the total streams and for the more volatile
component from the bottom to above plate m, as indicated by the loop II in Figure
and noting that L(m) = L(m+1) gives:
y(m) = L(m) * x(m+1) / V(m) - W * xw / V(m) equation(2)
This equation, which is similar to equation 1, gives the corresponding relation

between the compositions of the vapour rising to a plate and the liquid on the plate,
for the section below the feed plate. These two equations are the equations of the
operating lines.
In order to calculate the change in composition from one plate to the next, the
equilibrium data are used to find the composition of the vapour above the liquid,
and the enrichment line to calculate the composition of the liquid on the next plate.
This method may then be repeated up the column, using equation 2 for sections
below the feed point, and equation 1 for sections above the feed point.
In our case
Input (Feed): mixture of water and ethanol containing 10% mole per cent ethanol
at its boiling temp and Atmospheric pressure
Feed = 2 Kg/sec = .01 Kmol/sec
Required: ethanol with purity 96%
Givens:
Rm= (xd – yf)/(yf – xf)=(.87-.4375) / (.4375 - .1) = 1.28
reflux ratio = 1.28 * factor of relux = 1.28 * 3 = 4
bottom product containing not more than .08 mole per cent ethanol
overall mass balance gives:
.01 = D + W
Page | 74
A balance on the MVC, Ethanol, gives:

.1*.1 = .87*D + .08*W
Thus: W = .089 and D = .011 kmol/sec
Using reflux ratio = 4
L(n) = 4D = .0435 kmol/sec
and: V(n) = L(n) + D = .0545 kmol/sec
the top operating line from equation 1 is:
y(n) = L(n) * x(n+1) / V(n) + D * xd / V(n)
y(n) = .8 * x(n+1) + .175 equation(i)
Since the feed is all liquid at its boiling point, this will all run down as increased
reflux to the plate below.
Thus: L(m) = L(n) + F
L(m) = .0435 + .1 = .1435
Also: V(m) = L(m) − W
V(m) = V(n) = .1435 - .089 = .05458
Thus:
y(m) = 2.63 * x (m+1) − .013 equation(ii)
With the two equations (i) and (ii) and the equilibrium curve, the composition on the
various plates may be calculated by working either from the still up to the condenser,
or in the reverse direction. Since all the vapour from the column is condensed, the
composition of the vapour yt from the top plate must equal that of the product xd ,
and that of the liquid returned as reflux xr. The composition xt of the liquid on the top
plate is found from the equilibrium curve and, since it is in equilibrium with vapour of
composition, yt = 0.40, xt = 0.075.
By applying graphical solution No of theoretical stages = 25 tray
overall efficiency of tray =ηo=50.3(αμ)−0.226
α relative volatility at concentration of 10% = 7.274
μ viscosity of feed in cp = .31 cp
ηo=50.3(αμ)−0.226 = 4%
actual stage number required = No of theoretical stages/ηo = 25/.4 = 62 tray
number of trays = no of stage – 2 (reboiler stage) = 60 tray
Page | 75
Estimation of physical properties

Column top pressure= 101325 Pa (1 atm)
Assume Pressure drop of 1.25kPa per tray
Column pressure drop=1.25×103×40=50000 kPa
Top section Bottom section
Column top pressure= 101325 Pa Column bottom pressure= 101325 +
and temperature= 78 °C 50000 = 151325 bar ~ 1.5 bar
𝑃𝑚 101.325 ∗ 42.4 Boiling point of water at 1.5 bar = 112 °C

𝜌𝑣 = = = 1.5
𝑅𝑇 353 ∗ 8.314 (bottom contains 99 moles% water)
𝜌𝑙 =900 kg/m3 (density of the mixture) Average molecular weight of liquid = 18

Average molecular weight = 42.4 Average molecular weight of vapour= 43
From the steam table at 150000 Pa and

112 °C: 𝜌v = .86; 𝜌𝑙 = 950 kg/m3
Surface tension, σ =18×10-3 N/m Surface tension, σ =58*10-3 N/m
Plate spacing
Plate spacing of 600 mm is considered for the first trial to calculate capacity
parameter (𝐶𝑠𝑏𝑓) for the estimation of maximum allowable vapor velocity through
the net plate area. The suggested plate spacing is 600 mm for column diameter>1.5
m.
Column diameter
1st trial is started with the following considerations: Design is performed
• for 80% flooding at maximum gas flow rate.
• Total down comer top and bottom seal area is 10% of the net area.
Flow parameter (𝐹𝐿𝐺) based on mass flow
rate,
𝐿 𝜌𝑉 .5 0.0435 ∗ 42.4 1.5 .5 𝐿 𝜌𝑉 0.143 ∗ 18 . 86 .5
∗( ) = ∗( ) 𝐹𝐿𝐺 = ∗ ( ).5 = ∗( )
𝑉 𝜌𝐿 0.0545 ∗ 42.4 900 𝑉 𝜌𝐿 0.0545 ∗ 43 950
= .032 = .033
Capacity parameter (𝐶𝑠𝑏𝑓) = 0.12 m/s 𝐶𝑠𝑏𝑓 = 0.1 m/s
𝜎 .2 𝜌𝑙 − 𝜌𝑉 .5 𝜎 .2 𝜌𝑙 − 𝜌𝑉 .5
𝑈𝑛𝑓 = 𝐶𝑠𝑏𝑓 ∗ ( ) ∗( ) 𝑈𝑛𝑓 = 𝐶𝑠𝑏𝑓 ∗ ( ) ∗( )
20 𝜌𝑉 20 𝜌𝑉
18 .2 900 − 1.5 .5 58 .2 950 − .86 .5

𝑈𝑛𝑓 = .12 ∗ ( ) ∗( ) 𝑈𝑛𝑓 = .1 ∗ ( ) ∗( )
20 1.5 20 . 86
= 2.87 𝑚/𝑠 = 4.1 𝑚/𝑠
Page | 76
The linear design gas velocity (𝑈𝑛) based

on net area (80% flooding:
𝑈𝑛 = 0.8×2.87= 2.3 m/s 𝑈𝑛 = 0.8×4.1 = 3.2 m/s
The maximum volumetric vapor flow rate

𝑉∗𝑀 . 0545 ∗ 42.4 𝑉∗𝑀 . 0545 ∗ 43
𝑄𝑚𝑎𝑥 = = 𝑄𝑚𝑎𝑥 = = = 2.7 𝑚3 /𝑠
𝜌𝑣 1.5 𝜌𝑣 . 86
3
= 1.54 𝑚 /𝑠
Net area required Net area required

𝑄𝑚𝑎𝑥 1.54 𝑄𝑚𝑎𝑥 2.7
= = = .7 𝑚2 = = = .85 𝑚2
𝑈𝑛 2.3 𝑈𝑛 3.2
Totals tower cross-section area: Totals tower cross-section area:

.7 . 85
= = .78 𝑚2 = = .95 𝑚2
.9 .9
(Total down comer top and bottom seal (Total down comer top and bottom seal
area is 10% of the net area) area is 10% of the net area)
Colum (tower) diameter: Colum (tower) diameter:

. 78 . 95
𝐷=√ =1𝑚 𝐷=√ = 1.1 𝑚
. 785 . 785
Use the higher value of the tower diameter for the uniformity between sections, if the
difference is not greater than 20%. In this case, the bottom diameter is used both in
top and bottom sections.
Higher area than the design area (here top section) can be taken care by reducing the
perforated area. The nearest recommended shell (nominal diameter 1100 mm)
fabricated from carbon steel or stainless-steel sheet in IS 2844-1964: ID 2403 mm
with minimum wall thickness: 8 mm for carbon steel) and 6 mm for stainless steel.
Provisional plate design

Column (tower) diameter (ID): 𝐷𝑇 ≈ 1.1 m
Column cross-section area: 𝐴𝑇=0.785×1.1 = .86 m2
Down comer area: 𝐴𝐷=0.1*𝐴𝑇= 0.086 m2
Net area: 𝐴𝑁=𝐴𝑇−𝐴𝐷= 0.774 m2
Weir Length (𝑙𝑊) = 0.73×𝐷𝑇 = .8 m
Weir height, ℎ𝑤= 40 mm is considered.
Page | 77
Active area: 𝐴𝐴=𝐴𝑇−2×𝐴𝐷= .928 m2
For the first trial, consider hole diameter: 𝑑ℎ=12 mm (12inch). The plate
thickness=hole diameter is selected for the first trial.
Checking for weeping

Maximum liquid flow rate
𝑚𝑚𝑎𝑥 = .0435*42.4 = 1.84 kg/s 𝑚𝑚𝑎𝑥 = .1435*18 = 2.58 kg/s
Minimum liquid flow rate (𝑚𝑚𝑖𝑛) (70% Minimum liquid flow rate (𝑚𝑚𝑖𝑛) (70%
of 𝑚𝑚𝑎𝑥) = .7 *1.84 = 1.3 kg/s of 𝑚𝑚𝑎𝑥) = .7 *2.85 = 1.8 kg/s
Maximum weir crest, Maximum weir crest,

𝑙𝑤𝑐 2/3 𝑙𝑤𝑐 2/3
ℎ𝑤𝑐 = 750( ) ℎ𝑤𝑐 = 750( )
𝑙𝑤 𝜌𝑙 𝑙𝑤 𝜌𝑙
1.84 2 2.58 2
ℎ𝑤𝑐 = 750( )3 = 14 𝑚𝑚 ℎ𝑤𝑐 = 750( )3 = 17 𝑚𝑚
. 8 ∗ 900 . 8 ∗ 950
Minimum weir crest, Minimum weir crest,
𝑙𝑤𝑐 2/3 𝑙𝑤𝑐 2/3
ℎ𝑤𝑐 = 750( ) ℎ𝑤𝑐 = 750( )
𝑙𝑤 𝜌𝑙 𝑙𝑤 𝜌𝑙
1.3 2 1.8 2
ℎ𝑤𝑐 = 750( )3 = 11.1 𝑚𝑚 ℎ𝑤𝑐 = 750( )3 = 13.3 𝑚𝑚
. 8 ∗ 900 . 8 ∗ 950
The constant (𝐾2) of weep-point The constant (𝐾2) of weep-point

correlation= 30 at correlation= 30.2 at
ℎ𝑤𝑐+ℎ𝑤=11.1+40=51.1 mm using ℎ𝑤𝑐+ℎ𝑤=13.3+40=53.3 mm using
minimum liquid flow rate. minimum liquid flow rate.
The minimum vapor velocity (𝑈min) at The minimum vapor velocity (𝑈min) at
the weep point: the weep point:
𝐾2 − .9 ∗ (25.4 − 𝑑ℎ ) 𝐾2 − .9 ∗ (25.4 − 𝑑ℎ )
𝑈𝑚𝑖𝑛 = 𝑈𝑚𝑖𝑛 =
𝜌𝑣 .5 𝜌𝑣 .5
30 − .9 ∗ (25.4 − 12) 30.2 − .9 ∗ (25.4 − 12)
𝑈𝑚𝑖𝑛 = 𝑈𝑚𝑖𝑛 =
1.5.5 . 86.5
= 14.6 𝑚/𝑠 = 19.5 𝑚/𝑠
Actual minimum vapor velocity at Actual minimum vapor velocity at

minimum vapor flow rate: minimum vapor flow rate:
70% 𝑜𝑓 𝑄𝑚𝑎𝑥 . 7 ∗ 1.54 70% 𝑜𝑓 𝑄𝑚𝑎𝑥 . 7 ∗ 2.7
= = =
𝐴𝐻 . 15 ∗ .928 𝐴𝐻 . 15 ∗ .928
= 7.7 𝑚/𝑠 = 13.5 𝑚/𝑠
Therefore, the minimum operating velocity both in top and bottom sections is of
above the weep point velocity.
Page | 78
Plate pressure drop

Maximum vapor velocity: Maximum vapor velocity:
𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 𝑀𝑎𝑥𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒
𝑈𝑚𝑎𝑥 = 𝑈𝑚𝑎𝑥 =
𝐴𝐻 𝐴𝐻
1.54 2.7
𝑈𝑚𝑎𝑥 = = 11 𝑚/𝑠 𝑈𝑚𝑎𝑥 = = 20 𝑚/𝑠
. 15 ∗ .928 . 15 ∗ .928
Maximum dry plate pressure drop: Maximum dry plate pressure drop:
𝑈𝑚𝑎𝑥 2 𝜌𝑣 𝑈𝑚𝑎𝑥 2 𝜌𝑣
ℎ𝑑 = 51( ) ∗ ℎ𝑑 = 51( ) ∗
𝐶0 𝜌𝑙 𝐶0 𝜌𝑙
11 2 1.5 20 2 . 86
ℎ𝑑 = 51( ) ∗ = 13.3 𝑚𝑚 ℎ𝑑 = 51( ) ∗ = 25 𝑚𝑚
. 88 900 . 88 950
The orifice coefficient, 𝐶0=0.88 at The orifice coefficient, 𝐶0=0.88 at
𝐴𝐻/𝐴𝑃=15% and 𝐴𝐻/𝐴𝑃=15% and
(plate thickness hole/ diameter) =1 (plate thickness hole/ diameter) =1
Residual head: Residual head:

12.5 ∗ 103 12.5 ∗ 103 12.5 ∗ 103 12.5 ∗ 103
ℎ𝑟 = = ℎ𝑟 = = = 13 𝑚𝑚
𝜌𝑙 900 𝜌𝑙 950
= 13.8 𝑚𝑚
Total plate pressure drop: ℎ𝑡 =ℎ𝑑 + Total plate pressure drop: ℎ𝑡 =ℎ𝑑 +
ℎ𝑤𝑐 +ℎ𝑤 +ℎ𝑟= 13.3 + (40+11.1) + 13.8 ℎ𝑤𝑐 +ℎ𝑤 +ℎ𝑟= 25 + (40+13.3) + 13 ≈
≈ 80 mm liquid 91.3 mm liquid
Page | 79
CHAPTER 4: WATER AND WASTEWATER TREATMENT
4 CHAPTER 4: WATER AND WASTEWATER TREATMENT

4.1 INTRODUCTION
Although not often thought of as a commodity (or, for that matter, not thought about
at all), water is a commodity a very valuable commodity. In this text, it is our
position that with the passage of time, potable water will become even more
valuable. Moreover, with the passage of even more time, potable water will be even
more valuable than we might imagine. It may be possibly comparable in pricing,
gallon for gallon, to what we pay for gasoline, or even more. Earth was originally
allotted a finite amount of water we have no more or no less than that original
allotment today. It logically follows that, in order to sustain life as we know it, we
must do everything we can to preserve and protect our water supply. We also must
purify and reuse the water we presently waste (i.e., wastewater).
Historically, the purpose of water supply systems has been to provide pleasant
drinking water that is free of disease organisms and toxic substances. In addition,
the purpose of wastewater treatment has been to protect the health and well-being
of our communities. Water and wastewater treatment operations have
accomplished this goal by:
1. prevention of disease and nuisance conditions.

2. avoidance of contamination of water supplies and navigable waters .
3. maintenance of clean water for survival of fish, bathing, and recreation; and
4 generally conservation of water quality for future use.
The purpose of water supply systems and wastewater treatment processes has not
changed. However, primarily because of new regulations the paradigm has shifted,
these include:
1. protection against protozoan and virus contamination.
2. Implementation of the multiple barrier approach to microbial control.
3. New requirements of the Ground Water Disinfection Rule, the Total
Coliform Rule and Distribution System, and the Lead and Copper Rule.
4. Regulations for trihalomethanes and disinfection by-products (DBPs).
4.2 Water treatment

In Faga company the source of water is from the government, but we can't use it
directly, we must do more treatment before the water go to the boiler or to the
process This is a solution from Praj company for water treatment.
Page | 80
4.2.1 Treatment steps

Chlorination: Is used to prevent the spread of waterborne diseases such as
cholera, dysentery, and typhoid.
Clarifier: A settling tank is used to remove solid particulates or suspended solids
from liquid for clarification.
Filtration system: Which removes particulate matter from water by forcing the
water to pass through porous media.
(DM) Water Treatment Plants (Demineralization): Is the process of removing
mineral salts from Water by using the ion exchange process.
4.3 Wastewater treatment (process condensate)

Wastewater is treated in anaerobic and aerobic digesters. In the anaerobic digester,
a small amount of urea, phosphoric acid, and micronutrients are added as nutrients
for the anaerobic organisms. Biogas from the anaerobic digester is used as boiler
fuel. The wastewater is further treated aerobically. It is then held in a clarifying tank
where the settled solids are separated from the water. The solids are dewatered in
a belt filter press, with a polymer being added to aid in dewatering, followed by a
screw press. The resulting sludge is used as boiler fuel. The water from the clarifying
tank is recycled as process water.
The process will be designed for zero discharge to a municipal treatment plant in a
steady-state mode, and the treated water will be suitable for recycling to the
process.
Page | 81
▪ Any process upset (sudden increase of solids in the wastewater) will not be
considered in the model.
▪ Rain and snow run-off, equipment washing, and other non-process waters
are assumed to flow to the municipal wastewater treatment system; other
intermittent loads (process spills) will not be considered in the design.
▪ No insoluble components (cellulose, xylan) will be included in the chemical-
oxygen demand (COD) calculations because of uncertainty of their reactivity.
▪ Biological oxygen demand in the anaerobic digester is assumed to be 70% of
the COD.
❖ COD reduction in both digesters is considered as 99.4%.
Wastewater is treated in anaerobic and aerobic digesters. In the anaerobic digester,

a small amount of urea, phosphoric acid, and micronutrients are added as nutrients
for the anaerobic organisms. Biogas from the anaerobic digester is used as boiler
fuel. The wastewater is further treated aerobically. It is then held in a clarifying tank
where the settled solids are separated from the water. The solids are dewatered in
a belt filter press, with a polymer being added to aid in dewatering, followed by a
screw press. The resulting sludge is used as boiler fuel the water from the clarifying
tank is recycled as process water.
4.4 ETP (Effluent Treatment Plant)

▪ ETP (Effluent Treatment Plant) is a process design for treating the
industrial wastewater for its reuse or safe disposal to the environment.
▪ Influent: untreated industrial wastewater.
▪ Effluent: treated industrial wastewater.
▪ Sludge: solid parts separated from wastewater by ETP.
Page | 82
4.4.1 Available treatment options

1. Pretreatment of biological followed by membranes.
2. Only membrane-based system.
❖ We use in our project Pretreatment of biological followed by membranes option
because it is better in treatment process.
Figure 4-1 Block flow diagram
Page | 83
Figure 4-3 P and ID
Page | 84
4.5 Dosing pumps

4.5.1 Digital dosing pumps
SMART Digital diaphragm dosing pumps
(up to 200 l/h)
Covering flow rates up to 200 liters an hour, and output pressure
ratings up to 16 bar, the SMART Digital range delivers reliable, safe, and
cost effective dosing in any application across a wide selection of
businesses including water treatment, with industry-leading user
friendliness and flexibility. And the advanced monitoring and self-
analysis features offered by several control variants provide intelligent
process control that looks beyond the pump and keeps an eye on the
entire system for you.
A complete package with two pump size

The SMART Digital range includes the original SMART Digital DDA, DDC,
and DDE pumps which cover flows up to 30 l/h, and the SMART Digital
XL DDA and DDE pumps which cover flows up to 200 l/h. All pumps can
be supplied with a wide selection of accessories such as installation kits,
signal cables, and dosing tanks that make it even easier to customize the
pumps to any application.
Service and maintenance friendly

SMART Digital pumps have very long service and maintenance intervals,
significantly lowering pump life-cycle cost and contributing to
disruption-free, reliable dosing performance. And when service is
needed, our tailor-made service kits ensure optimal service that keeps
pumps running in top condition for years.
DDA: high-end solution for complex and demanding

applications
▪ Auto Flow Adapt: automatically adapts measured flow to attain
target flow.
▪ Auto-deaeration during pump standby.
▪ Flexible Fieldbus control.
▪ Turn-down ratio 1:3000 with constant 100% stroke length.
DDC: optimal price-performance ratio

▪ Two Slow Mode steps (25% and 50%), calibration mode, service
display.
▪ External stop, dual-level tank control, 2 relay outputs.
DDE: a cost-effective Digital Dosing™ solution

▪ Control options: manual control 0.1-100 %, pulse in % of stroke
volume, and analogue control (DDE XL).
▪ External stop, empty tank control.
Page | 85
DME: digital diaphragm

(dosing pumps up to 940 l/h)
Dosing is precision work, and Digital Dosing™ represents state of-the-art
technology. Grundfos DME Digital Dosing™ pumps combine perfect
precision with user-friendliness, covering large dosing quantities up to
940 l/h with few variants.
DME: precise and easy setting

▪ Two pump variants: 375 l/h at 10 bar, or 940 l/h at 4 bar.
▪ Turn-down ratio 1:800 with constant 100% stroke length.
▪ Adjustable slow mode for dosing high viscosity liquids (up to
3000 mPas).
DMH: hydraulic piston diaphragm dosing pumps

(up to 2 x 1500 l/h and up to 200 bar)
The Grundfos DMH range is a series of extremely strong, robust pumps
for applications requiring reliable dosing and high-pressure capability,
such as process engineering. The range is highly versatile: it covers a
wide flow range and offers a variety of dosing head sizes, materials and
accessories.
DMH: long lifetime in high-pressure applications

▪ Capacity from 0.15 to 2 x 1500 l/h and up to 200 bar; available in
simplex and duplex versions.
▪ Integrated pressure relief valve and active diaphragm protection
system.
▪ Available with ATEX design – certified for EX classified zones and
API 675 certificate.
▪ Double diaphragm design and breakage monitoring for max.
safety.
4.5.2 Mechanical diaphragm dosing pumps

DMX: mechanical diaphragm dosing pumps
“Pre-selected Range” up to 765 l/h
DMX pre-selected range is the fast lane to reliable, tough and well-proven
DMX dosing pumps up to 765 l/h. The DMX pre-selected range in the
product portfolio of mechanical diaphragm dosing pumps covers the
most common applications with a wide performance range from 16 l/h
(12 bar) to 765 l/h (3 bar) and a variety of accessories. DMX pre-selected
products can be chosen easily and delivered quickly. If necessary, they
can be replaced simply and quickly.
Page | 86
DMX: mechanical diaphragm dosing pumps

(“Standard Range” up to 2 x 4000 l/h)
The Grundfos DMX range has proven its worth in dosing applications
worldwide. With their robust diaphragm-based design and high-quality
motors, DMX pumps require minimum maintenance and are the best
choice for many dosing applications. The DMX range is highly versatile:
it covers a wide flow range and offers a variety of dosing head sizes,
materials and accessories.
DMX: robust design for minimum maintenance

▪ Capacity from 0.4 to 2 x 4000 l/h and up to 10 bar.
▪ Double-head versions increase flexibility or dosing flow rate.
▪ Available with ATEX design – certified for EX classified zones.
4.6 Biological treatment

4.6.1 Equalization tank
Firstly, we use equalization tank to make wastewater homogenous.
▪ The main aim of the equalization tank is to equalize the flow and
characteristics and load the effluent to the further treatment at a constant
uninterrupted rate.
▪ Retention time depends on the capacity of treatment plant (about 8-16
hours). and from here. the effluent is pumped to the Condensate Treatment
Plant. Here, the effluent pH is neutralized using Caustic Soda or Lime.
Preferably, lime is utilized as a first preference as the end use of water does not
rely on the TDS of the water and, therefore. moderate TDS in the water is
acceptable. The Equalization tank is designed for a retention time of 8 hrs.
generally, equalization tanks for wastewater treatment plants refer

to a holding tank that allows for flow to be equalized over a
specific period of time.
▪ the equalization tanks will be used for storing sewage temporarily and
used as a preventative measure to protect effluent quality in extreme storm
conditions.
▪ the equalization tank also acts to equate the flow in terms oforganic
loading. mixing will be provided by submersible mixers to prevent sewage
from septic.
Page | 87
The goal of an equalization tank:

• Equalize the flow rate.
• Equalize or balance the organic concentration.
• Dilute or dampen the impact from inhibitory compounds.
• Neutralize the ph.
• Even out temperature fluctuations.
• Minimize chemical usage (e.g., downstream ph adjustment).
• No need to design for large peak flows, the eq tank equalizes the flow
• And spreads out the peaks
• Minimize chemical usage;
• BOD/COD, TSS, Alkalinity, Ammonia and TKN are equalized for better
process control.
Types of equalization tank:

1. Flow through type- useful in assisting self-neutralization. a flow through
type tank once filled, gives output equal to input.
2. Intermittent flow type flow balancing and self-neutralization are both achieved by using
two tanks, intermittently one after another.
3. Variable flow/constant discharge type: - when flow is large an equalization tank of such
a size may have to be provided that inflow can be variable while outflow is at constant
rate.
Figure 4-4 Schematic view of equalization-homogenization tank
Page | 88
Figure 4-6 Equalization tank
Figure 4-5 Process condensate treatment plant
Page | 89
4.6.2 Anaerobic tank

Anaerobic digestion is a process in which microorganisms convert organic matter
into biogas in the absence of oxygen. It is an energy-efficient process that is typically
utilized to treat high strength industrial wastewater that is warm and contains high
concentrations of biodegradable organic matter (measured as BOD, COD, and/or
TSS). An anaerobic system can be used for pretreatment prior to discharging to a
municipal wastewater treatment plant or before polishing in an aerobic process.
Anaerobic processes use substantially less energy, require less chemicals, and incur
lower sludge handling costs compared to aerobic treatment options. In addition, the
biogas produced in the anaerobic process is a source of renewable energy that can
be used to displace fossil fuels such as oil or natural gas, or to generate electricity.
Anaerobic wastewater treatment

Anaerobic digestion is a biological process in which organic wastes are broken
down by microorganisms in the absence of oxygen. An anaerobic system can be
used for pretreatment prior to discharging to a municipal wastewater treatment
plant or before polishing in an aerobic process. Anaerobic treatment is typically
utilized to treat warm, high-strength industrial wastewater containing high
concentrations of biodegradable organic matter. This energy-efficient process
reliably removes biochemical oxygen demand (BOD), chemical oxygen demand
(COD), and total suspended solids (TSS) from wastewater.
Advantages of anaerobic digestion

As organics are removed from the wastewater during the anaerobic digestion
process, methane-rich biogas is produced. This valuable biogas can be captured,
treated, and used a source of renewable energy to displace fossil fuels or to generate
heat or electricity.
A hybrid reactor is an anaerobic digester that combines a UASB reactor with an

anaerobic filter. This combination is an advanced form enabling improved solid
retention time in the treatment of wastewater. This wastewater can be built up in
the secondary chamber and must be removed daily or an explosion is imminent to
occur.
Up flow anaerobic sludge blanket (UASB) technology, normally referred to as

UASB reactor, is a form of anaerobic digester that is used for wastewater treatment.
The UASB reactor is a methanogenic (methane-producing) digester that evolved
from the anaerobic clarigester.
Page | 90
Figure 4-7 Anaerobic hybrid reactor
In sewage treatment systems, an anaerobic filter (AF) is a form of anaerobic

digester. The digestion tank contains a filter medium where anaerobic microbial
populations organisms that live in the absence of oxygen — can establish
themselves. Such filters are commonly employed in the treatment of waste water.
These reactors are gaining in popularity versus more established aerobic waste-
water treatment systems because they produce a less solid residue[1] than do other
types of filter.
Advantages of hybrid anaerobic digester:
▪ Due to the presence of a fixed film of biomass that grows on the plastic fill
media, the need to develop and maintain a granular sludge is eliminated.
▪ The time required to start-up and stabilize the hybrid anaerobic digester is
significantly lower than other high rate anaerobic reactor technologies.
▪ Hybrid anaerobic digester can achieve BOD and COD (organic pollutants)
reductions of up to 90% and 70%.
▪ A Hybrid anaerobic digester requires less volume compared to a
conventional anaerobic digester.
In this process we get 3 components:
▪ Biogas: go to the boiler.
▪ Effluent substrate: complete the biological treatment.
▪ Sludge : goes to the decanter room.
Page | 91
Figure 4-8 Anaerobic digestor
4.6.3 Decanter room

The sludge came out from the anaerobic hybrid reactor is then goes to a decanter
Room contains centrifuge to separate solids from liquids.
Page | 92
Figure 4-9 Process condensate tank
4.6.4 Decanter Centrifuges

Are popular solid and-liquid separators used in multiple industries for a wide array
of products Decanters are used for the extraction of liquids from large proportions
of solids.It makes use of medium-low speed suspension to process large capacities
of solids as compared to a Basket Centrifuge.
Figure 4-10 Flottweg decanter
Page | 93
Figure 4-11 Decanter
4.6.5 Aeration tank

▪ The water is passed like a thin film over the different arrangements like
staircase shape.
▪ Dosing of Urea and DAP is done.
▪ Water gets direct contact with the air to dissolve the oxygen into water.
▪ BOD & COD values of water is reduced up to 90%.
Page | 94
Page | 95
Figure 4-12 Aeration tank
Figure 4-13 Aeration tank real view
Page | 96
Types of aeration
Selection of aeration type shall be made considering efficiency of mixing and oxygen
transfer and location of WWTPs. Aeration types include point injection diffuser
system, multiple injection diffuser, jet aerator, and submerged turbine aerator.
Depending on the types of aerator, design parameters shall be in the table.
Figure 4-14 Types of Aeration
5.6 shape, structure, and number of reactor tank

The shape shall be rectangular or square.
The width shall be 1 to 2 times of depth for standard type.
The width shall be about equal to the depth for deep aeration type.
Aeration equipment
Aeration equipment shall enable to provide air uniformly from all the release
points.
Aeration equipment shall be physically durable and resistant to chemical attac
Figure 4-15 Types of Diffuser
Page | 97
Air pipeline
▪ The material shall be steel, either SGP or STPY, with zinc coatings.
▪ The material for droplegs shall be stainless.
▪ The pipeline in the pipe gallery shall be insulated as temperature of blower
discharge reaches 80 degrees Celsius.
Air pipeline shall be installed above wastewater level to prevent backflow of waste
water into the pipeline and later corrosion.
Expansion joints shall be installed considering the thermal stress to pipeline.

Flexible joints shall be installed where pipeline passes different structures.
Valves shall be attached for check, flow adjustment, backflow prevention, and
waste air discharge.
▪ Air flow meter shall be equipped.
▪ Air flow meter shall be accurate with small head loss and few chances of
failure.
Aeration tank Blowers:

First of all, it is important to understand why a blower is required when treating
wastewater. Blowers are typically used to provide aeration in activated sludge
plants and to promote aerobic digestion. They keep solids suspended in channels
and in aeriated grit chambers, which is absolutely necessary for a proper treatment
ecosystem.
Types of Blowers
There are three main types of blowers; positive displacement lobe, centrifugal and
high efficiency.
Positive displacement lobe blowers are typically use for smaller applications. Their
output and pressure are directly governed by the speed you run them at. It is
perfect for these small or medium applications.
Centrifugal blowers are used in medium or large wastewater treatment
applications. True centrifugal vane-style blowers usually run at a constant speed,
but you can vary the airflow output by throttling the inlet valve to the blower.
Figure 4-16 Aeration blowers
Page | 98
Figure 4-17 Aeration Diffusers
Figure 4-18 Aeration blowers
For applications that require a high volume of air, a high efficiency blower like
the Sulzer-ABS HST (High Speed Turbocompressor) is an ideal blower. It is the only
blower that uses magnetic bearings, making it extremely efficient and allowing for
the fastest payback on investment.
Sizing of Blower
The size of your blower is determined by many variables in your application. You
must consider the load, flow, tank configurations, sidewater depth of the tank, and
specific treatment application. A design engineer should be involved when building
a new treatment facility or when drastically updating existing equipment. If you
have a municipal facility, you should consider the growth that your community
might experience.
A variable frequency device (VFD) and/or a dissolved oxygen monitoring device
can be added to a blower to give you better insight and control over your
application. This will allow you to adjust the efficiency and effectiveness of your
blower if your process changes.
Page | 99
Page | 100
4.7 Membrane system

After finishing the biological treatment, we start the membrane and reverse osmosis
treatment
Figure 4-20 Reverse osmosis

Figure 4-21 RO skid
Figure 4-22 Reverse osmosis vessel
Page | 101
4.8 Calculations
4.8.1 Flow calculations
In water and wastewater treatment, one of the major concerns of the operator is
not only to maintain flow, but also to measure it. Normally, flow measurements are
determined by metering devices. These devices measure water flow at a particular
moment (instantaneous flow) or over specified time (total flow). Instantaneous
flow can also be determined mathematically. In this section, we discuss how to
mathematically determine instantaneous and average flow rates and how to make
flow conversions.
Instantaneous Flow Rates
In determining instantaneous flows rates through channels, tanks and pipelines, we can use Q
= A  V.
❖ Note: It is important to remember that when using an equation such as Q = A  V the

units on the left side of the equation must match those units on the right side of
the equation (A and V) with respect to volume (cubic feet or gallons) and time
(seconds, minutes, hours, or days).
4.8.2 Velocity calculation

To determine the velocity of flow in a channel or pipeline we use the Q = A * V equation.
However, to use the equation correctly we must transpose it. We simply write into the
equation the information given and then transpose for the unknown (V in this case).
Equivalents, Formulae, and Symbols Equivalents
12 in. = 1 ft
36 in. = 1 yd
144 in2 = 1 ft2
9 ft2 = 1 yd2
43,560 ft2 = 1 ac
1 ft3 = 1728 in3
1 ft3 H20 = 7.48 gal
1 ft3 H20 = 62.4 lb
1 gal of H20 = 8.34 lb
1L = 1.000 mL
1g = 1.000 mg
1 MGD (million gal[MG]/d) = 694 gal/min, 1.545 ft3/sec

average BOD/capita/day = .17 lb
average SS/capita/day = .20
average daily flow = assume 100 gal/capita/day
Page | 102
Symbols
A = Area
V = Velocity
t = Time
SVI = Sludge Volume Index
v = Volume
ibs = Pounds
eff = Effluent
W = Width
D = Depth
L = Length
H = Height
Q = Flow
C = Circumference
r = Radius
π = pi (3.14)
WAS = Waste activated sludge
RAS = Return activated sludge
MLSS = Mixed liquor suspended solids
MLVSS = Mixed liquor volatile suspended solids
Page | 103
4.8.3 Chlorine dosage

Chlorine is a powerful oxidizer commonly used in water treatment for purification
and in wastewater treatment for disinfection, odor control, bulking control, and
other applications. When chlorine is added to a unit process, we want to ensure that
a measured amount is added. In describing the amount of chemical added or
required two ways are used: (1) mg/L, and (2) lb/d. In the conversion from mg/L
(or ppm) concentration to lbs/day.
Mg/L *MGD * 8.34= lb/d
4.8.4 Hypochlorite dosage

At many wastewater facilities sodium hypochlorite or calcium hypochlorite are
used instead of chlorine. The reasons for substituting hypochlorite for chlorine vary.
However, with the passage of stricter hazardous chemicals regulations under the
Occupational Safety and Health Administration and the U.S. Environmental
Protection Association many facilities are deciding to substitute the hazardous
chemical chlorine with nonhazardous hypochlorite. Obviously, the potential
liability involved with using deadly chlorine is also a factor involved in the decision
to substitute it with a less toxic chemical substance.
Step 1: Calculate the lb/d chlorine required using the mg/L to lb/d
equation:
Mg/L *MGD * 8.34= lb/d
Step 2: Calculate the lb/d hypochlorite required:
PERCENT REMOVAL
Percent removal is used throughout the wastewater treatment process to express
or evaluate the performance of the plant and individual treatment unit processes.
The results can be used to determine if the plant is performing as expected or in
troubleshooting unit operations by comparing the results with those listed in the
plant’s operations and maintenance manual. It can be used with either
concentration or quantities. For concentrations use:
Page | 104
Brake horsepower
Brake horsepower (Bhp) refers to the horsepower supplied to the pump from the
motor. As power moves through the pump, additional horsepower is lost from
slippage and friction of the shaft and other factors; thus, pump efficiencies range
from about 50 to 85% and must be taken into account.
Motor horsepower
Motor horsepower (Mhp) is the horsepower the motor must generate to produce
the desired brake and water horsepower.
4.8.5 Anaerobic Digestion

Systems for treatment of solid waste and slurries Systems used to digest solid
waste are classified according to the percentage of Total Solids (TS) in the waste
stream: 15-25% low solids anaerobic digestion: wet fermentation >30% high
solids anaerobic digestion: dry fermentation.
❖ Data gathering and design parameters evaluation for subsequent feasibility study
anaerobic digestion of vinasse.
Page | 105
Design parameters include:

▪ Digester size.
▪ Volumetric loading rate.
▪ Volume of gas produced.
▪ Electric power generating capabilities.
Process improvement project for the distillery, as gas of high calorific value is produced as well
as a stabilized sludge
Vinasse-Dependence on Raw Material and Ethanol Process

▪ When obtained straight from sugar cane juice.
✓ Light brown color with 20,000-40,000 mg/l solid content.
▪ When obtained from sugar cane molasses:
✓ Black-reddish color with 50,000-10,000 mg/1 solid content.
▪ pH between 4 and 5.
▪ BOD content between 10.000 and 50.000 mg/l.
Page | 106
▪ A mass balance on the microorganisms in the digester is given by equations:
Accumulation = Inflow-Outflow + Net Growth
𝑑𝑥
∗ 𝑉 = 𝑄𝑋𝑜 − 𝑄𝑋 = 𝑉𝑟 ∗ 𝑟′𝑔
𝑑𝑡 𝑟
Process Design Reactor Size

▪ Where Vch4 volume of methane produced at standard conditions (32° F and 1 atm),
Ft3/day
▪ 5.62 = theoretical conversion factor for the amount of methane produced from the
complete conversion of one pound of BOD to methane and carbon dioxide, ft3 CH4/lb
BODL Oxidized
* Q = Vinasse flow rate, Mgal/day
* So = Ultimate BODL in influent, mg/L
* S = Ultimate BODL in effluent, mg/L
Vr=Q(ϴc)
The electrical power is given by :
𝜂𝑜𝑣𝑒𝑟𝑎𝑙𝑙=Net Electric Energy Output/ Fuel Heat Input
▪ Operation temperature of anaerobic digestion: 40°C (104°F)

▪ Efficiency of waste utilization during anaerobic digestion (E) : 90%
▪ Overall thermal efficiency: 90%
▪ Methane heating value: 600 Btu/cu ft
▪ Vinasse specific gravity: 1.02 to 1.04
❖ If we know the range of vinasse we enter this table and get the range of the digester
volume and amount of effluent vinasse generated.
Vol of methane produced:
Page | 107
Vol of overall gas produced
Page | 108
Figure 4-23 Schematic drawings of septic tanks
❖ Since vinasse BOD equal about 30000 mg/l We select digester volume:
29,696,503 Liter So, Vol of methane produced 27,300,499 L/day.
4.8.6 Decanter
We select from FLOTTWEG CENTRIFUGES for High Efficient Stillage Separation in Bioethanol
Production
Figure 4-24 Flottweg decanter
Page | 109
Cost efficient due to:

• Minimized energy consumption for Flottweg Simp Drive.
▪ Maintenance friendly.
▪ High performance in terms of cake dryness and centrate clarity.
▪ Machine designs based on decades of experience in stillage separation.
High availability and reliability

▪ Secure supply of lubrication oil to the bearings via oil-air lubrication.
▪ Short downtime while servicing due to easy access to service points.
4.8.7 Aeration
Table 4-1 Design parameter of activated sludge process
Page | 110
V = 1008 * (8/24) = 336 m3
Page | 111
4.8.8 Reverse osmosis calculations
Page | 112
Page | 113
4.9 References
▪ Design Standard For Municipal Wastewater Treatment Plants Second Edition
Japan Sewage Works Association
▪ Flottweg separation technology
▪ Hydraulics ,a Nitto Denco Company
▪ Hydranautics,aNittoDenkoCompany
▪ Handbook of Water and Wastewater Treatment Plant Operations
▪ Praj BRIEF PROCESS DESCRIPTION OF 2G ETHANOL PROCESS
▪ Praj-Water-and-Waste-Water-Re-energize
▪ Praj-Water-and-Waste-Water-Brochure
▪ Basic Mathematics for Water and Wastewater Operators
▪ GRUNDFOS DOSING & DISINFECTION
▪ http://www.shrijee.com/turnkey-ethanol-plants
▪ http://reverseosmosischemicals.com/reverse-osmosis-guides/reverse-osmosis-
membrane-preservation-ro-nf-membranes
Page | 114
Page | 115
CHAPTER 5: EVAPORATION (VINASSE CONCENTRATION UNIT)
5 CHAPTER 5: EVAPORATION
(VINASSE CONCENTRATION UNIT)
5.1 INTRODUCTION
5.1.1 Process description
Vinasse is a liquid residue from the sugarcane-based ethanol industry. After
sugarcane juice fermentation by yeast, ethanol concentration in the fermented
broth is no more than 10% v/v (due to its toxicity). During distillation, the ethanol
is recovered, and everything left is called vinasse. It is produced in high volumes
(12–15 L for each liter of ethanol) and is rich in minerals .it also contains every
substance added to the fermenter, plus yeast metabolites and yeast cell contents
(all byproducts of the fermentation process) .The primary organic and inorganic
chemical components of vinasse are proteins, organic acids, amino acids,
unfermented carbohydrates, vitamins, and minerals .high concentrations of
potassium, calcium, magnesium, sulfur, and nitrogen are typically found as
components of vinasse .it is denser than water at room temperature (vinasse
density = 1.25–1.33 g mL–1; water density = 1.0 g mL–1).
The major problem related to vinasse is its high chemical and biological oxygen
demands: 29,000 and 17,000 mgO2/L, respectively, which makes it 100 times more
pollutant than average domestic wastewater. Vinasse polluting strength is mainly
due to high organic matter content and the presence of three important nutrients:
nitrogen, phosphorous, and potassium. Due to its composition, vinasse is largely
used as a fertilizer in sugarcane cultivation. Vinasse could be concentrated to
60%ds without much difficulty in terms of viscosity and scaling formation. Vinasse
is a liquid of low viscosity at 25 C. with increasing solute concentration, the viscosity
of the liquid will increase, often quite substantially, and this affects circulation and
the heat transfer coefficients leading again to lower rates of boiling. Design should
be based on the initial dry solid content of x % ds and a target of say 70 % ds. The
concentration process needs heat energy for removing the moisture.
Page | 116
A Multiple effect Evaporation system provides steam economy. Vinasse typically

has a moisture content of about 93%, and the present organic solids and minerals,
such as potassium, calcium, and magnesium, may provide a rich culture medium for
biological cultivation
Evaporation is the removal of solvent as vapor from a solution, slurry or suspension

of solid in a liquid. (Evaporation is the process of a substance in a liquid state
changing to a gaseous) The aim is to concentrate a non-volatile solute, such as
organic compounds, inorganic salts, acids or bases from a solvent. Hence the vapor
is not the desired product and may or may not be recovered according its value. The
volatile component is evaporated (in most cases the volatile component is water),
leading to an increased concentration of the non-volatile dry solid material.
Figure 5-1 General description of how Vinasse can be treated and processed
Figure 5-2 Schematic drawing of evaporator
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5.1.2 Purposes of Evaporation

▪ Concentrate liquid foods.
▪ Energy savings in subsequent operations (e.g. spray drying).
▪ Reduces weight (and volume) Energy savings in storage and transportation.
▪ Reduces water activity (preservation).
▪ Changes flavor and/or color (caramelized syrups in baking), Products: Salt,
sugar, milk, juices, tomato paste, hard candies, purees.
▪ Prepare for the next Unit operation – drying, crystallization etc.
▪ Reduces deteriorative chemical reactions.
▪ Better microbiological stability.
▪ Recovery of solvent.
5.1.3 Industrial Applications

▪ Food Industry
▪ Corn Industry
▪ Chemical Industry
▪ Waste Water Treatment
▪ Pharmaceutical Industry, Examples: -
✓ Concentration of milk to produce condensed milk Concentration of
juices.
✓ Concentration of NaOH, NaCl from aqueous solutions to produce
salt.
▪ Ether recovery from fat extraction.
5.2 Thermodynamics of Evaporation

1. Evaporation can be divided into three categories on the basis of boiling
phenomena. Pool boiling: In this phenomena bulk or pool of liquid boils.
Examples are kettle boiling, natural circulation boiling units, thermo siphon
reboilers in distillation.
2. Convection heating and boiling: Example is forced circulation-boiling units.
3. Film evaporation: In film evaporation, a thin liquid film is maintained on the
heating surface.
5.2.1 What happens during Evaporation?

▪ Boiling point of solution rises.
✓ Due to increase in solid content.
▪ ∆T between steam and product decreases.
✓ Due to steam temperature remaining constant and product
temperature (boiling temperature) increasing.
▪ Rate of heat transfer decreases.
✓ Due to ∆T between steam and product decreasing.
5.2.2 Mechanism of evaporation

Evaporation vs Vaporization: Evaporation is the process of a substance in a liquid
state changing to a gaseous state due to an increase in temperature and/or
pressure. Vaporization is also the phase change from liquid to gas state but above
Page | 118
the boiling point of the liquid. Evaporators are used to separate Materials based on
differences in their boiling temperatures.
Evaporation vs distillation: In evaporation no attempts to separate the component

of vapor.
Evaporation vs dehydration (Dehydration of Ethanol to Ethylene): the final product

of evaporation process remains in liquid state.
5.2.3 Processing factors – liquid characteristic

Liquid concentration -> relates to viscosity and heat transfer
▪ Solubility
▪ Temperature and Pressure.
▪ Boiling temperature is inversely proportional to pressure.
▪ Boiling points may increase as solution get concentrated (boiling point
rise)
▪ Temperature sensitivity of material (biomaterial)
▪ Foaming -> will determine the height of your
freeboard in the Design
▪ Solubility of materials -> May be the limit to the concentration that you can
achieve.
▪ Scale deposits -> decrease your heat transfer
coefficient.
Liquid concentration
In evaporation, concentration of liquid increase, thus viscosity will also increase
resulting in decreasing of overall heat transfer coefficient. So, additional agitation
is required.
Solubility
Solubility is increasing with temperature. However, as evaporation continues,
liquid solution will become more and more concentrated (saturated) and solubility
will exceed its limit.
Temperature sensitivity of materials

Products very sensitive to high temperature, i.e. protein and pharmaceutical
materials, may destroyed and degraded. Use vacuum instead to lower the boiling
point.
Foaming and frothing

Liquid solutions such as caustic solutions and skim milk. These foam and froth
accompany water vapor resulting in entrainment losses.
P&T
As T increase, solution will become more concentrated, resulting in increasing of
solution boiling point. Elevation or boiling-point-rise (BPR).
Scale deposition and material of construction deposit solid materials on heating
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surfaces resulting in decreasing of overall heat transfer coefficient, U. suitable

material to minimize corrosion.
5.2.4 Effect of processing variables

Feed temperature, Tf- if cold, some of steam is used to heat up the feed to the boiling
point. If feed is under pressure/vacuum and Tf is above the boiling point, additional
vaporization is obtained, flash of hot feed.
Operating Pressure- if in vacuum, high ΔT can be obtained, resulting large decrease

in heating surface area, A.
Steam pressure- increasing steam pressure will increase ΔT, resulting in low And
low capital cost. However, the price for high-pressure steam is more costly.
5.3 Thermal design of evaporator

For each effect, determine steam requirement (MS) by performing:
▪ Mass balance
▪ Solids balance
▪ Energy balance
✓ Use Q = UA(ΔT) to determine area required for heat transfer
“look at appendix 1”
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5.4 Classification of evaporators
5.4.1 Rising-film Evaporator

The liquid starts boiling at the lower part of the tube and the liquid and vapor flow
upward through the tube.
The upward movement of vapors causes a thin liquid film to move rapidly upward.
This co-current upward movement against gravity has the advantageous effect of
creating a high degree of turbulence in the liquid. This is useful during evaporation
of highly viscous and fouling solutions. Operates by natural circulation thermo-
siphon action and thereby eliminates the need for large pumping systems.
5.4.2 Falling Film Evaporators

The liquid is allowed to flow down through the inner wall of the tubes as a film. As
the liquid travels down the tubes the solvent vaporizes and the concentration
gradually increases. Vapor and liquid are usually separated at the bottom of the
tubes and the thick liquor is taken out Evaporator liquid is recirculated through the
tubes by a pump below the vapor-liquid separator The distribution of liquid in the
inner wall of the tubes greatly affects the performance of this type of evaporator
used for concentration of fruit juices and heat sensitive materials because of the low
holdup time. The device is suitable for scale forming solutions as boiling occur on
the surface of the film.
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The residence time is about 20-30 seconds, compared with a residence

time of 3-4 minutes in a rising-film evaporator.
Figure 5-3 Rising vs Falling Film evaporator
5.4.3 Forced circulation evaporators

Forced circulation evaporators are usually more costly than natural circulation
evaporators natural circulation evaporators are not suitable under some
situations such as:
▪ highly viscous solutions due to low heat transfer coefficient
▪ solution containing suspended particles
▪ for heat sensitive materials.
All these problems may be overcome when the liquid is circulated at high velocity
through the heat exchanger tubes to enhance the heat transfer rate and inhibit
particle deposition.
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The main components of a forced circulation

evaporator are a tubular shell and tube heat exchanger (either horizontal or
vertical), a flash chamber (separator) mounted above the heat exchanger and a
circulating pump the solution is heated in the heat exchanger without boiling and
the superheated solution flashes off (partially evaporated) at a lower pressure are
reduced in the flash chamber.
The pump pumps feed and liquor from the flash chamber and forces it through the
heat exchanger tubes back to the flash chamber. Axial flow pumps are used to
maintain high circulation rates with linear velocities of 2-6 m/s, compared with a
linear velocity of 0.3-1 m/s in natural-circulation evaporators.
Forced circulation evaporator is commonly used for concentration of caustic and

brine solutions and also in evaporation of corrosive solution.
Figure 5-4 Forced circulation evaporator
5.5 Evaporator configuration

5.5.1 Single stage evaporators
In this type, evaporator the vapor from the boiling liquid is condensed and
discarded.
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Figure 5-5 Simplified diagram of single –effect evaporator
Are used when

1. Through put is low.
2. Cheap supply of steam is available.
3. Vapors are contaminated.
Drawbacks
1. It uses steam inefficiently.
2. To evaporate 1 kg of water we need 1-1.3 kg of steam.
5.5.2 Multi-effect evaporators

Series of evaporators between the steam supply and condenser is called multiple
effect evaporator.
The vapors from one effect serve as the heating medium for the next.
Temp of vapors decreases and pressure also decreases.
Four types of feeding systems: -

1. Forward feed
2. Backward feed
3. Mixed feed
4. Parallel feed
Forward feeding
steam is used only in the first effect the liquid solution is heated to saturation
and eventually evaporated the vapors are reused as the heating medium in
another evaporator chamber.
The partially concentrated product leaving the first effect is introduced as

feed into the second effect. the product from the second effect becomes feed
for the third effect.
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The product from the third effect leaves at the desired

concentration This is called a forward feed system Forward feeding
operation is helpful when the concentrated product may degenerate if
exposed to high temperature.
It requires a pump for feeding of dilute solution to the first effect. A pump
removes thick liquor from the last effect. The liquid from one effect to the
next effect also can be transferred without a pump as the flow occurs in the
direction of decreasing pressure. Feed is hot and final product is
temperature sensitive.
backward feed
In backward feed configuration, the feed enters at the last effect (coldest
effect) and is pumped through the successive effects. The product is
withdrawn from the first effect (hottest) where the steam is introduced. This
method of feeding requires a pump between each pair of effects to transfer
liquid from lower pressure effects to higher pressure effects.
It is advantageous when cold feed entering needs to be heated to a lower
temperature than in forward feed operation. Backward feed is commonly
used when products are viscous and exposure to higher temperature
increases the rate of heat transfer due to reduction in viscosity of the liquid.
Cold fresh feed, pump is required, and final product is highly viscous.
Mixed feed
Mixed feed arrangement eliminates some of the pumps needed in backward
configuration as flow occurs due to pressure difference whenever
applicable.
Figure 5-6 Backward-feed, triple-effect

Figure 5-7 Forward -feed, triple effect
Parallel feed
The fresh feed is introduced to each effect and in this configuration the
product is withdrawn of from the same effect in parallel feed operation in
parallel feeding, there is no transfer of liquid from one effect to another
effect. It is used primarily when the feed is saturated and the product is solid
containing slurry. This is most common in crystallizing evaporators.
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5.5.3 Optimization of Multiple Effect Evaporators

The determination of the optimal number of effects in an evaporation system, were the
optimum is found when there is an economic balance between energy saving and added
investment, this is, a minimization of the total cost. The results observed that as number
of effects of evaporators increased, annual cost of steam decreases and annual cost of
evaporator increases.
Annual Cost of Steam

The steam consumption may be represented according to the following equations:
For single effect evaporator
Dsteam =Q/ λ
For multiple effect evaporator
Dsteamλsf +Gf CpTf = GC1 pT1 +VH1 1
Where, Dsteam is mass flow rate of steam consumption, kg/s, λ is latent heat of
vaporization, kJ/kg, Gf is the flow rate of feed solution, kg/s, G1 is the flow rate of
first effect evaporator, kg/s, T1 is temperature of solution in the first effect, °C, Cp is
specific heat of the solution, kJ/kg.deg., V1 is the amount of vapor produced from
first effect, kg/h., H1 is the enthalpy of the vapor leaving the evaporator, kJ/kg, Q is
the heat load of the evaporator, kJ/s
Annual Cost of Steam

Cost of steam = Dsteam CIII
Where CIII is the cost per ton steam, L.E/ton
Annual cost of steam = cost of steam x Annual operating days x operating hours
Annual Cost of Evaporator

Annual cost of evaporator may be calculated as follows,
Purchased cost = 75228.2 (A)0.5053
Annual cost of evaporator = Purchased cost (1+0.6) 0.15
Where, (1+0.6) is the cost of piping and installation, and 0.15 is the depreciation
cost. A is the area of heat transfer of the evaporator, calculated according to the
equation:
Q = UA ∆T
Where,
∆ T is the driving force = (Tsteam - Tboiling), °C (26) U is the overall heat transfer
coefficient, kW/m2 K
Annual Total Cost

The annual total cost is calculated by applying the following equations:
Annual total cost = Annual cost of steam + Annual cost of evaporator, L.E/year
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5.6 Quadrable effect evaporator
Figure 5-8 Quadrable effect evaporator
Figure 5-9 Comparison between multi-effect plate and tubular evaporator
5.7 Plate evaporator

Gasketed Plate Evaporator
Plate heat exchangers (PHE), often called plate-and frame heat exchangers, are used
to change the temperature of a liquid, vapor or gas media. A thin, corrugated plate
is used to transfer the heat from the media on one side of the plate to the media on
the other side.
The gasketed-plate evaporator is also called the plate evaporator because the
design is similar to that of a plate heat exchanger. A number of embossed plates
with four corner openings are mounted by an upper and a bottom carrying bar.
The gasket is placed at the periphery of the plates. The interfering gaskets of two
adjacent plates prevent the mixing of the fluids and lead the fluid to the respective
Page | 127
flow path through the corner opening (Figure 5-10). The fluids may either flow in
series or parallel depending on the gasket arrangement.
The heat transfer coefficient is greatly enhanced due to high turbulent flow through
narrow passages. This evaporator is suitable for high viscous, fouling, foaming and
heat sensitive solutions.
This type of evaporators is mainly used for concentration of food products,

pharmaceuticals, emulsions, glue, etc.
AlfaVap plate evaporators are specially designed for evaporation duties. They
combine the benefits of compact, efficient plate heat exchangers and can handle
small temperature differences between the hot and cold side. Typical uses: As
reboilers in distillation columns and as evaporators for the Vinasse.
Figure 5-10 Plate evaporator
Comparison face Phe Sht

Multiple duty Possible Impossible
Hold up volume Low High
Gaskets On each plate On flanged joints
modifications Easy by adding or removing plates impossible
Repair Easy to replace plates and gaskets Requires tube plugging
Detection of leakage Easy to detect Difficult to detect
Access for inspection On each side of plate Limited
Time reqd. for opening 15 min 60 to 90 min
Fouling 15 to 20 % of STHE
Sensitivity to vibrations Not sensitive sensitive
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Figure 5-11 Comparison of plate and sht heat exchanger
5.7.1 working modes

Once through
Due to the rising film concept and the high turbulence, AlfaVap provides
excellent wetting ability, which means that a once-through evaporation
process can often be used. In a concurrent system, this means no pumps are
needed between the effects. In a counter-current system, it means that
recirculation pumps are not necessary – only transportation pumps are
needed. The once-through mode also gives extremely low residence time.
Figure 5-12 Once through Mode
Forced circulation with boiling

This mode is used when the evaporated product has a tendency to foul.
The forced circulation increases the wetting and turbulence and thus
minimizes any fouling tendency.
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Figure 5-13 Forced circulation with boiling
Thermosiphon
In the thermosiphon mode, natural circulation is used, rendering
recirculation pumps unnecessary. This mode is used when the outlet vapour
fraction is too high for a once-through evaporation process. The
thermosiphon mode is also used for AlfaVap when used as a reboiler in
distillation systems.
Figure 5-14 Thermo siphon mode
Forced circulation with flashing

This mode is used when the evaporated product could cause considerable
fouling or when crystallization takes place during the evaporation process.
The evaporated liquid is recirculated so rapidly that boiling cannot take
place in the evaporator, and the liquid is thus just heated. The actual
evaporation then takes place when the liquid flashes in to the separator
vessel. A special type of AlfaVap with a wider gap is used for this mode, to
minimize the fouling.
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Figure 5-15 Forced circulation with flashing
5.7.2 AlfaFlash
The AlfaFlash is a plate evaporator, working as a forced circulation flash evaporator,
often used in the final concentration step as a finisher. It is designed with a high
wall shear to minimize viscosity (in case of a shear thinning product), fouling and
to maximize time intervals between cleaning. The considerably higher shear rate
(already at quite moderate flows) leads to substantially higher heat transfer
efficiency, much smaller pumps and significantly lower pump costs.
5.7.3 Plate technology

The novel pattern into which the plate material has been formed not only gives
strength and rigidity, but greatly increases the rate of heat transfer from the warmer
medium to the metal wall and from the wall to the other medium.
This high heat flow through the walls can be seriously reduced by the formation of
deposits of various kinds on the wall surfaces. The pattern of corrugation on Alfa
Laval plates mentioned above induces highly turbulent flow. The turbulence gives
strong resistance to the formation of deposits on the plate surface; it cannot always
eliminate fouling.
5.7.4 Patterns
1. Induce turbulence for high HT coefficient
2. Reinforcement and plate support points that Mainly 2 types of patterns
(corrugations) are used:
1. Intermating or washboard corrugations.
2. Chevron or herringbone corrugations maintains inter-plate
separation.
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CHEVRON OR HERRINGBONE
▪ Most common type
▪ Corrugations are pressed to same depth as plate spacing
▪ Operate at High pressure
▪ Corrugation depth 3mm to 5mm
▪ Velocity 0.1 to 1 m/s
INTERMATING TROUGH PATTERNS

▪ Pressed deeper than spacing
▪ Fewer connection points
▪ Operate at Lower pressure
▪ Max channel gap 3mm to 5mm
▪ Min channel gap 1.5 mm to 3 mm
▪ Velocity range in turbulent region is 0.2 to 3 m/s
The deposits may increase the total” wall thickness” substantially, and they consist
of materials that have a much lower thermal conductivity than the metal plate.
Consequently, a layer of deposits can severely reduce the overall heat transfer rate.
Figure 5-16 Typical cathegories of plate corrugations. (a) washboard, (b) zigzag, (c) chevron or
herringbone, (d) protrusions and depressions (e) washboard with secondary corrugations, e (f) oblique
washboard [3].
5.7.5 Plate Types

WideGap plate
WideGap plate heat exchangers are specially designed to handle fibrous
liquids and liquids that contain large amounts of suspended solids. The
design combines the benefits of compact, efficient plate heat exchangers
with a special plate pattern and port design that help prevent fouling.
Typical uses: Cooling mash to fermentation temperature and removing heat

generated in the fermentation process.
Solids & Particles:

Round:
> 1/8” dia ------- not recommended
<= 1/8” dia. = wide gap PHE
<= 1/16” dia. = standard PHE
Long Stringy: not recommended
Figure 5-17 Wide gap plate
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Figure 5-18 gap between plates
Double-wall plate
Composed of plates pressed simultaneously and laser welded at the port, this is
designed for applications where additional reliability against intermixing is
necessary to prevent catastrophe. Failure of one plate results in external detection
without intern leakage. The second wall provides a double barrier between fluids,
meeting local health code regulations.
Double-wall gasketed plate heat exchangers are ideal for use with fluids that
must not be allowed to mix. Pairs of identical plates are laser-welded around
the ports. The gasket is installed in the conventional manner and the welded
plate pairs are assembled in a plate pack in the same way as ordinary single
plates. In the unlikely event of leakage through a plate because of a puncture
or crack, the leaking fluid will never come into contact with the fluid in the
other circuit, as it will be stopped by the double plate and flow outside the
heat exchanger.
Perfect for use in Pharmaceutical, food or industries where the intermixing

of fluids is hazardous
Figure 5-19 double wall plate
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Semi-welded plates
Figure 5-21 Semi welded plate Figure 5-20 laser welding
Plates welded together into a cassette allow aggressive and difficult fluids -
that are not compatible with gaskets - to be handled in a plate heat
exchanger. This welding also expands the pressure range capable within the
heat exchanger. Perfect for use in refrigeration or chemical applications
where aggressive fluids might be found.
Figure 5-22 Semi welded plate
Diabon Graphite non-metallic

A composite of fused graphite and fluoroplastic, this unit provides excellent
resistance to hydrochloric acid, AlCl3, and other corrosive materials. Unlike
traditional graphite, Diabon F® has no porosity or permeability. It resists
cracking and breakage during handling and use.
Figure 5- Diabon Graphite non-metallic plate
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Figure 5-24 Plate evaporator
Figure 5-23 semi-welded plate
The port area has a double gasketed seal to prevent product mixing The interspace
is vented to atmosphere for leak detection
Figure 5-25 Leakage detection hole
Page | 135
5.7.6 Plate condensers

Plate condensers are specially designed for condensing duties. They combine the
benefits of compact, efficient plate heat exchangers with the low pressure drop
required for condensing. Typical uses: Condensing ethanol vapour from the
distillation column and the vapour from stillage evaporators.
Figure 5-26 plate condenser
5.7.7 Counter vs co counter

In counter flow heat exchanger, the hot fluid passes in direction opposite to cold
fluid.
Now we use LMTD method in order to find out the area of heat exchanger. Now for
same mass flowrate and same inlet and outlet conditions of temperature the LMTD
OF COUNTER FLOW HEAT EXCHANGER WILL BE MORE COMPARED TO PARALLEL
FLOW HEAT EXCHANGER as the flow is in opposite direction.
1. Hence the area for counter flow heat exchanger will be LESS compared to
parallel flow heat exchanger. Thus, more efficient.
2. The highest ideal effectiveness achieved in case of counter flow heat
exchanger is 100% while for parallel flow is only 50%.
3. In counter flow heat exchanger, the outlet temperature of hot fluid can be
cooled even less than outlet temperature of cold fluid which cannot be done
in case of parallel flow heat exchanger.
4. Counter flow HE needs less space compared parallel flow HE and even more
heat. This is the major factor why counter flow HE used in most of
applications.
5. co counter flow has higher thermal stress since large temperature difference
is large.
Page | 136
Figure 5-27 plate vs sht counter flow comparision
5.7.8 Arrangement of a plate heat exchanger

The simplest types of arrangements of plate heat exchangers are those in which
both fluids make just one pass, so there is no change in direction of the streams.
These are known as 1-1single-pass arrangements, and there are two types:
countercurrent and concurrent. A great advantage of the single-pass arrangement
is that the fluid inlets and outlets can be installed in the fixed plate, making it easy
to open the equipment for maintenance and cleaning, without disturbing the
pipework. This is the most widely used single-pass design, known as the U
arrangement. There is also a single-pass Z-arrangement, where there is input and
output of fluids through both end plates (Figure 5-28). Countercurrent flow, where
the streams flow in opposite directions, is usually preferred due the achievement of
higher thermal efficiency, compared to concurrent flow, where the streams flow in
the same direction. Multi-pass arrangements can also be employed to enhance the
heat transfer or flow velocity of the streams, and are usually required when there
is a substantial difference between the flow rates of the streams (Figure 5-29).
Page | 137
Figure 5-28 U arrangement and Z arrangement
Figure 5-29 Multi-pass PHE
Figure 5-31 Four possible 3-2 arrangements Figure 5-30 Four possible 4-1 arrangements
5.7.9 Plate materials
Page | 138
AISI 304 This is perhaps the most inexpensive grade of austenitic stainless steels,
and it offers good general corrosion resistance to a range of organic and non-organic
fluid media but exhibits poor resistance to sulfuric and hydrochloric acids. It does,
however, develop crevice corrosion when chlorides are present in water.
AISI 316 A higher grade of stainless steel, which contains 2.5% molybdenum
that makes it relatively more resistant to chloride-induced crevice corrosion. It can
also be used with low concentrations (10–15%) sulfuric acid, though this depends
upon the operating temperature.
5.7.10 Plate geometry

Plate thickness vary from 0.5- and 3-mm. Gap between two plates 1.5 to 5 mm.
Plate surface areas range from 0.03 to 1.5 m2, with a plate width:length ratio from
2.0 to 3.0.
The size of plate heat exchangers can vary from 0.03 m2 to 1500 m2.
The maximum flow-rate of fluid is limited to around 2500 m3/h.
Plates are available in a wide range of metals and alloys; including stainless steel
aluminum and titanium. A variety of gasket materials is also used.
5.7.11 Gaskets
They limit the maximum operating temperature for a plate heat exchanger.
Material selection depends upon
1. Chemical resistance.
2. Temperature resistance.
3. Sealing properties.
4. Shape over an acceptable period of time.
Rubber
1. The choice of rubber material depends on Fluids - chemical attack or not.
2. The combination of temperature and pressure.
3. Rubber materials change properties due to Time - the rubber relaxes.
4. Temperature - the rubber deteriorates
5. Hardening by attack of oxidizing agents (e.g., oxygen in air).
6. Swelling or softening by absorption of chemicals in the fluids.
Page | 139
EPDM
EPDM, or ethylene propylene diene monomer, is widely used to make O-rings,
washers and other sealing fittings in water and steam lines and in auto and truck
cooling and brake systems. EPDM seals are resistant to mild acids, detergents,
silicones, glycols, ketones and alcohols, and can handle temperatures from minus
22 degrees Fahrenheit up to 300 degrees. They are resistant to ozone. The major
weakness of EPDM rubber washers and other seals is that they break down and
deliver poor sealing performance in systems handling petroleum-based fuels, oils
and solvents.
Nitrile Rubber
Nitrile rubber, also known as Buna-N, is made by combining the polymers butadiene
and acrylonitrile. It offers excellent resistance to gasoline, diesel fuel, motor oil and
other petroleum-based products. For this reason, it’s widely used for washers and
O-rings that seal fuel systems of autos, boats, aircraft and stationary engines. It can
be formulated for temperatures ranging from minus 65 degrees Fahrenheit to 275
degrees. Nitrile rubber’s biggest drawback is that it can suffer from exposure to
sunlight, general weathering or ozone from electrical equipment unless specifically
compounded to resist them.
Page | 140
5.7.12 Frames materials

1. Carbon steel with a synthetic resin finish
2. stainless steel
5.7.13 Plate Evaporator Manufacturer:

1. APV
2. AlphaLaval
3. GEA
4. Trante
5.8 AlfaVap
The AlfaVap plate evaporator is the result of development work done in
collaboration with beet sugar manufacturers in the late 1980s. This new type of
cost-effective rising film evaporator rapidly became a success in the beet sugar
industry and has subsequently spread to many other applications.
There are currently more than 3000 AlfaVap evaporators installed in different
applications all over the world, and Alfa Laval provides a complete range of AlfaVap
evaporators for a wide selection of applications and capacities.
Figure 5-32 AlphaVap Models
Page | 141
Why use AlfaVap? Cost saving

How it works High heat transfer High heat transfer
AlfaVap is tailor-made for efficiency efficiency means that
evaporation, with two The special corrugated much less heat transfer
small inlet feed
plate pattern induces a area is needed compared
connections and a large high degree of turbulence, to shell-and-tube
outlet for the vapour and providing substantially evaporators.
concentrate. There is one better heat transfer
large inlet connection for This makes AlfaVap
coefficients than
the heating steam, and two extremely economical,
conventional shell-and-
small outlets for the especially
tube evaporators.
condensate. when exotic materials
AlfaVap is especially such as SMO, titanium,
AlfaVap uses the cassette efficient at high nickel and Hastelloy are
concept with the plates concentration required. In addition, the
welded in pairs. The and high viscosities, and compact and flexible
heating steam is can work with design of AlfaVap
condensed in the welded temperature differences drastically reduces
channels while the down to 3–4°C. This is a transport, erection and
evaporated product big advantage when installation costs
passes through the AlfaVap is used in TVR and compared to shell-and-
gasketed channels MVR systems tube units
Improved product quality

Easy to increase capacity The extremely low hold-up
A popular feature of AlfaVap is that volume means that very little
the capacity can be increased or product is actually in the
reduced by just adding or removing AlfaVap at any given time. The
short time the product spends in
cassettes in the existing frame. This
the evaporator is a big
is a major advantage in relation to
advantage for heat sensitive
shell-and-tube evaporators, where products. It also permits rapid
capacity is fixed at the level decided start-up and shut down, with
on at the time of installation only minimal waste.
Page | 142
Less fouling and easy

maintenance
The high turbulence over
the whole plate does not
just reduce fouling but
also makes chemical
Save space
cleaning very effective.
The compact, versatile design of
Due to the low holdup
AlfaVap and AlfaCond means that
volume, only very small
transportation, erection and
quantities of cleaning
installation costs are all drastically
chemicals are needed
reduced compared to conventional
compared to shell-and-
shell-and tube units.
tubes. The flexible design
of the AlfaVap means
the heat transfer surfaces
are easily accessible for
inspection or mechanical
cleaning by simply
removing the tightening
bolts and rolling back the
pressure plate.
Figure 5-33 Comparison between space of sht and plate
Page | 143
5.9 Separators
Why use separator?
▪ To reducing material losses in absorbers, evaporators, and distillation columns,
e.g., for reducing glycol or amine losses in natural gas treatment.
▪ To improve product quality in distillation plants because contamination by
entrained droplets is eliminated.
▪ To avoiding corrosion in the downstream process units through corrosive liquid
droplets.
✓ To protect compressors against liquid droplets.
✓ To reducing droplet emissions.
✓ To relieve vacuum pumps.
5.9.1 Selection Criteria for Vapor-Liquid Separators

The configuration of a vapor/liquid separator depends on a number of factors.
Before making a vessel design one has to decide on the configuration of the vessel
with respect to among others:
▪ Orientation
▪ Type of feed inlet
▪ Type of internals
▪ Type of heads
Factors that help to make the choice between the various alternatives are
discussed in this chapter.
Page | 144
5.9.2 Feed Inlet

Inlet Nozzle
The feed nozzle size and the type of feed inlet device (if any) have an impact
on the vapor / liquid separation that can be achieved. The feed nozzle is
normally sized to limit the momentum of the feed. The limitation depends
on whether or not a feed inlet device is installed.
Inlet device
Various inlet devices are available to improve the vapor / liquid separation.
Among others the following inlet devices may be installed:
▪ a deflector baffle
▪ a slotted tee distributor
▪ a half-open pipe
▪ a 90 ° elbow
▪ a tangential inlet with annular ring
▪ a schoepentoeter
For vertical drums, preferably a deflector baffle or a half open pipe shall be selected.
In case of a slug flow regime in the inlet piping, or if a high liquid separation
efficiency is required, a tangential inlet nozzle with annular ring can be used.
However, in case a high liquid removal efficiency is required, the application of a
wire mesh demister is preferred.
For horizontal drums normally a 90° elbow or a slotted diverter is installed. In some
cases, a submerged inlet pipe is installed, but this shall not be done in the case of a
two-phase feed.
Normally the selected inlet device for a horizontal drum shall be: a 90° elbow or a
slotted diverter in case of an all liquid or vapor-liquid feed a submerged pipe when
the feed is a subcooled liquid and the mixing of liquid and blanket gas is to be
minimized two 90° elbow inlets in case of high vapor loads.
Internals
After passing through the feed inlet, the vapor stream will still contain liquid in the
form of droplets. The maximum size of these entrained droplets depends on the
vapor up flow velocity. A separation device can reduce this entrainment
significantly. Wire mesh demisters are the most commonly used as separation
device. They are used for two reasons:
1. To minimize entrainment of the drum services having such a requirement,
suction drums for reciprocating compressors are the most notable examples.
2. To reduce the size of a vessel.
The allowable vapor velocity in a drum can be increased significantly by using a

wire mesh demister. So, when sizing is governed by vapor-liquid separation
criteria, this will result in a smaller diameter of the vessel
Major disadvantages of wire mesh demisters are:
▪ They are not suitable for fouling services
▪ Their liquid removal decreases significantly at reduced throughput
Page | 145
Although the size of the vessel often can be reduced by applying a wire mesh
demister, there are also many services where there is normally no demister
installed. Reflux accumulators, for example, seldom have mist eliminators. There
are several other types of mist eliminators such as vanes, cyclones, and fiber beds.
They are used when conditions are not favorable for wire mesh screens. Selection
criteria for these types of internals are the required efficiency, capacity, turndown
ratio, maximum allowable pressure drop and fouling resistance. These types
however will not be further addressed in this design guide.
Vessel Head
Most vessels have 2:1 elliptical head, welded to the shell of the vessel. However, in
some cases other types of heads are used. The major alternatives are:
▪ Flat heads in case of small vertical vessels (diameter less than
approximately 30”) often a flanged top head is used, which also serves to
provide access to the vessel. Depending on the pressure rating, this type of
head can either be flat or elliptical and shall be selected in consultation
with the mechanical engineer Hemispherical heads.
▪ A hemispherical head should be considered for an extremely large, high-
pressure vessel.
▪ A dished head should be considered in the case of a large diameter, low-
pressure vessel.
5.10 Theory of Vertical Separators

In the case of a vertical separator, the liquid droplets settle out in a direction
opposite to the direction of vapour flow. Therefore, the liquid will not disengage
from the vapour unless the vapour velocity is lower than the liquid settling velocity.
That is,
v max  v s Equation 3.2
Despite the fact that vertical separators are a less efficient alternative than
horizontal ones with an appropriate L/H ratio, they do offer some distinct
advantages which have seen them favored for applications as fuel gas and
compressor suction KO drums. Such advantages are detailed in section 3.4.
5.10.1 Orientation of the Vessel

The selection of the orientation of a gas-liquid separator depends on several factors.
Both vertical and horizontal vessels have their advantages. Depending on the
application one has to decide on the best choice between the alternatives.
Advantages of a vertical vessel are:

▪ A smaller plot area is required (critical on offshore platforms).
▪ it is easier to remove solids.
▪ liquid removal efficiency does not vary with liquid level because the area in
the vessel available for the vapor flow remains constant.
generally, the vessel volume is smaller.
Page | 146
Advantages of a horizontal vessel are:

▪ it is easier to accommodate large liquid slugs;
▪ less head room is required;
▪ the downward liquid velocity is lower, resulting in improved de-gassing
and foam breakdown;
additional to vapor / liquid separation also a liquid / liquid separation can
be achieved (e.g. by installing a boot).
▪ The preferred orientation for a number of typical vapor / liquid separation
applications are:
Application Preferred orientation

Reactor Effluent Separator (V/L) Vertical
Reactor Effluent Separator (V/L/L) Horizontal
Reflux Accumulator Horizontal
Compressor KO Drum Vertical
Fuel Gas KO Drum Vertical
Flare KO Drum Horizontal
Condensate Flash Drum Vertical
Steam Disengaging Drum Horizontal
5.10.2 Theory of Separators Applied To V-L Systems

In reality, the maximum allowable vapour velocity for liquid-vapour systems is
highly dependent on the specific separator application and indeed is vastly
different, for example, in cases where a demister pad is installed and cases where
one is not. Such flexibility is not catered for using Equations 3.1 and 3.2, where it is
not possible to effectively take into consideration any variation in separator
characteristics. Instead, a more appropriate equation to use for calculating the
maximum allowable vapour velocity for vapour-liquid systems is as follows:
(l − v )
vmax = K Equation 3.3
v
Where vmax = Maximum allowable vapour velocity, m/s
K = Empirical constant, m/s
l = Density of liquid phase, kg/m3
v = Density of vapour phase, kg/m3
A range of values for K are available for use in the above equation, as illustrated in
the following table taken from figure 7-9 of GPSA (SI units) Volume 1, Section 7,
page 7-7.
Page | 147
Table- 3.1
Typical K & C Factors for Sizing Woven Wire Demisters
Separator Type K Factor (m/s) C Factor (m/hr)
Horizontal 0.12 to 0.15 420 to 540
Vertical 0.05 to 0.11 200 to 400
Spherical 0.05 to 0.11 220 to 400
Wet Steam 0.076 270
Most vapours under vacuum 0.061 220
Salt & Caustic Evaporators 0.046 160
Adjustment of K & C Factor for
Pressure - % of design value.
Atmospheric 100
1000 kPa 90
2000 kPa 85
4000 kPa 80
8000 kPa 75
For glycol and amine solutions, multiply K by 0.6 to 0.8.

Typical use one-half of the above K or C values for approximate sizing of vertical
separators without wire demisters.
For compressors suction scrubbers and expander inlet separators multiply K by
0.7 to 0.8.
Advantages & Disadvantages of Horizontal / Vertical Separators

There are many factors
Horizontal Separators - Advantages:
▪ High separation efficiency due to higher vapour space volumes and vapour
residence times.
▪ Lower nozzle outlet elevations
▪ More applicable for use as reflux accumulators, which can be more readily
attached to and supported by horizontal separators.
▪ More suitable than vertical separators for handling large total liquid
volumes.
▪ May be used in applications requiring 3-phase separation.
Horizontal Separators – Disadvantages:

▪ Larger footprint area required than for vertical separators.
▪ Become less economical than vertical separators for high vapour / liquid
ratios.
Vertical Separators – Advantages

▪ Less potential for entrainment of liquid in vapour stream. Unlike a
horizontal separator, the area available for vapour flow is not reduced when
the liquid level rises during operation.
▪ Less footprint area required.
▪ Easier installation and operation of level alarms and shutdown control
systems.
▪ Generally, a lower cost option than horizontal separators.
▪ More efficient than horizontal separators for high vapour / liquid ratios.
Page | 148
Vertical Separators – Disadvantages

Not generally recommended for three-phase separation unless the total liquid
fraction present in the feed stream is very low (10 – 20% by weight).
Less suitable for a feed with a high liquid/vapour ratio.
5.10.3 Separator Sizing Principles

Vertical Vapour-Liquid Separators
Sizing Diameter
For a vertical separator, the vessel diameter required is determined by first
calculating the maximum allowable vapour velocity, (using equation 3.3) before
using the following equation:
4.Q
d min = Equation 5.1
 .vmax
Where dmin = Minimum Vessel Diameter (m)
Q = Vapour Flowrate (m3/s)
vmax = Maximum Vapour Velocity (m/s)
The vessel diameter should be selected as the next largest pipe/drum size to the
dmin value calculated, where deemed practical.
Sizing Vessel Length Amongst the most important factors required for
consideration when designing the length of a proposed vertical separator, are:
▪ The location of various liquid levels inside the vessel (LLSD, LLL, NLL, HLL,
HLSD, etc.).
▪ The location of inlet and outlet nozzles
▪ The surge volume required to permit corrective action to be taken by plant
operators in times of unsatisfactory plant operation. Such information is
usually provided by the vendor or based upon experience gained in sizing
similar vessels in the past.
Whether or not a demister pad is to be installed.
The following recommendations can be made regarding vessel shell lengths which
will assist the process engineer in addressing the important issues listed above.
The low liquid level (LLL) should be a minimum of 300 mm above the bottom
vessel tangent line. The precise level height may depend on the nature of level
control instruments available.
The high liquid shutdown (HLSD) level should be no less than 300 mm below the
inlet feed distributor / nozzle.
The shell length between the HLL and LLL should be set so as to provide sufficient
liquid surge volume.
The shell length between the HLSD and HLL should be made sufficient to provide
the operator with sufficient time to shut down the separator before the
performance and operation of downstream processes and equipment is
compromised.
Page | 149
The minimum T/T length of the vessel should be 2500 mm.
The clearance between the bottom of the demister pad and the top of the feed
distributor should be set at 70% of the vessel diameter or 750 mm, whichever of
the two is greater.
The clearance between the upper tangent line and the top of the demister pad
should be 10% of the vessel ID or 300 mm, whichever of the two is greater.
Following figure, adapted from GPSA (SI Units) Volume 1, Section 7, depicts an
example of a typical vertical separator containing a wire mesh mist extractor, in
which the above-mentioned recommendations have been adhered to.
Page | 150
h1: Low Liquid Level to Bottom Tangent Line

For operating pressure less than 1000 psig (70 barg), it is taken as 6 inch (150 mm) else it
is kept 12 inch (300 mm).
h2: Level Range

It is calculated based on holdup time required and slug capacity of the separator. Holdup
volume is calculated based on liquid flowrate multiplied by holdup (residence) time.
Minimum height is taken as 18 inch (450 mm) for proper level control.
h3: High Liquid Level to Inlet Nozzle

For separator with half pipe at inlet nozzle it is taken as maximum of 0.3D or 12 inch (300
mm).
h4: Diameter of Inlet Nozzle

This height is taken based on outside diameter of inlet nozzle.
h5: Inlet nozzle to Mist Eliminator/ Top Tangent Line

For separator without mist eliminator this height is taken as maximum of 0.9D or 36 inch
(900 mm). For separator with mist eliminator this height is taken as maximum of 0.45D or
24 inch (600 mm).
h6: Height of Mist Eliminator

Height of mist eliminator is typically 6 inch (150 mm).
h7: Mist Eliminator to Top Tangent Line

This height is taken as maximum of 0.15D or 12 inch (300 mm).
All heights are summed up to calculate overall length of separator. L/D ratio is typically
kept in the range of 3 to 5. If it is out of this range, new diameter is selected and all above
steps are repeated till desired L/D ratio is obtained.
5.10.4 Sizing Demister Pads

Mist extractors of the mesh-type are typically constructed of a pad of compact
stainless steel wire designed to capture entrained liquid droplets or those droplets
too small to settle by gravity. The liquid droplets impinge on the mesh pad, coalesce
and fall downward as larger droplets, back through the rising vapour. Demister
pads are generally aligned horizontally in both vertical and horizontal separators,
with the vapour and entrained liquid passing vertically upward through the pad. In
fact, the pad performance is found to be adversely affected if tilted at an angle of
greater than 30 degrees from the horizontal.
Page | 151
Figure 5-34 Alignment of demister pad
As reported by GPSA (SI) volume 1, most installations use a 150 mm thick pad with
the minimum recommended thickness being 100 mm. In order to size the diameter
of a demister pad, the following correlation may be used:
1
−
4.Q   l −  v  2
d=  
 .K   v
(Equation 5.4)

Where: Uv= superficial velocity of vapour through the demister pad (m/s).
K = Empirical constant, provided by vendor, but usually in the range of 0.1
– 0.12 m/s.
Q = Vapour flowrate (m3/s)
l = Density of liquid phase (kg/m3)
v = Density of vapour phase (kg/m3)
The diameter of the mist extractor is usually substantially less than the diameter
of the separator. In the case of vertical separators with diameters less than 1000
mm, a mesh diameter equivalent to the vessel diameter should be used. In
addition, the demister pads are typically located 300 mm below the vapour outlet
nozzle of a horizontal separator.
For any variety of service, the material of construction for the mesh pad should be
at least 304 ss. For application in corrosive service, either 316 ss or Monel mesh
pads should be used.
Page | 152
5.10.5 Control facilities

The required process conditions in a column are determined by the composition of
the feed mixture and the required specifications for the top and bottom product. In
order to achieve the desired separation, the column must operate under
equilibrium conditions.
The evaporator must steadily supply the required heating energy.

The pressure in the column must be held constant.
The condensation of the vapour must be correctly controlled.
The flows must be fed and drawn steadily.
Instruments for the following problem definitions are required:
▪ Feed flow control and control of product draws from the column: distillate,
side streams and bottom products.
▪ Level control and heat supply control from steam or hot oil.
▪ Cooling of the condenser and the after coolers for the products.
▪ Column pressure control.
Page | 153
Calculations of sextuple effect backward

evaporator :-
V1 V2 V3 V4 V5
V6
S
1 2 3 4 5 6
L1 L2 L3 L4 L5 L6 F
A Sextuple-effect rising-film evaporator is to concentrate a 10 per cent

solution of Vinasse to 70 per cent. The feed is to be at 40 °C and contains 49
tons vinasse per hour. Steam is available at 200 Kpa, and the last efect will
be assumed to be operated at vacuum of 15.01 Kpa. Overall Heat-transfer
coefficients may be assumed to be U1 = 1300, U2 = 1300, U3 =1400 U4 =1400,
U5 =1500, U6 =1500W/m2·K
Vinasse Solution has a Boiling point rise which can be calculated from
the next empirical correlation :-
valid for 6 % < S< 75 %
Page | 154
heat capacity of vinasse can be calculated according to the next

empirical correlation
cp,solid was calculated as a mean value for two different vinasses to

1270 J/(kg K)
Solution:-
Solute Balance:
𝑋𝐹 𝐹 = 𝑋1 𝐿1
∴ .7 ∗ 49 = .1𝐿1 ∴ 𝐿1 = 7 𝑡𝑜𝑛𝑠/ℎ𝑜𝑢𝑟
Over-all Material Balance:
𝐹 = 𝐿1 + Σ 𝑉
∴ Σ 𝑉 = 42 𝑡𝑜𝑛𝑠/ℎ𝑟
Assume initially equal rate of evaporation .
∴ 𝑉1= 𝑉2= 𝑉3= 𝑉4= 𝑉5= 𝑉6= 7 𝑡𝑜𝑛𝑠/ℎ𝑟
Mass Balance on each effect :-
𝐹 = 𝐿6 +𝑉6
𝐿6 = 𝐿5 + 𝑉5 𝐿6 = 42 t/hr
𝐿5 = 𝐿4 + 𝑉4 𝐿5 = 35 𝑡/ℎ𝑟
𝐿4 = 𝐿3 + 𝑉3 𝐿4 = 28 t/hr
Page | 155
𝐿3 = 𝐿2 + 𝑉2 𝐿3 = 21 t/hr
𝐿2 = 𝐿1 + 𝑉1 𝐿2 = 14 𝑡/ℎ𝑟
𝐿1 = 7 𝑡/ℎ𝑟
Solute Balance on each effect:-
𝑋2 𝐿2 = 𝑋1 𝐿1 𝑋2 =.35
𝑋3 𝐿3 = 𝑋2 𝐿2 𝑋3 =.233
𝑋4 𝐿4 = 𝑋3 𝐿3 𝑋4 =.175
𝑋5 𝐿5 = 𝑋4 𝐿4 𝑋5 =.14
𝑋6 𝐿6 = 𝑋5 𝐿5 𝑋6 =.1166
𝑥
𝐵𝑃𝑅 = 4.04 ∗ 10−5 ( )𝑇𝑏𝑤 2
100 − 𝑥
Σ Δ𝑇 = 𝑇𝑠 − 𝑇𝑉6 − Σ𝐵𝑃𝑅 = 44.891

Assume that the heat transfer area in all effects is equal
∴ 𝑈Δ𝑇 = 𝑐𝑜𝑛𝑠𝑡
1
𝑈𝑖
Δ𝑇𝑖 = Σ Δ𝑇
1 1 1 1 1 1
+ + + + +
𝑈1 𝑈2 𝑈3 𝑈4 𝑈5 𝑈6
Page | 156
10438.8781
Δ𝑇𝑖 =
𝑈𝑖
𝑇1 = 𝑇𝑆 − Δ𝑇1 =112.17°C
𝑇2 = 𝑇1 − 𝐵𝑃𝑅1 − Δ𝑇2 = 91.03°C
𝑇3 = 𝑇2 − 𝐵𝑃𝑅2 − Δ𝑇3 = 80.556°C
𝑇4 = 𝑇3 − 𝐵𝑃𝑅3 − Δ𝑇4 = 71.393°C
𝑇5 = 𝑇4 − 𝐵𝑃𝑅4 − Δ𝑇5 = 63.242°C
𝑇6 = 𝑇5 − 𝐵𝑃𝑅5 − Δ𝑇6 = 55.368°C
𝑇𝑉1 = 𝑇1 − 𝐵𝑃𝑅1 = 99.06°C
𝑇𝑉2 = 𝑇2 − 𝐵𝑃𝑅2 = 88.012°C
𝑇𝑉3 = 𝑇3 − 𝐵𝑃𝑅3 = 78.849°C
𝑇𝑉4 = 𝑇4 − 𝐵𝑃𝑅4 = 70.201°C
𝑇𝑉5 = 𝑇5 − 𝐵𝑃𝑅5 = 62.327°C
𝑇𝑉6 = 𝑇6 − 𝐵𝑃𝑅6 = 54.627°C
100 − 𝑥 𝑥
𝐶𝑃,𝑣𝑖𝑛𝑎𝑠𝑠𝑒 = ( ) ∗ 𝐶𝑝,𝑤𝑎𝑡𝑒𝑟 + ( )𝐶
100 100 𝑝,𝑠𝑜𝑙𝑖𝑑𝑠
Page | 157
latent heat of Enthalpy of vapor

vaporization
Ts=120.2 2202
𝑇𝑉1 =99.06 2259 2702
𝑇𝑉2 =88.01 2288 2666
𝑇𝑉3 =78.85 2311 2647
𝑇𝑉4 =70.2 2333 2631
𝑇𝑉5 =62.33 2352 2616
𝑇𝑉6 =54.63 2371 2602
energy balance:-
𝑠𝜆𝑠 + (𝐶𝑝2 𝑇2 − 𝐻1 )𝐿2 = (𝐶𝑝1 𝑇1 − 𝐻1 )𝐿1
(𝜆1 − 𝐶𝑝2 𝑇2 + 𝐻2 )𝐿2 + (𝐶𝑝3 𝑇3 − 𝐻2 )𝐿3 = 𝜆1 𝐿1
−𝜆2 𝐿2 - (𝜆2 − 𝐶𝑝3 𝑇3 + 𝐻3 )𝐿3 + (𝐶𝑝4 𝑇4 − 𝐻3 )𝐿4 =0
−𝜆3 𝐿3 - (𝜆3 − 𝐶𝑝4 𝑇4 + 𝐻4 )𝐿4 + (𝐶𝑝5 𝑇5 − 𝐻4 )𝐿5 =0
−𝜆4 𝐿4 - (𝜆4 − 𝐶𝑝5 𝑇5 + 𝐻5 )𝐿5 + (𝐶𝑝6 𝑇6 − 𝐻5 )𝐿6 =0
−𝜆5 𝐿5 - (𝜆5 − 𝐶𝑝6 𝑇6 + 𝐻6 )𝐿6 = −(𝐶𝑝𝐹 𝑇𝐹 − 𝐻6 )𝐿6
Page | 158
s l2 l3 l4 l5 l6 const
2202 -2413 0 0 0 0 -17229219
0 4636.005 -2382 0 0 0 15813000
0 -2287 4650 -2383 0 0 0
0 0 -2311 4678 -2390.22 0 0
0 0 0 -2333 4708 -2402.45 0
0 0 0 0 -2352 4739.839 119813771
s 9083.609
l2 15429.48
l3 23391.32
l4 30836.1
l5 37734.66
l6 44002.69
S=9083.608 kg/hr
V1=8429.48 kg/hr
V2=7961.84 kg/hr
V3=7444,78 kg/hr
V4=6898,56 kg/hr
V5=6268,03 kg/hr
V6=4997.31 kg/hr
𝑠𝜆𝑠 = 𝑈1 𝐴1 ∆𝑇1
𝑉1 𝜆1 = 𝑈2 𝐴2 ∆𝑇2
𝑉2 𝜆2 = 𝑈3 𝐴3 ∆𝑇3
𝑉3 𝜆3 = 𝑈4 𝐴4 ∆𝑇4
𝑉4 𝜆4 = 𝑈5 𝐴5 ∆𝑇5
𝑉5 𝜆5 = 𝑈6 𝐴6 ∆𝑇6
𝐴1 = 532.3 𝑚2
𝐴2 = 506.84 𝑚2
𝐴3 = 484.234 𝑚2
Page | 159
𝐴4 = 457.33 m2
𝐴5 = 428.063 m2
𝐴6 = 392.798 𝑚2
Since areas are not close, then another trial should be done
TRIAL 2:
new material balance using the computed L values
𝐴𝑚 = 466.9
𝐴
Δ𝑇𝑛𝑒𝑤 =Δ𝑇𝑜𝑙𝑑
𝐴𝑚
1 2 3 4 5 6
9.15 , 8.81, 7.832, 7.403, 6.835, 6.272
𝑇1 = 𝑇𝑆 − Δ𝑇1 =111.05°C
𝑇2 = 𝑇1 − 𝐵𝑃𝑅1 − Δ𝑇2 = 89.13°C
𝑇3 = 𝑇2 − 𝐵𝑃𝑅2 − Δ𝑇3 = 78.69°C
𝑇4 = 𝑇3 − 𝐵𝑃𝑅3 − Δ𝑇4 = 69.798°C
𝑇5 = 𝑇4 − 𝐵𝑃𝑅4 − Δ𝑇5 = 61.9007°C
𝑇6 = 𝑇5 − 𝐵𝑃𝑅5 − Δ𝑇6 = 54.7896°C
𝑇𝑆 = 120.2°C
𝑇𝑉1 = 𝑇1 − 𝐵𝑃𝑅1 = 97.94°C
𝑇𝑉2 = 𝑇2 − 𝐵𝑃𝑅2 = 86.522°C
𝑇𝑉3 = 𝑇3 − 𝐵𝑃𝑅3 = 70.858°C
𝑇𝑉4 = 𝑇4 − 𝐵𝑃𝑅4 = 62.395°C
𝑇𝑉5 = 𝑇5 − 𝐵𝑃𝑅5 = 61.0616°C
𝑇𝑉6 = 𝑇6 − 𝐵𝑃𝑅6 = 54°C
Page | 160
s l2 l3 l4 l5 l6
2202 -2380.46 0 0 0 0 -17230668
0 4632.986 -2380.37 0 0 0 15834000
0 -2292 4643.15 -2372.705 0 0 0
0 0 -2331.5 4687.516 -2380.426 0 0
0 0 0 -2352 4730.22 -2402.547 0
0 0 0 0 -2355.07 4743.879 127278804
s 9387.8636
l2 15922.472
l3 24338.481
l4 32247.123
l5 39662.539
l6 46520.339
S=9387.5674 kg/hr
V1=8922.198 kg/hr
V2=8415.749 kg/hr
V3=7908.398 kg/hr
V4=7412.993 kg/hr
V5=6862.877 kg/hr
V6=2477.785 kg/hr
𝐴1 = 482.72𝑚2
𝐴2 = 489.4 𝑚2
𝐴3 = 488.6 𝑚2
𝐴4 = 494 m2
𝐴5 = 472.38m2
𝐴6 = 477.19 𝑚2
𝐴𝑚 = 484 𝑚2
𝐴𝑜𝑣𝑒𝑟𝑑𝑒𝑠𝑖𝑔𝑛 = 533 𝑚2
D tube=.05 m
Number of tubes=340
Page | 161
EES:code for Sexstuple effect evaporator:-

"P[0]=200" "steam pressure"
Duplicate i=0,7
x[i]=1
End
x[11]=0
"last effect pressure"
x[9]=1
Tv[0]=Temperature(Steam,P=P[0],x=x[0])
Tv[9]=Temperature(Steam,P=P[9],x=x[9])
"P[9]=10"
L[0]=28
S[6]*L[6]=S[0]*L[0] "solute balance"
Duplicate i=1,5
L[i]=L[i+1]+V[i+1]
End
L[0]=L[6]+sumV "overall material balance"
Duplicate i=1,6
V[i]=sumV/6
End
S[6]=.4
S[0]=.08
Duplicate i=1,5
S[i]*L[i]=S[i+1]*L[i+1]
End
T_bw=373
Duplicate i=1,6
BPR[i]=4.04*10^(-5)*(100*S[i]/(100-S[i]*100))*T_bw^2
End
m=SUM(BPR[1..6])
Sum_T=Tv[0]-Tv[9]-m
invU[1]=1/2200
invU[2]=1/2200
invU[3]=1/2100
invU[4]=1/2100
invU[5]=1/2000
invU[6]=1/2000
L=SUM(invU[1..6])
U[1]=2200
U[2]=2200
U[3]=2100
U[4]=2100
U[5]=2000
U[6]=2000
Duplicate i=1,6
delta[i]=(Sum_T/U[i])/L
End
BPR[0]=0
T[1]=Tv[0]-BPR[0]-delta[1]
Duplicate i=1,5
T[i+1]=T[i]-BPR[i]-delta[i+1]
End
Duplicate i=1,6
Tv[i]=T[i]
End
C_pwater=4200
Cpsolids=1270
Duplicate i=1,6
C_P[i]=(((100-100*S[i])/100)*C_pwater+(100*S[i]/100)*Cpsolids)/1000
Page | 162
End
Duplicate i=1,6
hfg[i]=Enthalpy(Steam,T=Tv[i],x=x[0])-Enthalpy(Steam,T=Tv[i],x=x[11])
End
Duplicatei=1,6
g[i]=Enthalpy(Steam,T=Tv[i],x=x[0])
End
Duplicatei=1,6
hv[i]=g[i]+C_P[i]*BPR[i]/1000
End
T[0]=110
hfg[0]=Enthalpy(Steam,T=Tv[0],x=x[0])-Enthalpy(Steam,T=Tv[0],x=x[11])
"steam" "L1" "L2"
"L3" "L4"
"L5"
M[1,1]=hfg[0]; M[1,2]=-(C_P[1]*T[1]-hv[1]); M[1,3]=0;
M[1,4]=0; M[1,5]=0;
M[1,6]=0
M[2,1]=0; M[2,2]=-(hfg[1]-C_P[1]*T[1]+hv[2]); M[2,3]=-((C_P[2]*T[2])-hv[2]);
M[2,4]=0; M[2,5]=0;
M[2,6]=0
M[3,1]=0; M[3,2]=hfg[2]; M[3,3]=-(hfg[2]-
C_P[2]*T[2]+hv[3]); M[3,4]=-((C_P[3]*T[3])-hv[3]); M[3,5]=0;
M[3,6]=0
M[4,1]=0; M[4,2]=0 ; M[4,3]=hfg[3];
M[4,4]=-(hfg[3]-C_P[3]*T[3]+hv[4]); M[4,5]=-((C_P[4]*T[4])-hv[4]);
M[4,6]=0
M[5,1]=0; M[5,2]=0; M[5,3]=0;
M[5,4]=hfg[4]; M[5,5]=-((hfg[4]-C_P[4]*T[4]+hv[5]));
M[5,6]=-((C_P[5]*T[5])-hv[5])
M[6,1]=0; M[6,2]=0 ; M[6,3]=0;
M[6,4]=0; M[6,5]=hfg[5];
M[6,6]=-((hfg[5]-C_P[5]*T[5]+hv[6]))
Y[1]=-((C_P[1]*T[1])-hv[1])*L[0]; Y[2]=-hfg[1]*L[0];
Y[3]=0; Y[4]=0; Y[5]=0;
Y[6]=((C_P[6]*T[6])-hv[6]);
Duplicatei=1,6
Y[i]=sum(M[i,k]*J[K],K=1,6)
End
J[7]=L[6] "product"
Duplicatei=2,6
J[i]=J[i+1]+R[i+1] "R3 is V2 .... ..... ....."
End
L[0]=J[2]+R[2] "R2 is V1"
J[1]=R[1] "steam amount v0"
Duplicatei=1,6
1000*R[i]*hfg[i]/3.6=U[i]*A[i]*delta[i]
End
Am=Average(A[1],A[2],A[3],A[4],A[5],A[6])
"new trial"
"Sn[6]=.4"
"Sn[0]=.08"
Sn[0]*L[0]=Sn[1]*J[2]
Duplicate i=2,5 "check 5 0r 6 0 or 1"
Sn[i]*J[i]=Sn[i+1]*J[i+1]
End
Duplicate i=1,6
BPRn[i]=4.04*10^(-5)*(100*Sn[i]/(100-Sn[i]*100))*T_bw^2
End
Duplicate i=1,6
deltaNEW[i]=delta[i]*A[i]/Am
Page | 163
End
BPRn[0]=0
Tn[0]=T[0]
Tn[1]=Tv[0]-BPR[0]-deltaNEW[1]
Duplicate i=1,5
Tn[i+1]=Tn[i]-BPRn[i]-deltaNEW[i+1]
End
Duplicate i=1,6
Tvn[i]=Tn[i]
End
Duplicate i=0,6
C_Pn[i]=(((100-100*Sn[i])/100)*C_pwater+(100*Sn[i]/100)*Cpsolids)/1000
End
Duplicate i=1,6
hfgn[i]=Enthalpy(Steam,T=Tvn[i],x=x[0])-Enthalpy(Steam,T=Tvn[i],x=x[11])
End
Duplicatei=1,6
gn[i]=Enthalpy(Steam,T=Tvn[i],x=x[0])
End
Duplicatei=1,6
hvn[i]=gn[i]+C_Pn[i]*BPRn[i]/1000
End
"steam" "L1" "L2"
"L3" "L4"
"L5"
Mn[1,1]=hfg[0]; Mn[1,2]=-(C_Pn[1]*Tn[1]-hvn[1]); Mn[1,3]=0;
Mn[1,4]=0; Mn[1,5]=0;
Mn[1,6]=0
Mn[2,1]=0; Mn[2,2]=-(hfgn[1]-C_Pn[1]*Tn[1]+hvn[2]); Mn[2,3]=-((C_Pn[2]*Tn[2])-
hvn[2]); Mn[2,4]=0; Mn[2,5]=0;
Mn[2,6]=0
Mn[3,1]=0; Mn[3,2]=hfgn[2]; Mn[3,3]=-(hfgn[2]-
C_Pn[2]*Tn[2]+hvn[3]); Mn[3,4]=-((C_Pn[3]*Tn[3])-hvn[3]); Mn[3,5]=0;
Mn[3,6]=0
Mn[4,1]=0; Mn[4,2]=0 ; Mn[4,3]=hfgn[3];
Mn[4,4]=-(hfgn[3]-C_Pn[3]*Tn[3]+hvn[4]); Mn[4,5]=-((C_Pn[4]*Tn[4])-hvn[4]);
Mn[4,6]=0
Mn[5,1]=0; Mn[5,2]=0; Mn[5,3]=0;
Mn[5,4]=hfgn[4]; Mn[5,5]=-((hfgn[4]-C_Pn[4]*Tn[4]+hvn[5]));
Mn[5,6]=-((C_Pn[5]*Tn[5])-hvn[5])
Mn[6,1]=0; Mn[6,2]=0 ; Mn[6,3]=0;
Mn[6,4]=0; Mn[6,5]=hfgn[5];
Mn[6,6]=-((hfgn[5]-C_Pn[5]*Tn[5]+hvn[6]))
Yn[1]=-((C_Pn[1]*Tn[1])-hvn[1])*L[0]; Yn[2]=-hfgn[1]*L[0];
Yn[3]=0; Yn[4]=0; Yn[5]=0;
Yn[6]=((C_Pn[6]*Tn[6])-hvn[6]);
Duplicatei=1,6
Yn[i]=sum(Mn[i,kn]*Jn[Kn],Kn=1,6)
End
Jn[7]=L[6] "product"
Duplicatei=2,6
Jn[i]=Jn[i+1]+Rn[i+1] "R3 is V2 .... ..... ....."
End
L[0]=Jn[2]+Rn[2] "R2 is V1"
Jn[1]=Rn[1] "steam amount v0"
Duplicatei=1,6
1000*Rn[i]*hfgn[i]/3.6=U[i]*An[i]*deltaNEW[i]
End
Amn=Average(An[1],An[2],An[3],An[4],An[5],An[6])
q=sum(Rn[i]*hfgn[i]/3.6,i=1,5) +(Jn[1]*hfg[0]/3.6)
qa=Jn[1]*hfg[0]/3.6
Page | 164
Duplicate i=0,6
RHO[i+1]=(957+506*S[i]+.00011*(100*S[i])^2)
End
Duplicate i=1,6
rhosteam[i]=Density(Steam,T=Tvn[i],h=hvn[i])
End
Duplicate i=1,6
h100[i] = 44100*(100*Sn[i])^(-0.836)
end
"pressure drop calculations"
"Liquid"
Duplicate i=1,6
PL[i]=Pressure(Steam,T=T[i],x=x[11])
End
Duplicate i=1,5
deltaPL[i]= PL[i+1]- PL[i]
End
"vapor"
Duplicate i=1,6
Pv[i]=Pressure(Steam,T=Tv[i],x=x[0])
End
Duplicate i=1,5
deltaPv[i]= Pv[i+1]- Pv[i]
End
"sizing pipes"
Duplicate i=1,6
spv[i]=Volume(Steam,T=Tvn[i],h=hvn[i])
End
Duplicate i=1,6
IDS[i]=595*sqrt(Rn[i+1]*spv[i]/35)
End
IDS[0]=595*sqrt(Jn[1]*spv[0]/30) "steam inlet pipe diameter"
spv[0]=Volume(Steam,T=Tv[0],x=x[1])
Duplicate i=2,7
IDv[i]=595*sqrt(Jn[i]/RHO[i]*1.5) "2-p1...3-p2...4-p3.........product"
End
IDv[1]=595*sqrt(L[0]/RHO[1]*1.5) "Feed pipe diamter"
"separator sizing"
Duplicate i=1,6
veldesign[i]=.75*.04*sqrt((RHO[i]/rhosteam[i])-1)
End
Duplicate i=1,6
veslD[i]=sqrt(4*Rn[i]/(3.14*veldesign[i]))
End
"SI UNITS"
Duplicate i=1,7
JnSI[i]=Jn[i]/3.6
End
Duplicate i=1,7
RnSI[i]=Rn[i]/3.6
End
Page | 165
CHAPTER 6: CARBON DIOXIDE LIQUEFACTION UNIT
6 CHAPTER 6: CARBON DIOXIDE LIQUEFACTION UNIT
6.1 INTRODUCTION
Carbon dioxide (CO2) is the third-most abundant gas available in the air. CO2 content
of the atmospheric air ranges from 300 to 600 ppm (by volume) depending on the
measurement location on the earth. CO2 is an important constituent in the life cycle
of animals and plants. Naturally available CO2 gas is used in the photosynthesis
process by plants that are the basic sources of food. The decay (slow oxidation) of
all organic materials gives off CO2. In the respiratory action (breathing) of all
animals and humans, CO2 is released during exhalation. Plants also release some
amount of CO2 when they respire during night. CO2 is cycled through the oceans.
CO2 content of the oceans is about 60 times that of the atmosphere. Volcanic
eruptions may also release CO2. In addition, CO2 is released by a wide variety of
industries due to processing and due to the use of fossil fuels such as coal. Though
CO2 is a normal constituent of exhaled air, high concentration of CO2 gas is
hazardous, even lethal. A concentration of 3.5% CO2 (by volume) in air will cause
deeper breathing, and a concentration of 25% CO2 (by volume) can cause death of
humans. Importantly, continued increase of ambient CO2 content is believed to be
the main cause for global warming.
Industrially manufactured CO2 is used in solid, liquid, gas, and supercritical forms
in widely diversified commercial applications such as making explosive gas
atmospheres inert, beverage carbonation, chemical manufacturing, firefighting,
food preservation, foundry-mold preparation, greenhouses, mining operations, oil
well secondary recovery, rubber tumbling, pH depression for wastewaters, welding,
therapeutically work, and medical industry applications.
Fossil fuel fired plants are responsible for the one third of the CO2 emissions which
are thought to be a major contributor to the current rise in the earth’s surface
temperature. Reducing CO2 atmospheric concentrations by capturing emissions at
the source (power plants and chemical industries) and then storing them in
subsurface reservoirs is thought to be a reliable solution. The captured CO2 could
also be utilized for enhanced oil recovery, enhanced coal bed methane recovery,
enhanced gas recovery, food processing applications, manufacturing minerals and
fertilizer (e.g., urea production), promoting algae growth, and enhanced plant
growth in greenhouses. Currently, technologies are available to purify naturally
occurring CO2 into products suitable for the above applications.
Page | 166
6.2 Air pollution

Air pollution is defined as the presence of liquid, gaseous, or solid substances in the
air in quantities that cause many biological, economic and physiological damage,
affecting both humans, animals and plants. It should be noted that it is one of the
worst air pollutants, in this article we will inform you of its causes, damages, and
ways to reduce it.
Reasons for air pollution:
There are many natural factors that lead to air pollution, sources that have no
human income, and difficult to control, and divided into:
1. Basic pollutants:
▪ Oxides: They are caused by the burning of fuel, such as oil, coal or
natural gas, in full combustion, resulting in the production of carbon
dioxide, water vapor, sulfur dioxide, nitrogen oxides, heavy metals, Such
as cadmium, lead, and mercury.
▪ Volatile Organic Compounds: Vehicles that originate from vehicle
exhausts or from burning coal, such as methane and chloroform.
▪ Suspended compounds and droplets are solids in the air, such as germs,
dust, salts, and lead.
2. Secondary pollutants:
▪ Smog, acid rain and ozone are caused by the reaction of the main air
pollutants to each other, or with other contaminants, or with the sun, or
water.
▪ Such as some trades and different industries.
▪ Means of transport, air, and land.
▪ Agricultural activity, and frequent use of chemicals for fertilization and
agriculture purposes.
▪ Radioactivity resulting from atomic explosions.
Damage to air pollution:

▪ Lead to gastrointestinal diseases, respiratory, skin diseases, and eye
diseases.
▪ Causes many physiological changes to the animal and human, some
irritants may cause inflammation of the mucous surfaces.
▪ Reduces the proportion of oxygen in the inhaled air, due to increased
hydrogen content, or carbon dioxide in the body.
▪ It prevents blood from extracting oxygen from the inhaled air and
prevents tissue from absorbing oxygen in the blood.
▪ Affects the blood group.
▪ Slows down plant and animal life.
▪ Increases the average rainfall, soil moisture.
Page | 167
6.3 Carbon dioxide

Carbon dioxide (chemical code: CO2) is a colorless and non-flammable gas at normal
temperature and pressure. Although much less abundant than nitrogen and oxygen
in Earth's atmosphere, carbon dioxide is an important constituent of our planet's
air.
Carbon dioxide is an important greenhouse gas that helps to trap heat in our
atmosphere. Without it, our planet would be inhospitably cold. However, a gradual
increase in CO2 concentrations in Earth's atmosphere is helping to drive global
warming, threatening to disrupt our planet's climate as average global
temperatures gradually rise.
Carbon dioxide is the fourth most abundant component of dry air. It has a
concentration of about 400 ppmv (parts per million by volume) in Earth's
atmosphere. Scientists estimate that before human industrial activity, CO2
concentration was around 270 ppmv. Carbon dioxide levels in our atmosphere have
thus risen about 40% since the onset of human industrialization and are expected
to play a troubling role in raising global temperature. Atmospheric carbon dioxide
concentrations have varied substantially in the pre-human history of our planet and
have had profound impacts on global temperatures in the past.
❖ LATEST MEASUREMENT:
in March 2019: 410 ppm
Figure 6-1 Carbon dioxide levels in the atmosphere
Page | 168
Carbon dioxide plays a key role in Earth's carbon cycle, the set of processes that
cycle carbon in many forms throughout our environment. Volcanic outgassing and
wildfires are two significant natural sources of CO2 in Earth's atmosphere.
Respiration, the process by which organisms liberate energy from food, emits
carbon dioxide. When you exhale, it is carbon dioxide (amongst other gases) that
you breathe out. Combustion, whether in the guise of wildfires, as a result of slash-
and-burn agricultural practices, or in internal combustion engines, produces carbon
dioxide.
Photosynthesis, the biochemical process by which plants and some microbes create
food, uses up carbon dioxide. Photosynthetic organisms combine CO 2 and water
(H2O) to produce carbohydrates (such as sugars) and emit oxygen as a by-product.
Places such as forests and areas of the ocean that support photosynthetic microbes
therefore act as massive carbon "sinks", removing carbon dioxide from the
atmosphere via photosynthesis. Earth's early atmosphere had much higher CO2
levels and almost no oxygen; the rise of photosynthetic organisms led to an increase
in oxygen which enabled the development of oxygen-breathing creatures such as
us!
Burning generates CO2, although incomplete combustion due to limited oxygen

supply or an excess of carbon can also produce carbon monoxide (CO). Carbon
monoxide, a dangerous pollutant, eventually oxidizes to carbon dioxide.
6.3.1 Discovery of carbon dioxide

Carbon dioxide was discovered at the beginning of the 17th century by the Belgian
chemist Jan Baptiste van Helmont, who observed the presence of this gas at the time
of fermentation and combustion. By the middle of the 20th century, most of the
dioxide Carbon in liquid form.
6.3.2 Properties of carbon dioxide

Carbon dioxide can be derived in solid, liquid, gas, or supercritical state. Figure 6-3
shows the phase diagram of CO2 indicating the pressure and temperature ranges
for solid, liquid, gas, and supercritical forms of CO2. Gaseous CO2 is the most popular
and well-known form compared to the others. CO2 is a colorless gas with a faintly
pungent odor and has an acid taste. It is 1.53 times heavier than air at normal
temperature and pressure. CO2 has several special properties such as non-oxidizing
quality, inhibitive and partial disinfecting action on certain bacteria, and ability to
stimulate taste sensation, and thus, CO2 has found applications in various food and
processing industries.
Page | 169
Physical properties
Carbon dioxide is converted into liquid form when the pressure reaches 75 kg / cm3,
31 ° C, 16-24 kg / cm3, temperature between -23 and -12 ° C, and when cooled
Carbon dioxide is converted to dry ice and is used in fire extinguishers. It is stored
under extreme pressure in red cylinders of varying sizes. Its principle is to deplete
oxygen, which is one of the three main factors of fire formation: heat, fuel, oxidation),
And carbon dioxide comes out very cold from the extinguishers, which helps to
extinguish the fire.
Chemical properties
There are multiple chemical properties of carbon dioxide, including:
▪ A molecule of carbon dioxide (CO2) is made up of one carbon atom
and two oxygen atoms.
Figure 6-2 Molecule of carbon dioxide
▪ Carbon dioxide is an inactive gas at normal temperatures. If it is

exposed to a temperature higher than 1.700 °C, it decomposes to
carbon monoxide and oxygen. It also interacts with carbon or
hydrogen to produce carbon monoxide under high temperature.
Ammonia with carbon dioxide having pressure to produce
ammonium carbonate, and then urea.
▪ Carbon dioxide is an important component in the manufacture of
fertilizers and plastics.
▪ Carbon dioxide is soluble in water, forming a weak acid called
carbonic acid (H2CO3).
Figure 6-3 Phase diagram of carbon dioxide
Page | 170
6.4 Sources of carbon dioxide

1. Rocking of rocks
Carbonates are exposed to limestone to the air, and precipitation of
precipitation, as the earth progresses in age due to tectonic processes or
changes in sea level. Carbonic acid is formed by dissolving carbon dioxide in
water, causing the melting of carbon rocks.
2. Breathing and decomposition
Carbon dioxide is released when living organisms breathe, and during
cellular respiration, ie, cell respiration, to produce the energy needed by
living organisms by integrating glucose and oxygen from the air, and then
turning to energy, and carbon dioxide when the cell breathes. Breathing is
also known , As the process by which organisms decompose, when the death
of organisms is degraded by bacteria, thereby releasing carbon dioxide in the
atmosphere and water.
3. Human Resources
▪ Use of fossil fuels in power plants, industry and agriculture
Despite calls by those interested in environmental issues to switch to
renewable energy sources, many countries, especially the major
industrialized countries, have not been able to change their
traditional energy sources to renewable sources of energy. Fossil
fuels still account for a high proportion of energy sources in all
countries. Power plants currently operating mainly rely on coal, gas
and oil and consume millions of tons of fossil fuels to provide power
to factories, farms, homes, etc. The burning of fossil fuels is an
important and essential part of the energy sources used in industrial
and agricultural production in all countries. This increased fuel
combustion certainly leads to increased concentrations of
atmospheric carbon dioxide (CO2) in the atmosphere and is an
important source of this gas. This source did not have a significant
impact before the industrial revolution on CO2 concentration rates
due to weak industrial and mechanical industrial production. On the
other hand, the increase in population was not impressive at the
beginning of the industrial revolution.
The doubling of the world's population over the past two centuries
has led to a significant and significant increase in human
consumption of fossil fuels to meet the rising human needs of energy.
The improvement in the standard of living of the individual as a result
of scientific and cultural development has played an important role
in increasing its consumption of energy by increasing its use of
equipment and tools, which led to a very large increase in the volume
of industrial production. The massive population growth was
accompanied by a dramatic increase in the volume of agricultural
production in order to secure the human needs of food, clothing and
other necessities.
Page | 171
Figure 6-4 Carbon dioxide from fossil fuel combustion
Figure 6-5 Human sources of carbon dioxide
▪ Miscellaneous household uses

The population of the globe is currently more than 6 billion people
spread across six continents, almost all of which rely on electric
power produced in power plants to meet their growing daily needs in
various life magazines such as cooking, bathing, heating, lighting.
The modern lifestyle, especially in industrialized and developed

countries, made the use of electrical appliances (television,
calculator, refrigerator, washing machine, iron, etc.) an indispensable
daily need. This situation has increased the human consumption of
energy, which comes directly from the burning of fossil fuels in homes
as it is in the heating and cooking using natural gas or indirectly
through the consumption of electric power produced in power plants.
The population explosion and the increasing need for energy have led
to an increase in the consumption of fossil fuels, which is an
important factor in increasing the concentrations of greenhouse
gases in the planet's casing. The housing sector in the Arabian Gulf
region consumes about 49% of the total electricity produced in these
countries (Al-Nasser, 2009) Natural resources.
Page | 172
▪ In addition to the other sources mentioned above, natural

resources are responsible for the majority of atmospheric CO2
emissions, Including:
✓ oceans, where they provide the largest annual amount of
carbon dioxide, to any natural source, or human source.
✓ Forest fires, and emissions from volcanic eruptions.
Figure 6-6 Natural sources of carbon dioxide
4. Deforestation Carbon dioxide is released from trees when it is cut down for
the production of goods or heating, which is normally stored by trees, for
photosynthesis, according to research published by Duke University, and
annually releases about 1 billion tons of carbon in the atmosphere , Due to
deforestation, according to the Global Forest Resources Assessment in 2010.
Global industrial emissions of carbon dioxide are likely to have risen by 2.7% in
2018 to reach an all-time high, marking a second year of strong growth after a brief
period of relatively stable emissions, an international consortium of scientists'
reports.
The scientists said that deployment of renewable energies such as wind and solar
power is increasing rapidly around the world, but not fast enough to displace coal
use in places such as India and China or a growing global demand for oil and natural
gas.
The projections indicate that industrial CO2 emissions will hit an all-time high of
37.1 billion tones this year; the total, including CO2 emissions from deforestation
and other activities on land, will reach 41.5 billion tones — also the highest since
record began.
CO2 emissions grew by 1.6% in 2017. The spikes in 2017 and 2018 follow a three-
year period in which emissions growth slowed to a crawl (see ‘Carry on rising’).
Page | 173
Carry on rising
Industrial carbon dioxide emissions are projected to rise again globally this year,
even as individual countries' emissions look very different.
Figure 6-7 Industrial carbon dioxide emissions in different countries
“We had hoped that emissions had peaked beginning in 2014, but with strong
growth two years in a row, that is clearly incorrect,” says Rob Jackson, an Earth
scientist at
Stanford University in California and chair of the Global Carbon Project, which
tracks emissions and changes in the Earth's carbon cycle.
But the global economy is becoming more efficient, with economic growth
outpacing emissions; the researchers report that 19 countries experienced
economic growth while reducing their emissions over the past decade.
But it’s not enough for governments to just promote renewable energy, says Glen
Peters, a researcher at the Center for International Climate Research in Oslo who
worked on the emissions analysis. “We need more policies focusing on putting the
fossil fuels away,” he says, “but it’s much harder politically to penalize established
industries.”
Page | 174
The biggest driver of emissions growth is a rise in coal consumption in China, which
accounts for more than 46% of the projected increase in industrial CO2emissions in
2018.
India’s emissions rose by 6.3%, owing to strong economic growth and increasing
coal use. And in the United States, where emissions have fallen over the past decade,
they are projected to rise by around 2.5%, partly due to increased energy
consumption during a cold winter and hot summer.
Fossil-fuel infrastructure is still expanding, the scientists say, particularly in

developing countries. Overall, Jackson notes, humanity’s energy portfolio remains
as carbon intensive as it was three decades ago.
Peters says that the long-term trend is hard to decipher, because carbon emissions
still rise and fall on the basis of economic activity as well as weather trends. Since
2010, he says, global emissions growth has averaged about 1% per year, compared
with 3% per year in the 2000s. That’s progress, he adds, “but it’s still not good
enough”.
Table 6-1 Electrical energy produced by fossil fuel combustion
6.5 Source of carbon dioxide in the project

▪ Fermentation process
In brewing, alcoholic fermentation is the conversion of sugar into carbon
dioxide gas (CO2) and ethyl alcohol. This process is carried out by yeast cells
using a range of enzymes. This is in fact a complex series of conversions that
brings about the conversion of sugar to CO2 and alcohol. Yeast is a member
of the fungi family which I like to think of as plants but strictly they are
neither plant nor animal. To be specific yeast is a eukaryotic micro-
organism. Not all yeasts are suitable for brewing. In brewing we use the
sugar fungi form of yeast. These yeast cells gain energy from the conversion
of the sugar into carbon dioxide and alcohol. The carbon dioxide by-product
bubbles through the liquid and dissipates into the air. In confined spaces the
carbon dioxide dissolve in the liquid making it fizzy. The pressure builds up
caused by C02 production in a confined space can be immense. Certainly,
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enough to cause the explosion of a sealed glass bottle. Alcohol is the other
by-product of fermentation. Alcohol remains in the liquid which is great for
making an alcoholic beverage but not for the yeast cells, as the yeast dies
when the alcohol exceeds its tolerance level.
The overall process of fermentation is to convert glucose sugar (C6H12O6) to

alcohol (CH3CH2OH) and carbon dioxide gas (CO2). The reactions within the
yeast cell which make this happen are very complex, but the overall process
is as follows:
C6H12O6 ====> 2(CH3CH2OH) + 2(CO2) + Energy (which is stored in

ATP)
Sugar ====> Alcohol + Carbon dioxide gas + Energy
(Glucose) (Ethyl alcohol)
From the above it seems nice a simple chemistry one mole of glucose is
converted into two moles of ethanol and two moles of carbon dioxide but in
reality, it is far from this clear. There are many by products. In addition to
CO2 and alcohol, the sugar is incorporated into other by products such as
yeast biomass, acids (pyruvic, acetaldehyde, ketoglutaric, lactic), glycerol.
Hence if you read many home brewing books there is a table estimating the
conversion of sugar into alcohol. These tables tend to be derived from
measurements rather than a set formula. The efficiency of the yeast and
fermentation conditions alters the proportions of various by-products
meaning a simple single formula is not available. Wine makers will see
different efficiencies to beer makers. Fermentation conditions such as
temperature vary the production of byproducts. This knowledge is used by
wine makers to get fuller bodied wines by brewing in conditions that causes
fermentation to produce more of the by-product glycerol.
Fermentation by-product Glycerol gives wine its body. From time to time
you read in the press a very shocking tale of people adding anti-freeze to
wine but this statement on its own does not tell you the full extent of the
danger. Bear in mind Glycerol can be used as an anti-freeze and is a natural
byproduct of fermentation but not all anti-freeze use glycerol, most use very
toxic alternatives. So, the statement "Anti-freeze added to wine" does not tell
you if highly toxic chemicals were added or just Glycerol to supplementing
the natural Glycerol content. In fact, Glycerol is used in health foods and is
essential in fine wines. Wine produced in conditions where there was low
production of the glycerol by-product can tempt the producer to add
something to boost the wine's body. Adding food grade Glycerol to boost a
wine's body is not ideal but no need for panic as glycerol is natural and is
often used in food products. Adding toxic anti-freeze to boost a wine's body
can and does kill people.
❖ Note: The sugars used can be a range of fermentable sugars. These sugars
are converted by enzymes to glucose which is then converted to alcohol and
CO2. Some sugars are not able to be fermented and will remain in the liquid.
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CO2 Produced from Brewing
Figure 6-8 CO2 Produced from Brewing
6.6 Applications of Carbon Dioxide

6.6.1 Gas CO2
Carbonated Beverages
The most common and oldest application of CO2 is in producing
carbonated soft drinks and soda water. To some extent, this application
extends to beer and sparkling wine, though CO2 is naturally produced
during fermentation. The largest use of CO2 gas is in the manufacture of
carbonated In 1920s, about 90% of CO2 produced was used for the
manufacture of carbonated beverages in the U.S. Carbon dioxide
contributes to the characteristic pungent taste or “bite” to the soft drinks
because CO2 has a marked stimulating effect on the olfactory and
gustatory nerves.
The carbonation of a beverage helps to prevent mold growth. It also

inhibits the growth of bacteria, in some instances, destroys bacteria
depending on the extent of carbonation used. The acid used in the
beverage and the CO2 content satisfactorily preserve carbonated
beverages for a long time.
Modified Atmosphere Packaging / Controlled Atmosphere

Storage
When the concentration of CO2 increases beyond a certain level, it can
create a lethal effect on living beings. This property is effectively used to
protect grains, fruits, and vegetables from insects. It could be a practical
solution to replace the chemical fumigants used in grain industries.
Increasing the CO2 level in the surroundings of food material will prolong
their shelf-life with little or no adverse effect on quality. This technique
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usually named modified atmosphere packaging (MAP) or controlled

atmosphere storage (CAS). Previous literature reviews on this topic
confirm that MAP and CAS have been successfully tested and practiced in
many grains, fruits, vegetables, meats, and some processed food. Elevated
CO2 atmosphere finds a perfect fit in organic crops for non-chemical
preservation technology.
MAP or CAS is a potential chemical-free method of preserving fresh foods.

In MAP or CAS, the gaseous composition of the storage environment
around the food is altered by injecting either CO2 to create a high CO2
atmosphere, or N2 to create a low O2 atmosphere. Modified atmosphere
packaging is similar in principle to CAS, except in MAP the control of gas
concentration is less precise. In MAP, the gas composition is modified
initially, and it changes dynamically depending on the respiration rate of
the food product and the permeability of film or storage structure
surrounding the food product. In CAS, the gas atmosphere is continuously
controlled throughout the storage period.
Currently, CAS is used for controlling insect pests in stored grains for long-
term storage in Australia, USA, Canada, and several European nations. In
addition to providing an effective control of pests, CAS prevents mold
growth, preserves grain quality, and maintains a high germination
capacity of the stored grains. Disinfestation of stored grain using CAS
involves the alteration of the natural storage gases such as CO2, O2 and N2
to render the atmosphere in the stores lethal to pests. Controlled
atmosphere storage of grains is a suitable alternative to the use of
chemical fumigants and contact insecticides that are known to leave
carcinogenic residues in the treated product. CO2 affects complex
physiological processes in the insects and causes desiccation because
spiracles remain open and water loss cannot be regulated. For treatment
of stored grains with CO2 alone, the recommended dosages include 40%
CO2 for 17 days, 60% CO2 for 11 days, or 80% CO2 for 8.5 days at >21oC .
CO2 at and above 35% levels causes insect death by desiccation,
acidification at the cellular level, and creates a lack of triglycerides for
energy metabolism.
Inactivation of Microorganisms
In this section, inactivation of microorganisms using sub-critical CO2 gas
is presented. Later on, in a separate section, inactivation of
microorganisms using supercritical CO2 (temperature of ≥31.1oC and
pressure of ≥7.4 MPa) is discussed.
Combinations of carbon dioxide (30% CO2: 5% O2: 65% N2) and ethanol
(0.05%) or limonene (73 ppm) could inhibit the airborne microorganisms
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and Escherichia coli in ready-to-eat products stored at ambient pressure

and temperature.
Fraser (1951) was the first researcher who explored the application of
high-pressure CO2 for inactivating microorganisms. He found that high
pressure CO2 (3.4 MPa and 37oC) inactivated 95 to 99% of Escherichia
coli. Presence of CO2 under relatively mild pressures during heat
treatment can increase the rate of microbial inactivation. In this way, the
time and temperature for sterilization or pasteurization can be
significantly reduced. Use of pressurized CO2 in association with mild heat
treatment could provide an alternative to severe thermal processing often
responsible for degradation of nutritional qualities and changes in flavor
and texture of sensitive foods.
The U.S. Food and Drug Administration (FDA) has mandated

implementation of a Hazard Analysis Critical Control Point (HACCP)
program for processors of unpasteurized fruit and vegetable juices. The
core of the program depends on 5-log pathogen reduction. Therefore, in
most of the sterilization studies conducted using CO2, 5-log reduction in
the counts of microorganisms was the target.
At moderate temperature and pressure, CO2 is able to significantly

inactivate bacterial vegetative cells, molds and yeasts and, at suitable
conditions, CO2 can also inactivate intracellular and pectolytic enzymes.
The principal advantages of high-pressure CO2 are effective inactivation
of both airborne and exposed surface bacteria, as well as easy penetration
into porous materials to affect microbes inside the food. The principle of
high-pressure CO2 is based on gas dissolution in a cell by pressurization
that, when rapidly decompressed to atmospheric pressure, causes fatal
functional damage to the cell. Ballestra et al. (1996) reported that high
pressure CO2 treatment affects biological systems by causing protein
denaturation, lipid phase changes, and rupture of cell walls and
membranes. The literature review by Zhang et al. (2006) shows that high
pressure CO2 is a promising process medium to sterilize medical devices,
and liquid foodstuffs.
Inactivation of Enzymes
Lipolytic microorganisms such as psychrotrophic bacteria often are found
in fatty foods. These bacteria can produce lipase enzyme during storage.
The lipase enzyme can affect food quality. For instance, increased activity
of lipase enzyme can lead to rancidity of fatty foods.
Fadiloglu and Erkmen (2002) used CO2 gas at atmospheric pressure to

inactivate lipase enzyme. About 84% of initial activity of the enzyme was
lost at initial pH of 7.15 and 50oC within 5 min. This CO2 treatment under
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atmospheric pressure can be used as a potential non-thermal technique

for liquid food preservation. Also, this method may be an alternative to
pressure treatments (hydrostatic or CO2) in which extremely high
pressures are required for the inactivation of enzymes.
Perfusion of CO2 through immersion water, for reducing the oxygen

content, inhibited the enzymatic browning in pre-peeled potatoes without
any adverse effect on hardening. This may be due to the increase in acidity
of the water. This CO2 treatment was developed as an alternative to the
current sulfate treatment for inhibition of enzymatic browning of pre-
peeled potatoes.
In modified atmosphere packaging or controlled atmosphere storage, CO2

inactivates enzymes by dissolving in water present in the product.
Meat Industry
Carbon dioxide gas is commercially used for immobilizing animals prior
to slaughtering. Animals are led or driven into a tunnel in which CO2 gas
is injected. The animal falls unconscious onto a conveyor and is conveyed
directly to the slaughtering area. In this method, CO2 increases the
animal’s blood pressure, which helps recover more blood and results in
better quality meat (e.g., slower rate of pH decline) than other humane
slaughtering techniques. Also, CO2 is used for stunning of pigs. They found
that CO2 stunning yielded better meat quality compared to the usual
electrical stunning method.
A gas atmosphere containing 20% CO2 was found to be effective in

inhibiting the growth of slime-producing bacteria in meat at high storage
temperatures and high relative humidity. In Denmark, 42% of all retail
meat is packed under high CO2 atmosphere, following Denmark are U.K.
with 29%, France with 15%, and Germany with 5%.
Protein Precipitation
There are advantages to using CO2 instead of lactic or mineral acids for
casein precipitation. Because of relatively high residual pH of 6.0, the
whey would require less pretreatment for further processing and present
less of a disposal problem than conventionally produced whey with a pH
of 4.6.
High pressure CO2 can be used to precipitate soy protein. About 68.3 %
(by wt.) of soy protein was precipitated at 3.0 MPa of pressurized CO2, at
pH of 5.6, and at constant temperature of 22oC. Compared to the
conventional mineral oil-based precipitation technique, high pressure
CO2 precipitation is a clean process because this process produces highly
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purified food protein which needs no further treatments to purify the

product to be used in food or non-food applications.
High pressure CO2 was also used to precipitate protein constituents such
as glycinin and β-conglycinin from soybean.
Monitoring Food Quality

CO2 gas has not only been used to preserve and process the food products,
but it has also been used as an indicator for detecting quality changes in
food materials during processing and storage. Measuring the changes in
the CO2 concentration in grain storage bins, presence and growth of
insects and microorganisms such as fungi can be identified.
Measuring the CO2 gas produced from grains such as corn and wheat
during storage affected by moisture, temperature, and mechanical
damage, the amount of dry matter loss (i.e., deterioration) of grains can
be quantified. Therefore, relating CO2 content and grain quality would
help find the optimum grain storage conditions such as optimum moisture
and temperature, and manage the stored grain to preserve grain quality.
Miscellaneous Applications
Carbon dioxide has been used as a convenient inert medium for displacing
the air from bread manufacturing machinery, thus eliminating the dust
and bacteria carried by the air stream of the room.
Packaging food with CO2 can prevent oxidation of flavors and odors, and
vitamins in food products such as orange juice. By introducing CO2 while
churning, oxidation of the butter can be avoided, and the time to become
rancid may be delayed. Also, presence of CO2 gas can hasten the ripening
of citrus fruits, where CO2 was obtained from combustion gases from
kerosene.
In manufacturing of ice cream, CO2 is substituted for air before beating the
ice cream mix. Carbon dioxide increases mechanical strength of the ice
cream due to its greater solubility over air. Also, inclusion of CO2 helps
prevent oxidation, accentuates flavors, and has some bactericidal action
on the ice cream.
Carbon dioxide injection into an extrusion cooker was found to help

produce structured extrudates for wheat starch-sucrose mixtures under
low-temperature and high-moisture conditions. Similarly, carbon dioxide
is used at 0.1 to 0.6 MPa pressure to increase the expansion of pre-
gelatinized rice flour extrudates during twin-screw extrusion.
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Puffing of dehydrated, diced green bell peppers at a CO2 pressure of 6.48

MPa increased the bulk specific volume and rehydration ratio by 340 and
143%, respectively, compared to those of an air-dried process also CO2 is
used for puffing potato pieces. They also reported that the CO2 puffing
process resulted in higher bulk specific volume and rehydration ratio than
air-dried process.
CO2 has the ability to dissolve in materials and reduce their pH. This
characteristic can be used to prolong the membrane life in reverse
osmosis by introducing CO2.
Incorporating CO2 gas in milk before drying can increase the drying rate
by increasing the surface area.
6.6.2 Liquid CO2

Refrigeration
CO2 doesn’t exist in liquid form at ordinary atmospheric pressure and
temperature. It needs either very high pressure or very low temperature
or their combination to keep CO2 in liquid form. To use liquid CO2, a high
operating pressure is necessary which may require features like high
pressure joints leading to increased cost of the system. Though handling
high pressure CO2 raises some safety issues, it has been used widely in
food refrigeration. First, liquid CO2 was introduced as a refrigerant in
Europe and then in the U.S. Because of its inertness, liquid CO2 can be used
with any metal and any lubricating oil. Use of CO2 in mechanical
refrigeration systems has outstanding advantages such as safety from fire
explosion, and non-corrosiveness (Jones, 1923a). In addition, the inert
nature of CO2 gives more choices for construction material, and CO2 is low-
cost compared to NH3 and hydrofluorocarbons (HFCs). CO2 in
combination with NH3 would be a potential lower capital cost option for
low temperature applications. Today’s refrigeration industries code CO2
as R-744 refrigerant.
Liquid CO2 provides the most readily available method of obtaining rapid
refrigeration. CO2 manufacturers have developed refrigerated bulk-liquid
CO2 storage systems. Carbon dioxide refrigeration systems are used for
rapid chilling of loaded trucks and rail cars before shipment. Rapid cooling
and low cost of equipment are the two main factors for adopting liquid
CO2 refrigeration systems.
Curtis et al. (1995) first proposed the rapid cooling of shell eggs in a carton
using cryogenic gases (N2 and CO2), and showed it to be advantageous
over traditional refrigerated cooling to 7oC due to shorten cooling time.
The time required to equilibrate to 7oC is about 5 days for traditional
cooling and about an hour for cryogenic CO2 cooling.
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Cold storage of shell eggs at temperatures below 7oC results in

suppressing the growth of Salmonella enteritidis. Also, compared to the
traditional cooling methods, cryogenic carbon dioxide (-78oC) was found
to maintain or in some cases improve egg quality and increase shelf-life.
Quick Frozen Food Industry

The growing popularity of 'Quick Frozen Foods' throughout the world has
resulted in the phenomenal growth of this industry around the world.
Frozen sea foods top the global trade list, followed by 'ready-to-serve'
meals, vegetables, poultry-based foods, etc., The USA ranks first in the
world trade of frozen foods. European countries like Germany and UK are
also involved in the trade of frozen foods.
Quick freezing is a method of increasing the shelf-life of perishable foods

by subjecting them to conditions of temperatures below their freezing
point in a short period, say -20oC in 3 to 30 minutes to inhibit oxidative,
enzymatic, and microbial changes, which are responsible for the change
of flavor and color of foods and their spoilage. The process involves direct
immersion or indirect contact of foods with a refrigerant and the cold air
blasted over the foods being frozen. Because liquid CO2 provides a better
refrigerating effect at lower price, quick frozen food industries generally
use liquid CO2 based cryogenic freezing. It has been found that cryogenic
freezing provides the fastest rate for quick frozen foods.
Cryogenics
Cryogenics is defined as a branch of engineering specializing in technical
operations at very low temperatures of about -160oC to -50oC. Liquid
nitrogen and carbon dioxide (liquid or solid) are the two major cryogens
used for food applications. The total usable refrigeration effect available
in CO2, N2 and Freon-25 are 565, 690 and 287 kJ kg-1, respectively.
The quality of cryogenically frozen foods equals or exceeds that of

conventionally frozen foods, provided that the period of frozen storage is
limited to a few weeks or less and the temperature of frozen storage is -
18oC or lower. The cryogenic principle is applied for spice grinding and
freezing of foods to improve the organoleptic properties of the processed
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foods. Grinding of food in the presence of a cryogenic fluid is referred to

as cryo-grinding. Cryo-grinding of spices provides reduced oxidation of
spicy oil, extremely fine grinding, a 30% increase in product quality,
lowered microbial load, and causes no browning of spice. Cryo-grinding is
also applied for cocoa, coconut, chocolate, coffee, tea and dehydrated
meat. Liquid CO2 is commonly used for hamburger meat grinding
processes . Liquid CO2 is used to freeze the meat before grinding in order
to increase the grinding efficiency.
Cryogenic freezing and preservation of sea-foods, fruits, and vegetables

give reduced bacterial deterioration, reduced oxidation, better retention
of original color and texture, longer shelf-life, lower capital out lay, and
easy maintenance. Currently, cryogenic methods are used for peeling of
soft skinned fruits, and homogenization of biological tissues.
6.6.3 Solid CO2 (dry ice)

Dry ice is typically produced as solid blocks (30 kg) for the shipping industry, and
as cylindrical pellets (10-mm in diameter) for grocery and lab uses. Safe handling of
dry ice is important because dry ice can cause burns to the skin by merely touching
it.
Refrigeration
The first use of CO2 was started with refrigerating ice cream and meats
during 1920s in the form of solid CO2. The use of solid CO2 in refrigerated
transportation (truck, trailer and rail) has steadily increased from the
1960s. Solid CO2 has a greater refrigeration effect than ice made from
water because solid CO2 evaporates directly as a gas and it has an
extremely low temperature. Its low temperature makes it ideal for frozen-
food transportation. When it is used for fresh foods, the CO2 gas in the
atmosphere immediately surrounding the product serves to reduce the
oxygen content of the air, thus minimizing possible deterioration
resulting from oxidation. Also, it inhibits the growth and development of
bacteria and various molds that cause spoilage. Raspberries and
strawberries were shipped commercially under solid CO2 refrigeration
during 1940s. If the berries were cooled to 14.4oC and a CO2
concentration of 30 to 35% was maintained, no changes in flavor and
luster were observed.
Quick Frozen Food Industry

Dry ice is commonly used for transporting frozen foods. For instance, a
van-ceiling-mounted dry ice "bunker" system is presently operating
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commercially in the USA at a much lower cost of transportation of frozen

foods than that of the mechanical methods. Dry ice assisted rail shipment
of frozen-foods is also used for transporting to distant destinations.
Meat Industry
As discussed previously, one of the largest uses of dry ice is for the
refrigeration of meat products. The grinding of hamburger meat with the
addition of about 5% of dry ice increases the grinding capacity of the
machine and, the appearance and shelf-life of the product.
Miscellaneous Applications
Food products containing fat are apt to become rancid in the package. A
small quantity of CO2 in the package can act as an antioxidant. This applies
to coffee, nuts, and shredded coconut. Some coffee packers either put a
small pellet of solid CO2 into each cellophane bag/can just before filling,
or they pass CO2 gas into the container. A better textured product was
obtained by adding a small amount of solid CO2 in the bread dough, as the
dough cooled during the mixing. Dissolving 1.5% (by weight) CO2 into
grape juice completely inactivated microorganisms in a freshly pressed
juice . Dry ice can be added for carbonating water and juices prior to
consumption. Also, dry ice is being used for making ice cream.
In controlled atmosphere storage of grains, dry ice pellets or blocks can

be used as a source for CO2 gas.
6.6.4 Supercritical CO2

Carbon dioxide becomes supercritical when its temperature and pressure are
raised above the critical points. For CO2, the critical temperature (Tc) is 31.06oC and
the critical pressure (Pc) is 7.386 MPa. Supercritical CO2 at greater than 31.1oC and
pressures exceeding 7.4 MPa exists in a dense liquid state where the CO2 retains
the lower surface tension of a gaseous phase and the increased solubility of a liquid
phase. This supercritical state enables use of CO2 to extract various organic and
inorganic molecules, and to inactivate numerous microorganisms.
Supercritical CO2 Extraction

From the viewpoint of pharmaceutical, nutraceutical, and food
applications, supercritical CO2 is a good solvent, because it is relatively
inert, non-toxic, non-flammable, odorless, colorless, inexpensive,
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recyclable, readily available in high purity, and easy to remove from the
product (i.e., no chemical residue in the product).
Supercritical CO2 has a low critical temperature compared to other

supercritical chemicals such as propane (Tc = 96.7oC and Pc = 4.247 MPa),
which can help prevent thermal degradation of food components (e.g.,
carotenoids) while they are being extracted.
Supercritical CO2 has a higher diffusion coefficient and lower viscosity and
surface tension than a liquid solvent, which leads to a more favorable
mass transfer. However, supercritical CO2 cannot be used for dissolving
polar molecules because of its non-polar nature. For these situations,
addition of a polar co-solvent (e.g., ethanol) with supercritical CO2
enhances extraction efficiency. In addition, solubility of CO2 decreases
with increasing molecular weight. The major disadvantage is that
application of supercritical CO2 requires high pressure extraction vessels
leading to high capital and operating costs. However, costs of supercritical
extraction processes are competitive with other processes, and
sometimes supercritical processes are unique in their ability to produce
solvent-free products and handle high viscosity materials.
Because supercritical fluids have the solvating power of a liquid and

better mass transfer characteristics than traditional solvents, interest in
extraction with supercritical fluids has been growing rapidly in recent
years. Solvents such as ammonia, ethylene, toluene, and CO2 show
promise for supercritical fluid extraction. Of these, CO2 offers unique
advantages: it is abundant, non-reactive, non-toxic, and harmless. The
natural flavor and aroma of the extracts (e.g., oils) are preserved during
supercritical CO2 extraction since it is carried out at low temperatures (as
low as 31oC) and in an inert CO2 atmosphere.
Conventional extraction methods such as solvent extraction using Soxhlet

apparatus, although effective for extraction of oils, can lead to degradation
of heat sensitive compounds as well as leave traces of toxic solvents in the
solute. This is a concern for food and medicinal extracts. Supercritical CO2
extraction is a viable alternative to solvent extraction methods due to low
critical temperature (31.1oC). Moreover, supercritical CO2 extraction is a
popular technique for oil extraction due to its high extraction efficiency,
short extracting time, lower refining requirement, and absence of
chemical residues or contamination in the extracted oils.
Currently, commercial plants exist for decaffeinating coffee and tea,

extracting beer flavoring agents from hops, and separating oils and
oleoresins from spices using supercritical CO2. Supercritical CO2 replaces
water or methyl chloride for the extraction of these materials.
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Supercritical CO2 was used on a wide range of raw materials for: (i)
extraction of fats and oils, (ii) extraction of cholesterol, (iii) fractionation
of fats and oils, (iv) refining fats and oils (e.g., deacidification and
deodorization), (v) flavor/aroma extraction, and (vi) extraction of other
food constituents such as pigments and antioxidants. Selected examples
from the above categories, and additional applications of supercritical CO2
extraction from the recent literature are discussed below.
Supercritical CO2 has been used to extract oils from a variety of raw
materials such as peanut, almond, pistachio nut, wheat plumule, pecan,
egg yolk, garlic, hazelnut, and cotton seed. In addition, supercritical CO2
extraction of soybean oil, peanut butter, corn oil, evening primrose oil,
peppermint and spearmint oil, and fractional separation of marjoram
leaves and onion juice.
In the traditional solvent extraction plants, a great deal of money is spent

for removing the residual solvents in the extracts in order to use the
extract in food applications. Recently, supercritical CO2 extraction-based
techniques were developed to remove the residual chemicals from the
extracts obtained by traditional solvent extraction methods.
De-alcoholized wine or beer could be made by removing ethanol, where

ethanol is removed by supercritical CO2 in a stripping column. Also,
supercritical CO2 is used to extract flavor compounds from distillates of
beer produced by one-step evaporation. They concluded that the flavor
extracts are suitable for mixing with non-alcoholic beer. supercritical CO2
is used at (10 to 50 MPa pressure, 35 to 60oC, and 5 to 30 min) to extract
aroma from peels and pulp of passion fruit. Supercritical CO2 was found
to be the most effective in extracting off-flavor compounds (i.e., medium
chain aldehydes) from soybean protein among liquid CO2, supercritical
CO2, and supercritical CO2 with 5% ethanol.
Supercritical CO2 extraction can be used to extract natural colors from

leaf proteins. These colors can be used as food dyes. Supercritical CO2
extraction of annatto seeds gives carotenoid-type food colorant, used in
dairy products. Lycopene, a deep-red pigment and a natural anti-oxidant,
can be separated effectively from tomato peels by supercritical CO2
extraction. natural food colorants extracted (i.e., carotenoids) from carrot
using supercritical CO2 plus canola oil as a continuous co-solvent.
A liquid product can be entrapped by adsorption onto solid particles using

supercritical CO2, where the solid material provides a coating for the
liquid inside. An example of this is incorporation of tocopherol acetate in
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silica gel using supercritical CO2 (Brunner, 2005). This process is not
currently employed in food applications; however, this process can
potentially be used to add selective constituents in foods to enhance
quality and value.
In yeast inactivation, supercritical CO2 was found to be more effective

than the sub-critical state. In the supercritical state, it took only 15 min
compared to more than one hour in sub-critical state to inactivate the
yeasts. When high pressure CO2 in a supercritical state was used, it not
only destroyed the yeast but also removed the odor created by the broken
yeast cells. If the process temperature was less than 35oC, the protein
structure was retained.
Supercritical CO2 could also be used to sterilize milk and dairy products.
Werner and Hotchkiss (2006) studied the CO2-based sterilization of milk
to kill bacteria. The lethal effect of supercritical CO2 was found to be better
than sub-critical CO2. Continuous CO2 treatment is on par with or better
than the commonly used High Temperature Short Time (HTST) treatment
of milk. A carbon dioxide assisted milk pasteurization unit has been
developed in the United Kingdom.
Supercritical CO2 has been used to inactivate microorganisms in meat and

meat products. Is found that a CO2 pressure of 31.5 MPa and treatment
time of 120 to 180 min caused reduction of activity of Staphylococcus
aureus in ground beef. The supercritical CO2 treatment (7.4 to 15.2 MPa
at 31.1oC for 10 min) of pork samples had no effect on muscle pH,
tenderness, and water holding capacity; however, treated samples had
higher lightness values and more pronounced extent of sarcoplasmic
protein denaturation than the control samples.
6.6.5 Future Thrusts of CO2 in Food and Processing Industries

In the future, continued applications of gaseous CO2 in manufacturing carbonated
beverages, and modified atmosphere packaging/controlled atmosphere storage of
foods are expected. High pressure CO2 gas could be used for inactivating
microorganisms and enzymes in heat-sensitive foods. Applications of solid CO2
would be continued in refrigeration and frozen storage of foods. Applications of
liquid CO2 would be continued in the field of very low temperature applications (i.e.,
cryogenics).
Due to environmental and occupational concerns of using large amounts of toxic

organic solvents, liquid/supercritical CO2 would serve as an alternate, ideal solvent
for the future. Based on this review, we believe that commercial plants may be
founded for supercritical CO2 based inactivation of microorganisms in solid and
liquid foods.
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Commercial developments in the future might be expected to continue in the area

of food flavors, as well as in the extraction and refining of ”natural” food ingredients,
functional foods, alternative medicines, and specialty oils using supercritical CO2.
Also, supercritical CO2 applications could be extended to processes such as chemical
and enzymatic reactions, recrystallizations, supercritical fluid chromatography,
and extrusion technology.
6.7 Process equipment's

❖ The plant is designed for recovery of purified, high pressure liquid CO2
from impure ,low pressure CO2
CO2 comes from :(fermentation process)
What is liquification?
The liquification of gases is a complicated process that uses various compressions
and expansions to achieve high pressures and very low temperatures liquids.
The process of refrigerating a gas to a temperature below its critical temperature

so that liquid can be formed at some suitable pressure, also below the critical
pressure.
IMPURITIES:
Three kinds of impurities are present in raw CO2:
• Moisture
• Water Soluble
• Non-condensable gases
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6.7.1 Major Equipment & How the process occurs

1. BOOSTER FAN: To help move air through the ducts from fermenters.
2. LOW PRESSURE PRECOOLER: CO2 comes (impure & low pressure).
3. KNOCK-OUT DRUM
▪ Removes moisture.
▪ Water-Vapor separator.
▪ Demister ped is used to improve separation.
Figure 6-9 Demister ped
4. SCREW COMPRESSOR
▪ gate rotor & screw.
▪ Oil lubrication compressor: Used to increase the pressure of CO2.
Figure 6-10 Screw compressor structure
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▪ In this plant we used 2 stages the 1st one from 1bar to 6bar the
2nd one from 6 bar to 16 bar.
Figure 6-11 Oil lubrication compressor
5. SEPARATOR: The 2 stages Contain oil (lubricant &coolant).
6. HEATER & O2 TANK: Heater to make sure that reaction will occur O2 tank
with excess O2 to supply the reaction with enough oxygen to get rid of hydro
carbons and carbon monoxide.
7. CATOX ”reactor”: The equipment by which we can get rid of hydro

carbons by burning them with oxygen to be converted to CO2 with higher
purity.
8. AFTER COLEER: To decrease the temperature of CO2 comes from

separators “after compressors”.
Figure 6-12 After cooler
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9. HIGH PRESSURE SCRUBBER

▪ Remove water soluble impurities.
▪ Control current flow gas.
▪ Scrubbing liquid comes from nozzle to carry impurities then leave
from drain.
Figure 6-13 High pressure scrubber
10. HIGH PRESSURE PRECOOLER: To decrease the temperature of CO2.

11. TWIN TOWER DRAYER
▪ It’s automatic twin tower.
▪ contains molecular sieve dryer to dye CO2.
▪ final purification occurs by Activated carbon to remove any
Unpleasant odors.
Figure 6-14 Twin tower drayer
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12. CONDENSER: Single pass shell and tube heat exchanger that converts CO2
from gas to liquid.
Figure 6-15 Condenser
13. DISENGAGING CHMABER “gas- liquid separator”

▪ Liquid &Vaper CO2 enter to this chamber to be separated gas from top
and li quid from bottom Liquid-Vapor separator.
▪ Liquid &Vaper CO2 enter to this chamber to be separated gas from top
and li quid from bottom.
▪ Liquid-Vapor separator.
Figure 6-16 Gas- liquid separator
14. LIQUID FUEL PUMP: Takes liquid CO2 from disengaging chamber and
feeds CO2 to stripping column.
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15. REFLUX CONDENSER:

▪ Takes vaper CO2 from disengaging chamber.
▪ Decreases temperature of CO2 to condensate.
Figure 6-17 Reflux condenser
▪ Due to difference in dew point temperatures impurities “non-

condensable gases” leave from vent.
16. STRIPPING COLUMN

▪ Vapor stream passes over liquid stream.
▪ Stripping impure liquid CO2 is carried out by counter current
flowing pure CO2 vapor from Reboiler.
▪ CO2 gas venting from top is recondensated by reflux condenser.
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Figure 6-18 Stripping column
17. STORAGE TANK
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CHAPTER 7: AUXILIARY EQUIPMENT’S
7 CHAPTER 7: AUXILIARY EQUIPMENT’S

7.1 Cooling tower
7.1.1 INTRODUCTION
Cooling towers are a very important part of many chemical plants. The primary task
of a cooling tower is to reject heat into the atmosphere. They represent a relatively
inexpensive and dependable means of removing low-grade heat from cooling water.
The make-up water source is used to replenish water lost to evaporation. Hot water
from heat exchangers is sent to the cooling tower. The water exits the cooling tower
and is sent back to the exchangers or to other units for further cooling. Typical
closed loop cooling tower system is shown in Figure 7.1
Figure 7-1 Cooling water system
7.1.2 Cooling Tower Types

1. natural draft towers
2. Mechanical draft towers
1. Counter flows induced draft.
2. Counter flow forced draft.
3. Cross flow induced draft.
7.1.3 Components of Cooling Tower

The basic components of an evaporative tower are: Frame and casing, fill, cold
water basin, drift eliminators, air inlet, louvers, nozzles and fans.
Frame and casing: Most towers have structural frames that support the
exterior enclosures (casings), motors, fans, and other components. With
some smaller designs, such as some glass fiber units, the casing may
essentially be the frame.
Fill: Most towers employ fills (made of plastic or wood) to facilitate heat
transfer by maximizing water and air contact. Fill can either be splash or film
type. With splash fill, water falls over successive layers of horizontal splash
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bars, continuously breaking into smaller droplets, while also wetting the fill
surface. Plastic splash fill promotes better heat transfer than the wood
splash fill. Film fill consists of thin, closely spaced plastic surfaces over which
the water spreads, forming a thin film in contact with the air. These surfaces
may be flat, corrugated, honeycombed, or other patterns. The film type of fill
is the more efficient and provides same heat transfer in a smaller volume
than the splash fill.
Cold water basin: The cold water basin, located at or near the bottom of
the tower, receives the cooled water that flows down through the tower
and fill. The basin usually has a sump or low point
for the cold-water discharge connection. In many tower designs, the cold water
basin is beneath the entire fill.
Figure 7-2 Cooling tower types
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In some forced draft counter flow design, however, the water at the bottom of the
fill is channeled to a perimeter trough that functions as the cold-water basin.
Propeller fans are mounted beneath the fill to blow the air up through the tower.
With this design, the tower is mounted on legs, providing easy access to the fans
and their motors.
Drift eliminators: These capture water droplets entrapped in the air

stream that otherwise would be lost to the atmosphere.
Air inlet: This is the point of entry for the air entering a tower. The inlet
may take up an entire side of a tower–cross flow design– or be located low
on the side or the bottom of counter flow designs.
Louvers: Generally, crossflow towers have inlet louvers. The purpose of

louvers is to equalize air flow into the fill and retain the water within the
tower. Many counter flow tower designs do not require louvers.
Nozzles: These provide the water sprays to wet the fill. Uniform water
distribution at the top of the fill is essential to achieve proper wetting of the
entire fill surface. Nozzles can either be fixed in place and have either round
or square spray patterns or can be part of a rotating assembly as found in
some circular cross-section towers.
Fans: Both axial (propeller type) and centrifugal fans are used in towers.
Generally, propeller fans are used in induced draft towers and both
propeller and centrifugal fans are found in forced draft towers. Depending
upon their size, propeller fans can either be fixed or variable pitch. Afan
having non-automatic adjustable pitch blades permits the same fan to be
used over a wide range of kW with the fan adjusted to deliver the desired
air flow at the lowest power consumption. Automatic variable pitch blades
can vary air flow in response to changing load conditions.
7.1.4 Tower Materials

In the early days of cooling tower manufacture, towers were constructed primarily
of wood. Wooden components included the frame, casing, louvers, fill, and often the
cold-water basin.
If the basin was not of wood, it likely was of concrete. Today, tower manufacturers
fabricate towers and tower components from a variety of materials. Often several
materials are used to enhance corrosion resistance, reduce maintenance, and
promote reliability and long service life.
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Galvanized steel, various grades of stainless steel, glass fiber, and concrete are
widely used in tower construction as well as aluminum and various types of plastics
for some components.
Wood towers are still available, but they have glass fiber rather than wood panels
(casing) over the wood framework. The inlet air louvers may be glass fiber, the fill
may be plastic, and the cold-water basin may be steel.
Larger towers sometimes are made of concrete. Many towers–casings and basins–
are constructed of galvanized steel or, where a corrosive atmosphere is a problem,
stainless steel. Sometimes a galvanized tower has a stainless-steel basin. Glass fiber
is also widely used for cooling tower casings and basins, giving long life and
protection from the harmful effects of many chemicals.
Plastics are widely used for fill, including PVC, polypropylene, and other polymers.
Treated wood splash fill is still specified for wood towers, but plastic splash fill is
also widely used when water conditions mandate the use of splash fill. Film fill,
because it offers greater heat transfer
Efficiency is the fill of choice for applications where the circulating water is
generally free of debris that could plug the fill passageways.
Plastics also find wide use as nozzle materials. Many nozzles are being made of PVC,
ABS, polypropylene, and glass-filled nylon. Aluminum, glass fiber, and hot-dipped
galvanized steel are commonly used fan materials. Centrifugal fans are often
fabricated from galvanized steel. Propeller fans are fabricated from galvanized,
aluminum, or molded glass fiber reinforced plastic.
7.1.5 Cooling tower for fermentation section

In industrial ethanol fermentation the yeast cells are submitted to stresses, such as
ethanol and sugar concentrations and those originating from environmental
factors, operating conditions and physic-chemical factors such as temperature, pH
and salts concentration. Of these factors, temperature has the greatest effect on the
fermentation kinetics of the process and cell viability.
Temperature and ethanol can have synergistic effects on the dynamic behavior of
the fermentation process. Another consideration with regard to thermal stress is
the formation of by-products, such as glycerol and organic acids, mainly succinic
and acetic.
Studies have shown that the ideal fermentation temperature for increased
productivity and maintenance of cell viability is around 32◦C.
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The fermenting temperature cannot be higher than 32°C, as it should allow bacteria
to grow very fast which in turn would cause the adverse impact on fermentation
efficiency, the result is the reduction of ethanol yield of the plant.
it is recommended to use chilled water system in cooling of fermenters and mash.

Approximately 60-70% of total chilling water load is mostly used in fermentation.
Chiller system was designed that Chilled water inlet and outlet temperature were
12°C and 18°C respectively.
Figure 7-3 Cooling Tower and chiller plant piping
For Fermentor:
mm ̇ olasse = 1.5 kg/sec
ṁ biomass = 0.37 kg/sec
the growing microorganism 65 kj energy per mole of biomass
1332kg/hr of biomass produces 1 MW energy
Q grows
Q evap(water, ethanol)
Q excess = Q grows - Q evap = 1 MW
Q chilled water for 1 fermentor =300 TR
We have 10 fermentors with heat load 1MW, we have to cool the fermentors by
using 10 chillers, the capacity of the one chiller is 300 TR
By using EES program the heat load of the condenser of the chiller is 1191 kw, the
heat load for 10 condenser 11910 kw, the cooling towers cool the condenser of the
chiller
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Technical specification for the chiller

Flow rate of chilled water 43 ton/hr
Cooling agent (30-10) c
Flow rate of the refrigerant 6.89 kg/sec
Heat load of the condenser 1191 kw
Technical specification for the fermentation cooling tower

Flow rate of the water 570 kg/sec
Inlet water temperature 35 c
outlet water temperature 30 c
Wet bulb temperature 21 c
Dry bulb temperature 35 c
Heat load 11.91 MW
From the catalog of the evapco company, The selection of the cooling tower is:
AT 424 -236 (4 cells cooling tower)
model no. AT 424-236
Nominal tons* 2198
Shipping 20285
Weight(kg)
Operating 37195
Heavies section 3445

(upper)
Fan motor (kw) (4) 18.5
Air flow rate (𝑚3 /sec) 231.4
Ht 5347
T 2845
Dimensions(mm) P 3689
L 11030
O 216
Q 2743
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7.1.6 Cooling tower of rest all section

In this section the cooling tower cools the evaporation section and distillation
section
For evaporation section the flow rate of the water 140 ton/hr the difference
temperature 10 c (40 -30)
For distillation section we have 3 condenser to cool the ethanol the flow rate of the
water is 126 ton/hr and the difference temperature 10 c (40 -30)
Technical specification for the rest all cooling tower
Flow rate of the water 266 ton/hr
Inlet water temperature 40
outlet water temperature 30
Wet bulb temperature 24
Dry bulb temperature 35
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From the catalog of the evapco company ,The selection of the cooling tower is :
AT 28-921 (2 cell cooling tower )
model no. AT 28-921
Nominal tons* 554
Shipping 4125
Weight(kg)
Operating 7095
Heavies section 2340

(upper)
Fan motor (kw) (2)15.0
Air flow rate (𝑚3 /sec) 54
Ht 4105
T 2762
Dimensions(mm) P 2956
L 6401
O 565
Q 1594
Performance of the cooling tower:
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Fermentation C.T Rest all C.T

Cells number 4 2
Range 5 10
Approach 6 6
Cooling tower 45.4 % 62.5
effectiveness
Evaporation loss (𝑚3 /hr) 21.35 2.76
Drift loss (𝑚3 /hr) 0.02 0.00225
Windage loss (𝑚3 /hr) 10.26 1.33
Make up water (𝑚3 /hr) 31.36 4.1
Cycles of concentration 3.13 3.05
(c.o.c)
Blow down (𝑚3 /hr) 10.02 1.34
Fan motor (kw) (4) 18.5 (2) 15
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7.2 Boiler Selection

Boiler selection from:
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Models available:
▪ SG 600: up to 6.000 Kg/h
▪ SG 800: up to 8.000 Kg/h
▪ SG 1000: up to 10.000 Kg/h
▪ SG 1200: up to 12.000 Kg/h
▪ SG 1500: up to 15.000 Kg/h
▪ SG 2000: up to 20.000 Kg/h
▪ SG 2200: up to 22.000 Kg/h
▪ SG 2500: up to 25.000 Kg/h
Steam boiler STEAM-MATIC SG functional diagram
Figure 7-1 Steam boiler STEAM-MATIC SG functional diagram
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TECHNICAL SPECIFICATIONS:
Design Pressure is 12 Bar
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P&ID - STEAM-MATIC SG - BOILER ROOM
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UNIVERSAL steam boiler UL –S

The UNIVERSAL steam boiler UL -S is a three-pass shell boiler, which fulfils all the
requirements in the medium to high output ranges.
▪ Thought out to the final detail

The flame tube, the internal wet-back rear smoke gas reversing chamber, as
well as the first smoke tube and second smoke tube, are all arranged for
optimum flow within the horizontal cylindrical pressure vessel. Radiant and
convection heat surfaces generate in tandem a rapid water circulation,
which accelerates the steam bubble transport to the steam chamber. The
transferred fuel heat is converted into steam quickly and without material
stress through an even heat transfer. The large water chamber offers
sufficient storage volume to be able to cover off even sudden peaks in
consumption.
▪ Optimized efficiency
The flue gas flow from the steam boiler contains significant heat potential.
For an increased boiler efficiency this series of boiler is also available with
an integrated economizer for flue gas heat recovery. In addition the optional
modules for continuous feed water control, speed controlled burner fan and
O2 or CO control should also be used to give an even more efficient and
environmentally friendly operation.
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▪ Construction
Our three-pass patent dating from 1952 forms the basis for the outstanding
and ongoing success of this series.
The flame tube (first pass) and two smoke tube bundles (second and third
pass) are integrated with the wetback rear reversing chamber in the
pressure vessel in an ideal way. The laterally positioned flame tube, and the
horizontal rear and vertical front heating gas reversal produce a large
radiant and convection heating surface with a large steam chamber, and all
of this within the smallest dimensions. The floors are anchored stably by the
large continuous flame tube and they are connected with the boiler shell by
means of the cleverly devised use of corner anchors for even load
distribution.
❖ Note:
▪ Equipment level
You can obtain all our shell boilers inclusive of all equipment* as fully
functioning units. The basic equipment level includes the boiler pressure
vessel, the control and safety technology, the burner unit, a pump module, a
terminal box and the control switchgear cabinet including our easily
operated boiler control BCO. The integrated terminal box is already wired.
Pre-assembled, plug-in and coded cable bundles simplify the electrical
wiring installation between the boiler control cabinet and the terminal box.
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Associated boiler house components:

▪ Water treatment module WTM
▪ Water service module WSM
▪ Condensate service module CSM
▪ Blow-down, expansion and cooling module BEM
▪ Water analyzer WA
▪ Flue gas heat exchanger ECO 1, stand-alone
▪ Flue gas heat exchanger ECO 6 for condensing use
▪ Expansion and heat recovery module EHM
▪ Pump module PM
▪ Expansion, heat recovery and blow-down module EHB
▪ Vapour cooler VC
▪ Gas regulation module GRM
▪ Oil circulation module OCM
▪ Oil supply module OSM
▪ Oil preheater module OPM
▪ System control SCO
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CHAPTER 8: FIREFIGHTING
8 CHAPTER 8: FIREFIGHTING
8.1 Detectors
The four types of fire detectors are heat, ionization, photoelectric, and
ionization/photoelectric. The differences in each of these how they detect fires, heat
being from temperature, and the other three being from smoke. The best detector
is the combination ionization/photoelectric.
8.1.1 Heat Detector

Heat detectors detect the presence of heat and an increase in air temperature. These
detectors have few false alarms but, they take longer to identify a fire than a smoke
detector. They’re ideal in situations where smoke detectors may cause false alarms
such as steamy, humid, or dusty environments. Infrequently occupied areas like
storage facilities, warehouses, or machine rooms also use these types of detectors.
The three most common smoke detectors are ionization, photoelectric, and
combination ionization/photoelectric. All smoke detectors sound an alarm, when
they identify smoke, in order to notify a building’s occupants. What differentiates
these detectors from one another is the way that they detect smoke.
Ionization Smoke Detector

Ionization smoke detectors have a constant electrical current that occurs
between two metal plates in the device. When smoke enters the chamber, it
disrupts the electrical current and causes the alarm to sound. These
detectors are excellent at detecting fast burning fires.
Figure 8-1
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Photoelectric Smoke Detector

Photoelectric smoke detectors have a beam of light in the device and when
smoke scatters the light it causes the alarm to go off. This type of device is
quicker to identify small smoldering fires than an ionization smoke detector.
They’re extremely reliable and produce few false alarms.
Figure 8-2
Ionization/Photoelectric Smoke Detector

A combination smoke detector is the best way to protect your facility and its
occupants from a fire. When both forms of smoke detection are together on
one device it helps to ensure that regardless of the type of fire, it will be
detected as soon as possible.
Flame detector
A flame detector is a type of device that uses optical sensors in order to
detect flames. Essentially, there are seven different types of flame detectors
available. These types include ultraviolet, infrared, UV/IR, IR/IR, IR/IR/IR,
visible sensors and video cameras.
Ultraviolet detector
Ultraviolet detectors have the ability to detect fires and explosions in three
to four milliseconds. From the moment that a small flame has been ignited,
an ultraviolet detector can distinguish the type of flame. While incredibly
accurate, ultraviolet detectors can be fooled by sunlight, radiation,
arc welding, and lightning.
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Infrared flame detector

An infrared flame detector works by using an infrared band. When hot
gasses are released near an infrared detector, a small thermal
imaging camera immediately picks up on the presence of these gasses. On
occasion, other sources of hot gas that happen to be near an infrared flame
detector can cause this type of detector to set off a false alarm.
UV/IR detectors
UV/IR detectors use a combination of both ultraviolet and infrared technology to
detect heat. These detectors gather information from an ultraviolet perspective
and an infrared perspective. When these two technologies work together, false
alarms are often minimized
8.2 Foam
Foam: A firefighting foam is simply a stable mass of small air-filled bubbles, which
have a lower density than oil, gasoline or water. Foam is made up of three
ingredients - water, foam concentrate and air. When mixed in the correct
proportions, these three ingredients form a homogeneous foam blanket.
Foam solution: This is a solution of water and foam concentrate after they have
been mixed together in the correct proportions.
Foam concentrate: This liquid concentrate is supplied from the manufacturer

which when mixed with water in the correct proportion forms a foam solution
Finished foam: Foam solution as it exits a discharge device, having been aerated.
8.2.1 How foam extinguishes a flammable liquid fire

Fire burns because there are four elements present. These elements are heat, fuel,
air (oxygen) and a chemical chain reaction. Under normal circumstances if any one
of the elements is removed/interfered with, the fire is extinguished. Firefighting
foam does not interfere in the chemical reaction. Foam works in the following ways:
▪ The foam blankets the fuel surface smothering the fire
▪ The foam blanket separates the flames/ignition source from the fuel
surface
▪ The foam cools the fuel and any adjacent metal surfaces.
▪ The foam blanket suppresses the release of flammable vapors that can mix
with air.
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Before we review the different types of mechanical foam concentrates, please

understand that there are two different basic flammable or combustible fuel
groups:
▪ Standard hydrocarbon fuels such as gasoline, diesel, kerosene, jet fuel, etc.
These products do not mix with water or are not miscible in water, i.e. these
products all float on top of water and, for the most part, they do not intermix.
▪ Polar solvent or Alcohol type fuels are fuels that mix readily with water or
are miscible in water.
Following is a list of mechanical foam concentrates that are the most common
types currently used by fire fighters today:
▪ Aqueous Film Forming Foam (AFFF).
▪ Alcohol Resistant (AR-AFFF).
▪ Synthetic – medium or high expansion types (detergent).
▪ Class “A” Foam Concentrate.
▪ Wetting Agent.
▪ Fluoroproteins.
▪ Protein.
▪ Film Forming Fluoroproteins (FFFP).
8.2.2 Alcohol resistant-aqueous film forming foam (ar-afff)

AR-AFFF’s are available in a 3%-6% type or 3%-3% type concentrate. Flammable
liquids that readily mix with water are a more difficult fire to extinguish as opposed
to a hydrocarbon fire. Polar solvent/alcohol liquids destroy any foam blanket that
has been generated using standard AFFF or Fluoroproteins type concentrates.
Water in the generated foam blanket mixes with alcohol causing the foam blanket
to collapse and disappear until the fuel surface is completely exposed again. To
overcome this problem, AR-AFFF type concentrates were developed. Using plain
AFFF concentrate as a base material, a high molecular weight polymer is added
during the manufacturing process. When AR-AFFF is used on a polar solvent fuel
fire, the polar solvent fuel tries to absorb water from the foam blanket. A polymer
precipitates out forming a physical membrane/barrier between the fuel surface and
foam blanket. This barrier now protects the generated foam blanket from d.
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CHAPTER 9: TANKS
9 CHAPTER 9: TANKS
9.1 INTRODUCTION
Storage tanks containing organic liquids, nonorganic liquids, vapors and can be
found in many industries. Most storage tanks are designed and built to the American
Petroleum Institute API-650 specification.
These tanks can have different sizes, ranging from 2 to 60 m diameter or more. They
are generally installed inside containment basins in order to contain spills in case
of rupture of the tank.
Industries where storage tanks can be found are petroleum producing and refining,
petrochemical and chemical manufacturing, bulk storage and transfer operations,
other industries consuming or producing liquids and vapors.
9.2 Types of storage tanks

BASICALLY, THERE ARE EIGHT TYPES OF TANKS USED TO STORE LIQUIDS:
1. Fixed-roof tanks.
2. External floating roof tanks.
3. Internal floating roof tanks.
4. Domed external floating roof tanks.
5. Horizontal tanks.
6. Pressure tanks.
7. Variable vapor space tanks.
8. LNG (Liquefied Natural Gas) tanks
The first four tank types are cylindrical in shape with the axis oriented
perpendicular to the sub grade. These tanks are almost exclusively above ground.
Horizontal tanks can be used above and below ground. Pressure tanks often are
horizontally oriented and spherically shaped to maintain structural integrity at high
pressures. They are located above ground. Variable vapor space tanks can be
cylindrical or spherical in shape.
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CHAPTER 9: TANKS
9.2.1 Fixed-Roof Tank

Of currently used tank designs, the fixed-roof tank is the least expensive to construct
and is generally considered the minimum acceptable equipment for storing liquids.
A typical fixed-roof tank consists of a cylindrical steel shell with a cone- or dome-
shaped roof that is permanently affixed to the tank shell. Storage tanks are usually
fully welded and designed for both liquid and vapor tight, while older tanks are
often having a riveted or bolted construction and are not vapor tight.
A Breather Valve (pressure-vacuum Valve), which is commonly installed on many

fixed-roof tanks, allows the tank to operate at a slight internal pressure or vacuum
Figure 9-1 Breather Valve (pressure-vacuum Valve)
This Valve prevents the release of vapors during only very small changes in
temperature, barometric pressure, or liquid level, the emissions from a fixed-roof
tank can be appreciable.
Additionally, gauge hatches/sample wells, float gauges, and roof manholes provide
accessibility to these tanks and also serve as potential sources of volatile emissions.
9.2.2 External Floating Roof Tank

A typical external floating roof tank consists of an open-topped cylindrical steel
shell equipped with a roof that floats on the surface of the stored liquid, rising and
falling with the liquid level. The floating roof is comprised of a deck, fittings, and rim
seal system. Floating roof decks are constructed of welded steel plates and are of
three general types: pan, pontoon, and double deck. Although numerous pan-type
decks are currently in use, the present trend is toward pontoon and double-deck
type floating roofs.
Manufacturers supply various versions of these basic types of floating decks, which
are tailored to emphasize particular features, such as full liquid contact, load-
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CHAPTER 9: TANKS
carrying capacity, roof stability, or pontoon arrangement. The liquid surface is

covered by the floating deck, except in the small annular space between the deck
and the shell; the deck may contact the liquid or float directly above the surface on
pontoons.
External floating roof tanks are equipped with a rim seal system, which is attached
to the roof perimeter and contacts the tank wall. The rim seal system slides against
the tank wall as the roof is raised and lowered. The floating deck is also equipped
with fittings that penetrate the deck and serve operational functions. The external
floating roof design is such that evaporative losses from the stored liquid are limited
to losses from the rim seal system and deck fittings (standing storage loss) and any
exposed liquid on the tank walls (withdrawal loss).
9.2.3 Internal Floating Roof Tank

That tanks have both, a permanent fixed roof and a floating roof inside. There are
two basic types of internal floating roof tanks:
▪ tanks in which the fixed roof is supported by vertical columns within the
tank.
▪ tanks with a self-supporting fixed roof and no internal support columns.
The fixed roof is not necessarily free of openings but does span the entire open plan
area of the vessel. Fixed roof tanks that have been retrofitted to employ an internal
floating roof are typically of the first type, while external floating roof tanks that
have been converted to an internal floating roof tank typically have a self-
supporting roof.
Tanks initially constructed with both a fixed roof and an internal floating roof may
be of either type. An internal floating roof tank has both a permanently affixed roof
and a roof that floats inside the tank on the liquid surface (contact deck) or is
supported on pontoons several inches above the liquid surface (noncontact deck).
The internal floating roof rises and falls with the liquid level.
9.2.4 Domed External Floating Roof Tank

Domed external floating roof tanks have the heavier type of deck used in external
floating roof tanks as well as a fixed roof at the top of the shell like internal floating
roof tanks. Domed external floating roof tanks usually result from retrofitting an
external floating roof tank with a fixed roof.
As with the internal floating roof tanks, the function of the fixed roof is not to act as
a vapor barrier, but to block the wind. The type of fixed roof most commonly used
is a self-supporting aluminum dome roof, which is of bolted construction. Like the
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CHAPTER 9: TANKS
internal floating roof tanks, these tanks are freely vented by circulation vents at the
top of the fixed roof. The deck fittings and rim seals, however, are basically identical
to those on external floating roof tanks.
9.2.5 Horizontal Tank

Horizontal tanks are constructed for both above ground and underground service.
Horizontal tanks are usually constructed of steel, steel with a fiberglass overlay, or
fiberglass-reinforced polyester. Horizontal tanks are generally small storage tanks.
Horizontal tanks are constructed such that the length of the tank is not greater than
six times the diameter to ensure structural integrity. Horizontal tanks are usually
equipped with pressure-vacuum vents, gauge hatches and sample wells, and
manholes to provide accessibility to these tanks. In addition, underground tanks
may be cathodically protected to prevent corrosion of the tank shell. Cathodic
protection is accomplished by placing sacrificial anodes in the tank that are
connected to an impressed current system or by using galvanic anodes in the tank.
However, internal cathodic protection is no longer widely used in the petroleum
industry, due to corrosion inhibitors that are now found in most refined petroleum
products.
9.2.6 Variable Vapor Space Tank

Variable vapor space tanks are equipped with expandable vapor reservoirs to
accommodate vapor volume fluctuations attributable to temperature and
barometric pressure changes. Although variable vapor space tanks are sometimes
used independently, they are normally connected to the vapor spaces of one or
more fixed roof tanks. The two most common types of variable vapor space tanks
are lifter roof tanks and flexible diaphragm tanks. Lifter roof tanks have a
telescoping roof that fits loosely around the outside of the main tank wall. The space
between the roof and the wall is closed by either a wet seal, which is a trough filled
with liquid, or a dry seal, which uses a flexible coated fabric.
Flexible diaphragm tanks use flexible membranes to provide expandable volume.
They may be either separate gasholder units or integral units mounted atop fixed
roof tanks. Variable vapor space tank losses occur during tank filling when vapor is
displaced by liquid. Loss of vapor occurs only when the tank's vapor storage
capacity is exceeded.
9.2.7 LNG Storage Tank

A liquefied natural gas storage tank or LNG storage tank is a specialized type of
storage tank used for the storage of Liquefied Natural Gas. LNG storage tanks can
be found in ground, above ground or in LNG carriers. The common characteristic of
LNG Storage tanks is the ability to store LNG at the very low temperature of -162°C.
LNG storage tanks have double containers, where the inner contains LNG and the
outer container contains insulation materials. The most common tank type is the
full containment tank. Tanks are roughly 55 m (180 ft) high and 75 m in diameter.
Page | 227
CHAPTER 9: TANKS
In LNG storage tanks if LNG vapors are not released, the pressure and temperature
within the tank will continue to rise. LNG is a cryogen and is kept in its liquid state
at very low temperatures. The temperature within the tank will remain constant if
the pressure is kept constant by allowing the boil off gas to escape from the tank.
This is known as auto-refrigeration.
The world's largest above-ground tank (Delivered in 2000) is the 180 million liters
full containment type for Osaka Gas Co., Ltd. The world's largest tank (Delivered in
2001) is the 200 million liters Membrane type for Toho Gas Co., Ltd.
9.3 Floating Roof Tanks

9.3.1 History and Introduction
Floating roof tank was developed shortly after World War I by Chicago Bridge &
Iron Company (CB & I). Evaporation of the product in fixed roof caused a great lost
of money; this led to research to develop a roof that can float directly on the surface
of product, reducing the evaporation losses.
9.3.2 Principles of the Floating Roof

The floating roof is a circular steel structure provided with a built-in buoyancy
which allowing it to sit/ float on top of the liquid product in a close or open top tank.
The overall diameter of the roof is normally 400 mm smaller than the inside
diameter of the tank, which has about 200 mm gap on each side between the roof
and the inside tank wall.
This is due to the limitation on the accuracy of dimension during construction for
the large diameter tanks. The gaps allow the floating roof to rise and fall without
binding on the tank wall. To protect the product inside the tank from evaporation
to the atmosphere and contamination from the rainwater through the gaps between
the outer rim of the floating roof and the tank wall, the gaps will be closed or sealed
up by mean of flexible sealing system.
Due to environmental issue, selection of the roof seal is one of the major concerns
in the floating roof tank design. In single deck roof which shown in Figure 9-3, is
also called pontoon roof, the buoyancy is derived in the pontoon, an annular circular
pontoon radially divided into liquid tight compartments. The center deck which is
formed by membrane of thin steel plates are lap welded together and connected to
the inner rim of the pontoons.
Double deck roof (Figure 9-4) consists of upper and lower steel membranes
separated by a series of circumferential bulkhead which is subdivided by radial
bulkhead. The outer ring of the compartments is the main liquid tight buoyancy for
the roof. Double deck roof is much heavier than single deck one, hence it is more
rigid. The air gap between the upper and bottom plates of the deck has insulation
effect which helps against the solar heat reaching the product during the hot climate
and preventing heat loss of the product during cold climate.
Page | 228
CHAPTER 9: TANKS
Figure 9-2 Single deck floating roof tank
Figure 9-3 Double Single deck floating roof tank
9.3.3 Advantages of the floating roof storage tank

As the roof floats directly on the product, there is no vapour space and thus
eliminating any possibility of flammable atmosphere. It reduces evaporation losses
and hence reduction in air pollution. Vapour emission is only possible from the rim
seal area and this would mainly depend on the type of seal selected and used.
Despite of the advantages of the floating roof, to design and construct a floating roof
tank will be much more complicated and costly than the fixed ones. In term of tank
stability and design integrity, floating roof tank is never better than the fixed roof
tank as there are still many unknown parameters and factors in designing the
floating roof.
Page | 229
CHAPTER 9: TANKS
9.3.4 Process Description and Requirements

Capacity determination is the one of the first steps in designing the tank. Only after
the capacity is known, the tank can be sized up. The definition of the maximum
capacity can be explained easily in Figure 9-4.
Figure 9-2 Storage tank capacities levels
The maximum or total capacity is the sum of the inactive capacity (minimum
operating volume remaining volume in tank), actual or net working capacity and
the overfill protecting capacity.
1. Bottom Plate Design

API 650 has a very straight forward requirement on the bottom plate
thickness and width requirement.
Figure 9-3 Tank bottom Plate
Page | 230
CHAPTER 9: TANKS
Types of bottom plate

1. conical bottom with sluice point device
Conical bottom tanks (ICB) are available in seamless molded one-piece units
from either virgin high density crosslink or FDA-compliant linear
polyethylene. A funnel shaped conical bottom with 30° or 45° slope is
molded-in as are gallon markers and access openings. They have more
resistance to corrosion and chemicals than fiberglass, stainless or mild steel.
Wall thickness conforms to ASTM D-1998 standards for liquid containment.
Our storage tank systems possess excellent low temperature impact
resistance and are U.V. stabilized against degradation by sunlight. Factory
approved steel support work is required or can be supplied. Plastic storage
tanks are available in natural color or optional blue, green, yellow or black.
Other options include agitator support brackets, ladders, and tie-down
assemblies. They can be equipped with accessories to fit your specifications.
Figure 9-4 conical bottom with sluice

point device
2. Inclined flat bottom

Flat inclined bottom tank with legs, built in stainless steel Aisi storage of
small, middle and big quantities of wine, Standard/optional accessories:
▪ Pneumatic floating built in stainless steel with air chamber built in
alimentary plastic, two-way valve pump with manometer.
▪ N. 2 welded sleeves built in stainless steel.
▪ N. 2 taps or globe/throttle valves.
▪ Lifting arm.
▪ Sample-taker.
▪ Stair-support.
▪ Level with protection built in stainless steel.
3. pike beak shaped bottom

All the grape seeds fall to the bottom thanks to the exclusive cap re-stirring
method. Once collected at the bottom, grape seeds can be partially or totally
removed from the extraction process (removal of astringent tannins),
according to the winemaker's needs.
Page | 231
CHAPTER 9: TANKS
Grape-seeds are often a source of bitter and aggressive tannins and,

depending on the vintage and vines they represent a variable to be
considered with great care.
In traditional fermenters, the mechanical action and washing out of the
wine over the cap, combined with temperature and alcohol action, dissolve
the protective cuticle present in the grape-seeds, leading to the passage of
the substances they contain right into the wine-must.
Vertical Bending of Shell

When the tank is filled with product, the shell will expand radially due to the
elasticity of the shell plate material. This natural expansion is restricted at the point
where the shell is welded to the bottom plate. The shell-to-bottom joint is very rigid
and it rotates as a unit when the tank is under hydrostatic load.
Figure 9-5 Rotational of the shell to bottom connection
The shell tends to rotate in an outward direction about the rigid joint as depicted in
Figure 9-7, the bottom plate will also rotate and cause it to lift off the foundation for
a distance inside the tank until the pressure of the product acting on the floor,
balances the lifting effect. This action causes high bending stresses in the bottom
plate and the toe of the internal fillet weld. Due to the continual filling and emptying
of the tank, the load is cyclic, and this area is subject to low cycle fatigue.
9.4 Shell Design

The thickness of she}] plates shall be either 3/16 in. (7.65 lb. per sq. ft.) nominal, or
1/4 in. 00.20 lb. per sq. ft.) nominal, as specified on the purchase order. The width
of shell plates should be determined by the manufacturer, but preferably should be
not less than 60 in.
The tank shell is designed accordance to the API 650 (2007) and the design
considerations had been stated in the literature review under Chapter 2.12,
Mechanical Design Consideration. It was also mentioned in the literature review
that there are several methods stated in API 650 (2007) to determine the shell wall
thickness. Based on the tank size of 39 m diameter, 1-Foot Method was the most
appropriate method to be used.
Page | 232
CHAPTER 9: TANKS
The 1-foot method calculates the thickness required at design points 0.3 m (1ft)
above the bottom of each shell course. The required minimum thickness of shell
plates shall be the greater of the value computed as followed [API 650, 2007].
Design shell thickness:
Hydrostatic test shell thickness:
Where:
td = design shell thickness, mm
tt = hydrostatic test shell thickness, mm
D = nominal tank diameter, m
H = design liquid level, m
G = design specific gravity of the liquid stored
C.A = corrosion allowance, mm
Sd = allowable stress for the design condition, MPa
St = allowable stress for the hydrostatic test condition, MPa
Foot Method can be derived from the basic membrane theory, the two main stresses
exerting on the cylindrical shell due to the internal pressure are longitudinal stress
and circumferential stress. Let’s look into each stress individually by analyzing the
stresses in the thin-walled cylindrical shell which an internal pressure exerted on
it.
Longitudinal Stress
a thin walled cylindrical in which the longitudinal force FL resulted from the
internal pressure, Pi, acting on the thin cylinder of thickness t, length L, and
diameter D
Figure 9-6 Longitudinal Stress
Page | 233
CHAPTER 9: TANKS
Longitudinal force, FL = Pi x _/4 x D2

Area resisting FL, a = _ x D x t
Circumferential Stress
Similarly Figure 9-9 considers the circumferential stresses caused by internal
pressure, Pi, acting on the thin cylinder of thickness t, length L, and diameter D.
Figure 9-7 Circumferential stress
Page | 234
CHAPTER 9: TANKS
Longitudinal Stress versus Circumferential Stress

Comparing the both thickness equations due to the longitudinal stress and
circumferential stress, with a specific allowable stress, pressure and fixed
diameter, the required wall thickness to withstand the internal pressure, Pi, for
circumferential stress will twice that required for the longitudinal stress.
Circumferential stress in the thin wall will be the governing stress and hence the
Circumferential Stress Thickness Equation (tC) is used.
Circumferential Stress Thickness Equation and 1-Foot Method

From the Circumferential Stress Thickness Equation, replace the internal
pressure, pi to the hydrostatic pressure due to product liquid head ( gh),
consider the effective head at 0.3 m height (H – 0.3), and consider the corrosion
allowance (C.A) by adding in to the equation as per Figure. The minimum
required thickness from the 1-Foot method can be now be derived.
Shell Design Thickness Calculation

The design calculation for the shell wall thickness is attached in Appendix B. The
calculation result for the shell wall thickness is summaries
Where,
t. design = Minimum required thickness due to design condition,
t. hydro. = Minimum required thickness due to hydrostatic test,
t. min = The greater value of t, design and t .hydro., and
t sc = Actual thickness us
Page | 235
CHAPTER 9: TANKS
Figure 9-8
Tank Shell Testing

The tank shells should be water tested/ hydro tested after completion of the
wind girder. The tank will be filled up with water to its design level. The water
test not only to ensure no leakage of the tank, it also tested the foundation for
its capability of taking the filled tank load. Settlement will also be measured
during the water testing.
Page | 236
CHAPTER 9: TANKS
Figure 9-9 Tank Shell Testing
9.5 Fixation
A pipe support or pipe hanger is a designed element that transfer the load from
a pipe to the supporting structures. The load includes the weight of the pipe
proper, the content that the pipe carries, all the pipe fittings attached to pipe, and
the pipe covering such as insulation. The four main functions of a pipe support
are to anchor, guide, absorb shock, and support a specified load. Pipe supports
used in high or low temperature applications may contain insulation materials.
The overall design configuration of a pipe support assembly is dependent on the
loading and operating conditions.
Page | 237
CHAPTER 9: TANKS
9.5.1 Types of pipe support

▪ Rigid Support
Rigid supports are used to restrict pipe in certain direction(s) without
any flexibility (in that direction). Main function of a rigid support can be
Anchor, Rest, Guide or both Rest & Guide.
Figure 9-10 Rigid springs
▪ Spring support
Spring supports (or Flexible supports) use helical coil compression
springs (to accommodate loads and associated pipe movements due to
thermal expansions).
Figure 9-11 Variable spring hanger Figure 9-12 Variable spring hanger
Page | 238
CHAPTER 9: TANKS
Details of pipe support clip C
1 R1 pdf:
Figure 9-14
Figure 9-13
Page | 239
CHAPTER 9: TANKS
Figure 9-16
Figure 9-15
Figure 9-17
Page | 240
CHAPTER 9: TANKS
9.5.2 Details of drain tube C1 R1 pdf:

A surgical drain is a tube used to remove pus, blood or other fluids from a wound.
They are commonly placed by surgeons or interventional radiologists.
Figure 9-18 Drain tube
Figure 9-19 Details of drain tube
Details of sheet clamping C1 R2 pdf
❖ Notes
1. Fasteners are #17 x 7/8'' SS 18-8 Sheet metal screw with washers
spaced on 12'' [305mm] centers.
2. Fasteners supplied in U.S. standard sizes.
Figure 9-20 Sheet clamping
Page | 241
CHAPTER 9: TANKS
9.6 Welding
Welding procedures shall be established, and welding operators qualified by the
manufacturer. Qualification of welders in accordance with the applicable parts of
the latest edition of Section IX of the ASME Boiler and Pressure Vessel Codes is
recommended. Welding apply to tank joint designs that apply to welders and
welding procedures.
9.6.1 Types of welding

1. butt-weld: A weld placed in a groove between two abutting members.
Grooves may be square~ V-shaped (single or double) ~ or V-shaped (single
or double), or they may be either single or double beveled.
2. double-welded butt joint: A joint between two abutting parts lying in
approximately the same plane that is welded from both sides.
3. double-welded lap joint: A joint between two overlapping members in which
the overlapped edges of both members are welded with fillet welds.
4. fillet weld: A weld of approximately triangular cross-section that joins two
surfaces at approximately right angles~ as in a lap joint, tee joint. or corner
joint.
5. full-fillet weld: A fillet weld whose size is equal to the thickness of the thinner
joined member.
6. single-welded butt joint with backing: A joint between two abutting parts
lying in approximately the same plane that is welded from one side only with
the use of a strip bar or another suitable backing material.
7. single-welded lap joint: A joint between two overlapping members in which
the overlapped edge of one member is welded with a fillet weld.
8. tack weld: A weld made to hold the parts of a weldment in proper alignment
until the final welds are made.
9.6.2 Weld Size

The size of a groove weld shall be based on the joint penetration (that is, the depth
of chamfering plus the root penetration when specified).
The size of an equal-leg fillet weld shall be based on the leg length of the largest
isosceles right triangle that can be inscribed within the cross-section of the fillet
weld. The size of a equaling fillet weld shall be based on the leg lengths of the largest
right triangle that can be inscribed within the cross-section of the fillet weld.
Page | 242
CHAPTER 9: TANKS
Restrictions on Joints
▪ The minimum size of fillet "welds shall be as follows: On plates 5 mm
(3/16 in.) thick, the weld shall be a full-fillet weld, and on plates more
than 5 mm (3/16 in.) thick, the weld thickness shall not be less than one-
third the thickness of the thinner plate at the joint and shall be at least 5
mm (3/16 in.).
▪ Single-welded lap joints are permissible only on bottom plates and roof
plates.
▪ Lap-welded joints, as tack-welded, shal
l be lapped at least five times the nominal thickness of the thilmer plate
joined; however, with double-welded lap joints, the lap need not exceed
50 mm (2 in.), and with single-welded lap joints, the lap need not exceed
25 ml (1 in.).
▪ For manual welding processes, fillet weld legs or groove weld depths
greater than 6 mm (1/4 in.) shall be multi pass.
▪ For semi-automatic, machine, and automatic welding processes, with the
exception for electro-gas welding fillet weld legs or groove weld depths
greater than 10 mm (3/8 in.) shall be multi pass.
▪ All attachments to the exterior of the tank shall be completely seal
welded. Intermittent welding is not permitted. The only exception to this
requirement is wind girders.
9.6.3 Welding Symbols

Welding symbols used on drawings shall be the symbols of the American Welding
Society.
Vertical Shell Joints
a. Vertical shell joints shall be butt
joints with complete penetration
and complete fusion attained by
double welding or other means
that will obtain the same quality
of deposited weld metal on the
inside and outside weld surfaces.
b. Vertical joints in adjacent shell

courses shall not be aligned but
shall be offset from each other a
minimum distance of 5t, where t
is the plate thickness of the
thicker course at the point of
offset. Figure 9-21 Welding symbols
Page | 243
CHAPTER 9: TANKS
Horizontal Shell Joints

a. Horizontal shell joints shall have complete penetration and complete
fusion; however, as an alternative, top angles may be attached to the
shell by a double-welded lap joint.
b. Unless otherwise specified, abutting shell plates at horizontal joints
shall have a common vertical centerline.
Figure 9-22 Horizontal shell joints
Lap-Welded Bottom Joints

Lap-welded bottom plates shall be reasonably rectangular. Additionally,
plate may be either square cut or may have mill edges. Mill edges to be
welded shall be relatively smooth and uniform, free of deleterious deposits,
and have a shape such that a full fillet weld can be achieved. Unless otherwise
specified by the Purchaser.
Three-plate laps in tank bottoms shall be at least 300 mm (12 in.) from each
other, from the tank shell, and from joints between annular plates and the
bottom. A three-plate lap is created where three plates come together, and
all plates are joined to one another by lap welds. A location where a pair of
bottom plates are lap-welded to each other and are lapped onto an annular
plate constitutes a three-plate lap, but lapping a single bottom plate onto a
Figure 9-23 Method for Preparing Lap-

Welded Bottom Plates under Tank Shell
Page | 244
CHAPTER 9: TANKS
butt-welded annular plate splice does not constitute a three-plate lap weld
since the two annular plates are not joined together by a lapweld.
Butt-Welded Bottom Joints
Butt-welded bottom plates shall have their parallel edges prepared for butt
welding with either square or V grooves. Butt-welds shall be made using an
appropriate weld joint configuration that yields a complete penetration
weld.
Typical permissible bottom butt welds:

▪ The use of a backing strip at least 3 mm (1/8 in.) thick tack to the
underside of the plate is permitted.
▪ If square grooves are employed, the root openings shall not be less
than 6 mm (1/4 in.). A metal spacer shall be used to maintain the root
opening between the adjoining plate edges unless the Manufacturer
submits another method of butt-welding the bottom for the
Purchaser's approval.
▪ Three-plate joints in the tank bottom shall be at least 300 mm (12 in.)
from each other and from the tank shell.
Bottom Annular-Plate Joints

Bottom annular-plate radial joints shall be butt-welded and shall have
complete penetration and complete fusion. The backing strip, if used, shall
be compatible for welding the annular plates together.
Shell-to-Bottom Fillet Welds

For bottom and annular plates with a nominal thickness 13 mm), and less,
the attachment between the bottom edge of the lowest course shell plate and
the bottom plate shall be a continuous fillet weld laid on each side of the shell
plate. The size of each weld shall not be more than 13 mm) and shall not be
less than the nominal thickness of the thinner of the two plates joined (that
Figure 9-24 Spacing of Three-Plate

Welds at Annular Plates.
is, the shell plate or the bottom plate immediately tmder the shell). For
annular plates with a nominal thickness greater than 13 mm (1/2 in.), the
Page | 245
CHAPTER 9: TANKS
attachment welds shall be sized so that either the legs of the fillet welds or
the groove depth plus the leg of the fillet for a combined weld is of a size
equal to the annular-plate thickness, but shall not exceed the shell plate
thickness.
Wind Girder Joints

Full penetration butt-welds shall be used for joining ring sections.
Continuous welds shall be used for all horizontal top-side joints and for all
vertical joints. Horizontal bottom-side joints shall be seal-welded unless
specified otherwise by the Purchaser.
Roof and Top-Angle Joints

a. Roof plates shall, as a minimum, be welded on the top side with a
continuous full-fillet weld on all seams. Butt-welds are also
permitted.
b. For frangible roofs, roof plates shall be attached to the top angle of a
tank with a continuous fillet weld on the top side only, For non-
frangible roofs, alternate details are permitted.
c. The top-angle sections, tension rings, and compression rings shall be

joined by butt-welds having complete penetration and fusion.
d. At the option of the Manufacturer, for self-supporting roofs of the

cone, dome, or umbrella type, the edges of the roof plates may be
flanged horizontally to rest flat against the top angle to improve
welding conditions.
e. For fixed roof tanks equipped with full shell height insulation or
jacketing, the horizontal leg of the top shell stiffener shall project
outward. For insulation system compatibility, the Purchaser shall
specify if the horizontal leg is to be larger than specified above.
f. For tanks with a diameter less than or equal to 9 m (30 ft) and a
supplied cone roof the top edge of the shell may be flanged in lieu of
installing a top angle.
Page | 246
APPENDIX I: HYSYS REPORTS
10 APPENDIX I: HYSYS REPORTS

10.1 Fermentation hysys report
Stream (1) of sucrose:

Condition:
Composition:
Page | 247
Stream (2) of H2O:

Condition:
Composition:
Stream (3) of molasses:

Condition:
Page | 248
Composition:
Properties:
Page | 249
Stream (4) of diammonium phosphate:

Condition:
Composition:
Stream (5) of sodium chloride:

Condition:
Composition:
Page | 250
Stream (8) of air:

Condition:
Composition:
Stream (10) of H2SO4:

Condition:
Page | 251
Composition:
Stream (heavy) of sludge yeast:

Condition:
Composition:
Stream (21) of CO2 product:

Condition:
Page | 252
Composition:
Steam (24) of ethanol to distillation chapter:

Condition:
Composition:
Air compressor:
Page | 253
Fermenters:
Page | 254
Centrifuges:
Page | 255
Scrubber:
Page | 256
Page | 257
10.2 Carbon dioxide hysys report
Page | 258
10.2.1 Streamlines composition
Stream 1: “row gas from fermentation process to booster fan”

Conditions:
Composition:
Page | 259
Stream(5-1): “from 1st stage compressor to 2nd stage compressor”

Conditions:
Composition:
Page | 260
Stream6: “stream of CO2 after 2nd stage of compressors”

Conditions:
Composition:
Page | 261
Stream7: “stream of CO2 before catox”

Conditions:
Composition:
Page | 262
Stream O2: ”from oxygen tank to catox”

Conditions:
Composition:
Page | 263
Stream (8-2): “after Catox”

Conditions:
Composition:
Page | 264
Page | 265
Stream12: “before condenser”

Conditions:
Composition:
Page | 266
Stream 14: “after condenser”

Conditions:
Composition:
Page | 267
Stream 21: “final product stream to tanks”

Conditions:
Composition:
Page | 268
10.2.2 Process equipment:
1. Booster fan
Parameters:
Dynamics:
2. Knock-out drum with chilled water “as pre-cooler”
Parameters:
Nozzles:
Conditions:
Page | 269
3. 1st stage compressor
Parameters:
Dynamics:
4. After cooler
Parameters:
Performance profiles:
Performance plot:
Page | 270
Dynamics:
5. 2nd stage compressor
Parameters:
Dynamics:
6. Heater
Parameters:
Profile plot:
Page | 271
Dynamics:
7. Catox
Reaction details:
8. Cooler
Parameters
Page | 272
Performance plot:
Dynamics:
9. Cooler with ammonia
Parameters:
Performance plot:
Page | 273
Dynamics:
10. Knock-out drum
Parameters:
Conditions:
11. Dryer
Parameters:
Page | 274
12. Condenser
Parameters:
Conditions:
Performance plot:
Dynamics:
13. Disengaging column “liq-gas separator”
Parameters:
Page | 275
14. Pump1 “from disengaging column to stripping column”
Parameters:
15. Stripping column
Parameters:
Conditions:
16. Pump2 “from stripping column to tank”
Parameters:
Dynamics:
Page | 276
10.2.3 Important functions
1. Adjust
“to adjust mass flow of chilled water to control flow temperature before
compressor 2”
2. Tee
3. Recycle
“to take a branch of stream produced from catox to be mixed again with the
stream before it to achieve lower Concentration of hydrocarbons”
4. Mixer
“to mix 2 streams togeather one from catox and the 2nd from compressor
before catox”
5. Mixer
“to mix the disengaging column 2treams togeather before stripping
column”
Page | 277
APPENDIX II: TANK DRAWINGS
1 APPENDIX II: TANK DRAWINGS
Page | 278
Page | 279
Page | 280
Page | 281
APPENDIX III: P AND ID
2 APPENDIX III: P AND ID
Page | 282
Page | 283
Page | 284
Page | 285
References
11 References
▪ Technical and Economic Feasibility of Production of Ethanol from Sugar
Cane and Sugar Cane Bagasse.
▪ Fermentation & Bio-Chemical Engineering Handbook by Henry C. Vogel.
▪ Technical and Economical Feasibility of Production of Ethanol from Sugar
Cane and Sugar Cane Bagasse.
▪ Distillation: Equipment and Processes Edited by Andrzej Górak and Žarko
Olujić.
▪ Distillation: Operation and Applications Edited by Andrzej Go´rak and
Hartmut Schoenmakers.
▪ NPTEL – Chemical Engineering – Chemical Engineering Design – II.
▪ Particle Technology and Separation Processes Coulson and Richardson’s
CHEMICAL ENGINEERING VOLUME 2 FIFTH EDITION.
▪ APV Distillation handbock.
▪ www.klmtechgroup.com.
▪ Production of Pure Ethanol from Azeotropic Solution by Pressure Swing
Adsorption 1P. Pruksathorn and 1, 2T. Vitidsant.
▪ https://mawdoo3.com/%D9%85%D8%A7_%D9%87%D9%88_%D9%85
%D8%B5%D8%AF%D8%B1_%D8%BA%D8%A7%D8%B2_CO2
▪ http://al3loom.com/?p=9609
▪ https://www.nature.com/articles/d41586-018-07666-6
▪ https://whatsyourimpact.org/greenhouse-gases/carbon-dioxide-
emissions
▪ https://www.yobrew.co.uk/fermentation.php
▪ https://lifefermented.wordpress.com/2014/01/22/how-much-co2-is-
produced-from-brewing/
▪ https://www.sc.edu/ehs/training/Fire/05_co2.htm
Page | 286
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Page | 288
Page | 289

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ETHANOL production

No. Team Name Seat No.

Figure 1-1 Structure of ethanol

1.1 Physical properties

1.2 Chemical properties

Barbiturates (Verona, Barbital, Luminal, Amytal), ethyl orthoformate, and other

2. Hydrolysis of ethyl sulfates to ethanol:

3. Re-concentration of the dilute sulfuric acid.

1. Direct hydration process

Fermentation processes was accounting for 83% of total production and by

➢ Sugar Beet Molasses

Figure 1-2 Molasses

1.4 Uses of Ethanol

causes cell dehydration by disrupting the osmotic balance across cell

2 CHAPTER 2: FERMENTATION SECTION

Reaction: C6 H12 O6 ------> 2 C2 H5 OH + 2 CO2

C6H12O6 --> 2 C2H5OH +2 CO2 + 2 ATP + heat

2.2 Ethanol Fermentation with Yeast

A small concentration of oxygen must be provided to the fermenting yeast as it is a

Fermentation at PDM is done through two ways:

2.3 What is a Fermentor?

Fermentor provides a sterile environment and optimum condition that are

Figure 2-1 Fermentor

1. Material used for fermentor

A fermentor should provide the facility to control and monitor various

9. Foam controlling device

10. Bottom drainage system

2.4 Classification of Fermentation Processes

Figure 2-2 Multistage continuous separation: Multiple separate addition is

Figure 2-4 single stage continuous system

2.5 The Main Fermenter Layout

2.5.1 Nutrient Feed Tanks

2.5.2 Sterile Filters

Figure 2-5 Domnick -hunter sterile air filter

2.5.3 Air Compressors

2.5.6 Cooling Equipment

2.5.7 Environmental Control

2.5.8 General design data

2.6 Fermentation section

The fermentation is carried out in 10 vessels to maintain a continuous operation

2.6.1 Process Control

2. Level Controllers (LC)

3. Ratio Controllers (RC)

4. Temperature Controllers (TC)

5. Pressure Controllers (PC)

2.7 Fermentation process

The preceding topic about the design of a continuous sterilizer emphasized

Cooling a fermenter after batch sterilization is more similar to a co-current

1. Heat Loss by Convection and Radiation

Ql = UA (T1 – T2) = Btu/hr

Convection and radiation depend upon whether the tanks are

2. Heat Loss by Evaporation

3. Heat Removed by Refrigerant

Q3 = Sp.Ht. x broth vol. x 8.345 x ΔT ÷ time (hr)

4. Heat Added by Mechanical Agitation

5. Heat of Fermentation = ΔHF

Figure 2-6 Disk-bowl centrifuge

Figure 2-7 Theory of centrifugation

2.8.1 Biomass Separation (centrifuges) (F-011, F-012)