Finalsubmissibleversion8-170315160655 2

Final Year Design Project
A Plant Design Report on The Production of

Biodiesel from 30 TPD Waste Cooking Oil
Project Supervisor
Dr. Maria Mustafa
Muhammad Abubakar
DDP-SP13-BEC-043
Muhammad Hashim Khan
DDP-SP13-BEC-053
Shahzaib Younas
DDP-SP13-BEC-085
Zohaib Uzair
DDP-SP13-BEC-101
Department of Chemical Engineering

Biodiesel Production Using Waste Cooking Oils
Muhammad Abubakar
DDP-SP13-BEC-043
Muhammad Hashim Khan
DDP-SP13-BEC-053
Shahzaib Younas
DDP-SP13-BEC-085
Zohaib Uzair
DDP-SP13-BEC-101
A report submitted in partial fulfilment of the

requirements for the award of the degree of
Bachelor of Science in Chemical Engineering
Department of Chemical Engineering

I declare that this I declare that this thesis entitled “title of the thesis” is the result of my
own research
except as cited in the references. The thesis has not been accepted for any degree and
is not concurrently submitted in candidature of any other degree.
Signature: ....................................................
Name: ....................................................
Date: ....................................................
iii
ACKNOWLEDGEMENT
We would like to express our sincere gratitude to all those who have assisted and guided
us during our project study. First of all, we would like to thank our supervisor, Doctor
Maria Mustafa for her guidance and support during the course of this project. She provided
us with invaluable supervision from the beginning until the completion of our project. We
would also like to thank the lab engineers and technicians, who have assisted us through
this project. They have catered to our equipment needs during the project. I would also like
to express my most sincere feelings of gratitude towards Doctor Fahad who helped the
group in designing the reactors. Last but not the least, we also express our honest gratitude
to all our colleagues, friends and beloved family for their endless love and support
throughout the project.
iv
ABSTRACT
Biodiesel is a type of bio fuel which can be derived from new or used vegetable oils and
animal fats. It is a biodegradable, renewable energy and clean burning alternative. Due to
the price hike in conventional fuels in the last decade studies have been made to introduce
biodiesel as a feasible alternative to conventional diesel. Diesel Engines can also be made
to run on cooking oils as such but due to their high viscosity and carbon content they cause
some undesirable problems in diesel engines. To make these cooking oils more suitable for
diesel engine consumption we turn them into esters via the process of transesterificatio n.
This reduces their molecular weight to one thirds and lowers their viscosity, essentially
making them more suitable as engine fuels. But even then, it is mostly recommended that
this biofuel be used with commercial diesel as a mixture i.e. 20% biodiesel 80% diesel.
The process we’ve worked upon is the base-catalysed trans-esterification method, which
will be used to produce biodiesel from waste oils. This process is initially assisted by acid
catalysed esterification for the reduction of free fatty acids to acceptable limits. To induce
simplicity and understanding we have assumed waste soya bean oil to be our raw material.
The core objective of this paper would to design and develop a profitable biodiesel
production plant. Relying on the conventional mass and energy balances we can estimate
the real-life construction of this plant.
v
List of Figures
Figure 3.1.1-Process Flow Diagram ................................................................................... 9
Figure 4.1.1 Material Balance (Filter) .............................................................................. 18
Figure 4.2.1 Material Balance (R-1) ................................................................................. 19
Figure 4.3.1 Material Balance (R-2) ................................................................................. 21
Figure 4.4.1 Material Balance (C-1) ................................................................................. 22
Figure 4.6.1 Material Balance (MT-1).............................................................................. 26
Figure 4.8.1 Material Balance (FT) .................................................................................. 28
Figure 4.9.1 Material Balance (MT-2).............................................................................. 29
Figure 4.10.1 Material Balance (C-4) ............................................................................... 31
Figure 4.11.1 Material Balance (MT-3)............................................................................ 32
Figure 4.12.1 Material Balance (D-1) ............................................................................... 33
Figure 4.13.1 Material Balance (D-2) ............................................................................... 34
Figure 5.2.1 Steam Properties ........................................................................................... 36
Figure 5.3.1 Energy Balance (HE-1) ................................................................................ 37
Figure 5.7.1 Energy Balance (R-1) ................................................................................... 41
Figure 5.8.1 Energy Balance (R-2) ................................................................................... 43
Figure 5.9.1 Energy Balance (FT) .................................................................................... 44
Figure 5.10.1 Energy Balance (Condenser) ...................................................................... 45
Figure 5.11.1 Energy Balance (HE-5) .............................................................................. 46
Figure 5.12.1 Energy Balance (DC-1) .............................................................................. 48
Figure 5.13.1 Energy Balance (DC-2) .............................................................................. 50
Figure 6.3.1 Flash Tank .................................................................................................... 68
Figure 7.2.1 Reactor Control ............................................................................................ 99
Figure 7.3.1 Heat Exchanger Control ............................................................................. 100
vi
Figure 7.4.1 Distillation Column Control ....................................................................... 101
vii
List of Tables
Table 4.1-1 Material Balance (Filter) ............................................................................... 18
Table 4.2-1 Reactor1 Parameters ...................................................................................... 19
Table 4.2-2 Material Balance (R-1) .................................................................................. 19
Table 4.3-2 Material Balance (R-2) .................................................................................. 20
Table 4.4-1 Centrifuge1 Parameters ................................................................................. 21
Table 4.4-2 Material Balance (C-1) .................................................................................. 22
Table 4.6-1 Mixing Tank Parameters ............................................................................... 24
Table 4.6-2 Material Balance (MT-1)............................................................................... 25
Table 4.8-1 Material Balance (FT) ................................................................................... 28
Table 4.9-1 Material Balance (MT-2)............................................................................... 29
Table 4.10-1 Centrifuge4 Parameters ............................................................................... 30
Table 4.10-2 Material Balance (C-4) ................................................................................ 30
Table 4.11-1 Material Balance (MT-3)............................................................................. 32
Table 4.12-1 Material Balance (D-1) ................................................................................ 32
Table 4.13-1 Material Balance (D-2) ................................................................................ 33
Table 5.3-1 Energy Balance (HE-1) ................................................................................. 37
Table 5.7-2 Energy Balance (R-1) .................................................................................... 42
Table 5.8-2 Energy Balance (R-2) .................................................................................... 44
Table 5.9-1 Energy Balance (FT) ..................................................................................... 45
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Table 5.10-1 Energy Balance (Condenser) ....................................................................... 46
Table 5.11-1 Energy Balance (HE-5) ............................................................................... 47
Table 5.12-1 Energy Balance for Boiler of DC-1 ............................................................. 49
Table 5.12-2 Energy Balance for Condenser of DC-1...................................................... 49
Table 5.13-1 Energy Balance for Boiler of DC-2 ............................................................. 51
Table 5.13-2 Energy Balance for Condenser of DC-2...................................................... 51
ix
Table of Contents
Chapter 1 INTRODUCTION ___________________________________________ 1
1.1 Biofuels _______________________________________________________ 1
1.2 What Is Biodiesel? _______________________________________________ 1
1.3 Advantages & Disadvantages_______________________________________ 2
1.4 What Are Oils? __________________________________________________ 3
1.5 Vegetable Oils as Fuels (Properties) _________________________________ 3
Chapter 2 LITERATURE REVIEW ______________________________________ 4
2.1 Process Selection ________________________________________________ 4
2.2 Transesterification _______________________________________________ 4
2.3 Pre-treatment ___________________________________________________ 4
2.4 Standard Practices & Their Flowsheets _______________________________ 5
2.5 Raw Materials __________________________________________________ 6
2.5.1 Choice of Oil ________________________________________________ 6
2.5.2 Catalyst ____________________________________________________ 6
2.5.3 Alcohol ____________________________________________________ 7
2.5.4 Factors Affecting the Transesterification Process ___________________ 7
Chapter 3 PROCESS DESCRIPTION & FLOWSHEET ______________________ 9
3.1 Process Flow Diagram & Description ________________________________ 9
3.1.1 Filter ______________________________________________________ 9
3.1.2 Heat Exchanger (HE-1)_______________________________________ 10
3.1.3 Pre-Treatment Reactor _______________________________________ 10

x
3.1.6 Pre-treatment Heat Exchanger (PT_HE-1) ________________________ 10
3.1.7 Pre-treatment Heat Exchanger (PT_HE-2) ________________________ 10
3.1.8 Pre-treatment Distillation (P_D) ________________________________ 11
3.1.9 Reactor1 (R1) ______________________________________________ 11
3.1.11 Reactor2 (R2) ______________________________________________ 11
3.1.12 Centrifuge1 (C1) ____________________________________________ 11
3.1.13 Centrifuge2 (C2) ____________________________________________ 11
3.1.14 Mixing Tank1 (Wash Tank) ___________________________________ 12
3.1.15 Centrifuge 3 (C3) ___________________________________________ 12
3.1.16 Flash Tank (FT1) ___________________________________________ 12
3.1.17 Mixing Tank2 (MT2) ________________________________________ 12
3.1.18 Centrifuge4 (C4) ____________________________________________ 12
3.1.19 Mixing Tank3 (MT3) ________________________________________ 12
3.1.21 Distillation Column 1 (D1) ____________________________________ 12
3.1.22 Distillation Column 2 (D2) ____________________________________ 13
3.2 Products ______________________________________________________ 13
3.1.23 Glycerine __________________________________________________ 13
3.3 Testing of Used Oil _____________________________________________ 13
Chapter 4 MATERIAL BALANCE _____________________________________ 16
4.1 Survey for Waste Cooking Oil Collection ______________________________ 16
3.1.24 Capacity Selection___________________________________________ 17
4.2 Material Balance (Filter) _________________________________________ 17
4.3 Material Balance Reactor1 (R-1) ___________________________________ 18
xi
4.4 Material Balance (Reactor 2) ______________________________________ 20
4.5 Material Balance (Centrifuge1) ____________________________________ 21
4.6 Material Balance (Centrifuge 2)____________________________________ 22
4.7 Material Balance (Mixing Tank 1) __________________________________ 24
4.8 Material Balance (Centrifuge 3)____________________________________ 26
4.9 Material Balance (Flash Tank) _____________________________________ 27
4.10 Material Balance (Mixing Tank 2) ________________________________ 28
4.11 Material Balance (Centrifuge 4) __________________________________ 29
4.12 Material Balance (Mixing Tank 3) ________________________________ 31
4.13 Material Balance (Distillation Column 1) __________________________ 32
4.14 Material Balance (Distillation Column 2) __________________________ 33
Chapter 5 ENERGY BALANCE _______________________________________ 35
5.1 Cp Calculation _________________________________________________ 35
5.2 Equipment ____________________________________________________ 36
5.3 Energy Balance Heater (HE-1) ____________________________________ 37
5.7 Energy Balance (Reactor 1) _______________________________________ 41
5.8 Energy Balance (Reactor 2) _______________________________________ 42
5.9 Energy Balance (Flash Tank) ______________________________________ 44
5.10 Energy Balance Condenser ______________________________________ 45
5.11 Energy Balance Heater (HE-5) ___________________________________ 46
5.12 Energy Balance Distillation Column (DC-1) ________________________ 48
5.13 Energy Balance Distillation Column (DC-2) ________________________ 50
xii
Chapter 6 EQUIPMENT DESIGN ______________________________________ 52
6.1 Reactor Design _________________________________________________ 52
6.1.1 Reactor Selection ___________________________________________ 54
6.1.2 Rate Constants______________________________________________ 55
6.1.3 Reactor Impeller ____________________________________________ 57
6.1.4 Specifications Sheet _________________________________________ 57
6.1.5 Pressure Drop ______________________________________________ 58
6.2 Heat Exchanger Design __________________________________________ 58
6.2.1 Types with respect to Structure_________________________________ 58
6.2.2 Principal Parts ______________________________________________ 59
6.2.3 Working Principle of Double Pipe Heat Exchanger _________________ 60
6.2.4 HEAT TRANSFER MODES __________________________________ 60
6.2.5 Types of Double Pipe Heat Exchanger ___________________________ 60
6.2.6 Double Pipe Heat Exchangers__________________________________ 60
6.2.7 Operation of Double Pipe Heat Exchanger________________________ 61
6.2.8 Heat Exchanger Design_______________________________________ 62
6.2.9 Mechanical Design __________________________________________ 67
6.3 Flash Tank ____________________________________________________ 68
6.4 Distillation Column Design (D-1) __________________________________ 70
6.4.1 Choice between Plate and Packed Column________________________ 70
6.4.2 Choice of Plate Type_________________________________________ 71
6.4.3 Design Steps for A Distillation Column __________________________ 71
6.4.4 From which the theoretical no. of stages to be 7 ___________________ 75
6.4.5 Feed plate location __________________________________________ 75
6.4.6 Column Diameter ___________________________________________ 75
xiii
6.5 DISTILLATION COLUMN DESIGN ______________________________ 79
6.5.1 Top Operating Line __________________________________________ 81
6.5.2 Bottom Operating Line _______________________________________ 82
6.5.3 Ideal no of trays is 8 _________________________________________ 83
6.5.4 Efficiency And Total Number Of Real Stages _____________________ 83
6.5.5 Superficial Vapor Velocity ____________________________________ 85
6.5.6 Net Area Required __________________________________________ 85
6.5.7 Column Diameter ___________________________________________ 86
6.5.8 Height of the column : _______________________________________ 86
6.5.9 Plate Pressure Drop __________________________________________ 88
6.5.10 Residual Head ______________________________________________ 89
6.5.11 Check Residence Time _______________________________________ 89
6.5.12 Check Entrainment __________________________________________ 89
6.6 Mixing Tank Design_____________________________________________ 91
6.6.1 Volume Calculation _________________________________________ 91
6.6.2 Thickness _________________________________________________ 91
6.6.3 choice of closure :- __________________________________________ 92
6.6.4 Impeller design _____________________________________________ 93
6.6.5 Design Data________________________________________________ 96
Chapter 7 INSTRUMENTATION & PROCESS CONTROL _________________ 97
7.1 Introduction ___________________________________________________ 97
7.1.1 Requirements of Control ______________________________________ 97
7.1.2 Safety ____________________________________________________ 97
7.1.3 Product Specification ________________________________________ 97
7.1.4 Environmental Regulation ____________________________________ 97
xiv
7.1.5 Operational Constraints_______________________________________ 97
7.1.6 Economics _________________________________________________ 98
7.2 Reactors ______________________________________________________ 98
7.3 Heat Exchanger ________________________________________________ 99
7.4 Distillation Column ____________________________________________ 100
Chapter 8 COST ESTIMATION _______________________________________ 102
8.1 Introduction __________________________________________________ 102
8.2 Equipment Cost Estimation ______________________________________ 103
8.1.1 Reactor Cost Estimation _____________________________________ 103
8.1.2 Flash Tank Cost Estimation __________________________________ 103
8.1.3 Heat Exchanger Cost Estimation ______________________________ 104
8.1.4 Centrifuge Cost Estimation ___________________________________ 105
8.1.5 Distillation Column Cost Estimation (D-1) ______________________ 106
8.1.6 Distillation Column Cost Estimation (D-2) ______________________ 108
8.3 Total Equipment Cost___________________________________________ 110
8.4 Total Physical Plant Cost (PPC)___________________________________ 110
8.5 Total Investment_______________________________________________ 111
8.6 Annual Operating Cost __________________________________________ 111
8.7 Direct Production Costs _________________________________________ 112
8.8 Annual Production Cost _________________________________________ 113
8.9 Production Cost _______________________________________________ 113
Chapter 9 SITE & MATERIAL SELECTION ____________________________ 114
9.1 The Project ___________________________________________________ 114
9.2 Proposal for Site Location _______________________________________ 114
9.2.1 Raw Materials _____________________________________________ 114
xv
9.2.2 Climate __________________________________________________ 115
9.2.3 Market ___________________________________________________ 115
9.2.4 Waste Disposal ____________________________________________ 115
9.2.5 Transport _________________________________________________ 115
9.2.6 Water Supply______________________________________________ 115
9.2.7 Labour Supply_____________________________________________ 116
9.3 Conclusion ___________________________________________________ 116
Chapter 10 HAZOP STUDY ___________________________________________ 117
10.1 HAZOP On Double Pipe Heat Exchanger _________________________ 117
10.2 HAZOP On Distillation Column (Parameter Pressure) _______________ 118
10.3 HAZOP On Distillation Column (Parameter Temperature) ____________ 119
10.4 Hazard Analysis _____________________________________________ 120
Appendix A Matlab Program __________________________________________ 124
Appendix B Flash Tank Data _________________________________________ 128
Appendix C D-1 Data _______________________________________________ 130
Appendix D D-2 Data _______________________________________________ 135
Appendix E Heat Exchanger Charts & Graphs ____________________________ 139
Appendix F Costing Indices __________________________________________ 143
References ___________________________________________________________ 145
xvi
Chapter 1 INTRODUCTION
1.1 Biofuels
Such fuels which are usually obtained from the flora and fauna around us are usually called
as biofuels. Ever since the start of the industrial revolution people have had the idea of
running automobiles on edible oils. In that sense biodiesel is also a biofuel. It dates back
to 1853 and was coined by E. Duffy and J. Patrick. At the Paris, International Exhibitio n
in 1900, Rudolf Diesel demonstrated a test engine sample working on peanuts oil. In 1912,
Rudolf Diesel said, “The use of vegetable oils for engine fuels may seem insignifica nt
today. But such oils may become in course of time as important as petroleum and the coal
tar products of the present time” (Marco Aurélio, 2011).
Diesel was indeed right as in the previous decade we saw conventional fuel prices sky
rocketing. This immensely helped the sustainable energy sector as it put in the minds of
people, the fear of economic shakedown both on an individual as well as on a national
basis.
1.2 What Is Biodiesel?

To a layman term biodiesel implies diesel obtained from biological sources such as plant
or animals. It is a type of biofuel. As it turns out there are essentially 4 ways of converting
organic sources into biodiesel. These are listed as.
1. Direct use or blending of oils
2. Micro-emulsion
3. Pyrolysis (gasification)
4. Trans-esterification
Biodiesel or fatty acid methylated esters are derived or obtained from animal or plant
stocks, due to their renewability they form a sustainable class of fuels. This very reason
makes them a very viable choice for future fuels and hence they are receiving considerable
importance from the scientific community. One of the very simple production methods of
biodiesel is transesterification in which the triolein sources are reacted with methanol under
appropriate conditions, often in the presence of a catalyst. The catalyst even through it is
not consumed during the reaction helps decrease the reaction times. The main product of
these reactions is simply biodiesel while glycerol is produced as a by-product in the
aftermath of the reaction. Due to higher conversions in this reaction it is understood that
very little oil is wasted. In order to bypass the catalyst, use we can run the reaction under
supercritical conditions however this amounts to increased costs. Another method is via
the use of biochemical routes.
Now looking at the point number one the confusion persists that whether or not vegetable
oil is or is not an alternative of conventional fuels in pure form. Actually, vegetable is a
whole lot more viscous that biodiesel, it also has very high flash point due to this very
reason and some others vegetable cannot be used as an alternative to diesel as it is and has
to be processed before usage. One of the methods as listed above is the transesterifica tio n
of the oils. This involves the conversion of the triglycerides (oils) into methylated or
ethylated esters. However due to the efficiency and other concerns methylated ester are
often preferred. Also, that they burn efficiently and provide more power.
Because of the lesser energy costs and greater viability as opposed to the other processes
we will prefer the method of transesterification.
1.3 Advantages & Disadvantages

1. One of the key advantages of this biofuel is sustainability. The fact that we grow
cooking oil sources means that an abundance can theoretically be made.
2. Biodegradability is another important factor which contributes to the pro camp of
biodiesel. A simple proof of that is when left in open atmospheric conditions biodiesel
degrades much more rapidly as compared to commercial diesel.
3. There is less sulphur in biodiesel as compared to commercial diesel. This leads to
some major environmental pros while the greater amount of oxygen ensures that this
biofuel burns completely deceasing the emission of CO2.
Biodiesel despite being “greener” has its own demerits some of which are discussed below.
1. Greater NOx emissions.
2. Despite being less viscous that cooking oils biodiesel is still more viscous than
diesel, this is the reason we still have to mix biodiesel with commercial grade diesel.
2
Viscosity leads to stresses and large droplets which can cause wear on the fuel inject or
systems.
3. Remember the degradation part, here is when it becomes a problem. When exposed
to the open environment for longer periods these esters degrade into smaller components
and decrease some of the desirable properties of our fuel.
4. Except for a few countries vegetable oils are generally very expensive. Even in
Pakistan which is an agricultural economy the price of vegetable oil is higher than that of
commercial diesel. This takes a huge toll on the economic viability of the whole process.
1.4 What Are Oils?

Fats and oils are primarily water-insoluble, hydrophobic substances in the plant and animal
kingdom that are made up of one mole of glycerol and three moles of fatty acids and are
commonly referred to as triglycerides. The difference between a fat and oil is signified by
their physical states at room temperature. A triglyceride that is a liquid at room temperature
is called as oil while a triglyceride that is solid at room temperature is called as a fat. One
important thing to note here is that triglycerides derived from mammals are usually fats
while those derived from cold blooded animals as well as plants are oils.
1.5 Vegetable Oils as Fuels (Properties)

Vegetable cooking oils have viscosities 11-17times that of diesel fuel. Volumetric heating
values is about 39-40 Mega Joule/kg while for diesel it is 45 Mega Joule/kg. The flash
point for vegetable oils is very high, more than 200 degrees centigrade. It has been found
that the utilization of vegetable oils as fuels led to problems related to type and grade of oil
as well as climate conditions. Some common problems are carbon deposits, plugging if the
fuel lines, gelling of lubricating oils, foiled piston heads and ring sticking. Cetane number
of vegetable oils is very high hence reducing the ignition delay. In addition to all this they
have high iodine value which increases their oxidation rate. Therefore, long time storage
is not recommended for vegetable oils.
3
Chapter 2 LITERATURE REVIEW
2.1 Process Selection
Of the several methods, available for producing biodiesel, transesterification of natural
oils and fats is currently the method of choice. The purpose of the process is to lower the
viscosity of the oil or fat. As far as the other processes are concerned, although blending
of oils and other solvents and micro emulsions of vegetable oils lowers the viscosity it
causes engine performance problems, such as carbon deposit and lubricating oil
contamination. Meanwhile, pyrolysis produces more bio gasoline than biodiesel fuel [1].
2.2 Transesterification
Transesterification of vegetable oils with alcohol is the best method for biodiesel
production. There are two types of transesterifications, one is with catalyst and other one
is without catalyst. Transesterification is a reversible reaction and the excess of alcohol
shifts the equilibrium to the product side.
Base-catalysed transesterification is one process that converts waste cooking oil to
biodiesel fuel. Fats and oils are tri esters of glycerol (triglycerides), with three long chain
fatty acids that give the molecule a high molecular weight and low volatility. A base-
catalysed transesterification (using methanol as the alcohol and NaOH as the catalyst)
converts fats and oils to the methyl esters of the three individual fatty acids. It is to be noted
here that the reaction would still proceed without a catalyst but would be too slow and may
take days to complete, therefore the addition of catalyst becomes necessity. With molecular
weights about a third of the original triglyceride, these methyl esters are more volatile and
work well in diesel engines, the mixture of fatty acid methyl esters is called biodiesel [2].
The purpose of using methanol is its low commercial price and the reason that it gives
better performance in engines. Methanol has both physical as well as chemical advantages.
Esters produced using methanol gave higher power and produced more torque [3].
2.3 Pre-treatment
Free fatty acids are known as to cause saponification during the transesterification reaction.
Soaps make biodiesel purification harder and hence it is necessary to limit the FFA content.
4
This is done by the esterification process in which acid along with methanol is employed
to convert the FFAs into esters (biodiesel). Glycerine washing is then employed to purify
the refined oil. After such a treatment, the oil phase, having a low level of free fatty acids
(less than 0.5 wt.%), was subjected to the alkali-catalysed transesterification.
2.4 Standard Practices & Their Flowsheets

Conventionally the alcoholysis or transesterification of virgin or used cooking oils is done
via base catalyst. This can be done in either batch mode or it can be a continual process.
In most cases the catalyst is sodium hydroxide or sodium methylate. It is recovered after
the transesterification reaction as sodium glycerate, sodium methylate and sodium soaps in
the glycerol phase. An acidic neutralization step with, for example, aqueous hydrochlo r ic
acid is required to neutralize these salts. In that case glycerol is obtained as an aqueous
solution containing sodium chloride. Depending on the process, the final glycerol purity is
about 80% to 95%.
When caustic is employed in the catalyst role it can react with the broken glycerides to
form soap. These soaps can dissolve in the glycerol produced during the reactions in the
reactors. They cause a major hurdle in the purification of glycerol. These soaps need to be
broken down into FFAs by employing HCl. We have done this in our process. The loss of
esters converted to fatty acids can reach as high as 1% of the biodiesel production.
5
Figure 2.4 Global Scheme for A Typical Biodiesel
Setup
2.5 Raw Materials
2.5.1 Choice of Oil

There are more than 350 oil bearing crops identified, among which only sunflo wer,
soybean, cottonseed, rapeseed and peanut oils are considered as potential alternative fuels
for diesel engines [4]. We will be considering soya oil because the biodiesel produced by
this type of waste shows similar properties as diesel. Another point that warrants its
selection is it’s cetane number which is closer to petroleum diesel. Also, it is abundantly
produced as waste.
2.5.2 Catalyst
Transesterification can also be catalysed by Lowry acids. These catalysts give very high
yields in alkyl esters but reactions are slow, requiring typically temperature above 100
degrees centigrade and hours to complete the conversion [5]. We therefore use base
catalysed reactions which are comparatively less time consuming as compared to the before
mentioned. For that purpose, we can use potassium or sodium hydroxide but because of
better solubility of KOH with methanol we would likely prefer methanol. As we will come
6
to know the topic of catalyst is a sensitive one and affect heavily on the yield and reaction
times of the process.
The biodiesel industry currently uses sodium methoxide, because methoxide cannot form
water upon reaction with alcohol such as with hydroxides, which influence the reaction
and the quality of the production biodiesel [6]. Furthermore, base-catalysed reactions are
performed at generally lower temperatures, pressures, and reaction times and are less
corrosive to industrial equipment than acid-catalysed methods [7]. Therefore, fewer capital
and operating costs are incurred by biodiesel production facilities in the case of the base-
catalysed transesterification method.
2.5.3 Alcohol
Studies have shown that methylated esters are more suitable for diesel engines as compared
to ethylated ones. Hence, we will want a source for a methyl group and not an ethyl group.
The obvious choice is methanol. Another advantage is the cost factor because methanol is
cheaper than ethanol and easier to source as compared to ethanol. Ethanol could even be a
banned item in a specific country due to various reasons.
2.5.4 Factors Affecting the Transesterification Process

Main factors affecting the transesterification process are.
1. Methanol/Oil Molar Ratio
2. Temperature
3. Reaction Time
4. Mixing
5. FFAs & Moisture
6. Catalyst Conc.
7
Figure 2-5-Factors Effecting FAME
8
Chapter 3 PROCESS DESCRIPTION &
FLOWSHEET
3.1 Process Flow Diagram & Description
Figure 3.1.1-Process Flow Diagram
3.1.1 Filter
First of all, the waste cooking oil or WCO goes to a filter where solid chunks of impurities
in it are removed. These are chunks from the eatables that have been heated in the oil. This
filtered WCO is then pumped into the reactor R1. The oil is still high In FFAs however
hence and cannot be processed by regular base catalysed transesterification method hence
9
we first need to perform acid assisted esterification in order to bring the FFAs to an
acceptable level before we can pursue the traditional base catalysed transesterification.
3.1.2 Heat Exchanger (HE-1)

Water is heated to 55 °C in HE-1. This water is used to wash the biodiesel further along
the process. According to [8] hot water washing is a good way to obtain high purity
biodiesel (FAME) product.
3.1.3 Pre-Treatment Reactor

In the pre-treatment reactor esterification reaction is carried out at 70 °C, 400 kPa and a
6:1 molar ratio of methanol to crude oil. This is necessary in order to bring the FFAs downs
to a level where they can be processed by the transesterification reactor i.e. R-1. Otherwise
the free fatty acids can react with the alkali catalyst to produce soaps causing emulsio ns.
Emulsions make the purification of biodiesel difficult.

Mix of caustic and alcohol is heated to 60 °C in this heat exchanger. This stream is used
both in R-1 & R-2 and since our reaction takes place at 60 °C, hence this stream is heated
to 60 °C.

The HE-3 heats the filtered waste cooking oil from ambient temperatures to 60 °C.
3.1.6 Pre-treatment Heat Exchanger (PT_HE-1)

Effluents of the pre-treatment reactor are cooled in this heat exchanger to 46 °C.
3.1.7 Pre-treatment Heat Exchanger (PT_HE-2)

The glycerine washing separates the oil and it is heated in this heat exchanger. This oil is
then routed to the R-1 for base catalysed transesterification. The purpose of this heat
exchanger is angina, to bring the temperature of oil to 60 °C. The FFAs by now have been
brought down to acceptable levels.
10
3.1.8 Pre-treatment Distillation (P_D)
The stream other than the majority oil stream emanating from the glycerine washing
column is treated in this distillation unit. In P_D, five theoretical stages and a reflux ratio
of 5 are used. At 28 °C and 20 kPa, 94% of the total methanol fed to the column is recovered
in the distillate (i.e., stream 111) at the rate of 188 kg/h. It contained 99.94% methanol and
0.06% water and is recycled to pre-treatment esterification reactor. At 70 °C and 30 kPa,
bottom stream 112 (147 kg/h) is composed of 75% glycerol, 8% methanol, 7% sulfur ic
acid, 7% oil and 3% water.
3.1.9 Reactor1 (R1)

Filtered WCO then enters the reactor1 where a feed of caustic mixed with methanol is
already coming in. The oil is heated to approx. 55-60 degree centigrade at atmospheric
pressure. Under such condition 90% conversion is achieved in the first reactor. Effluent of
R1 contains biodiesel, un-reacted oil, soap, salts etc.

Effluents of R-1 are heated to 60 °C.
3.1.11 Reactor2 (R2)

Stream originating from C1 goes to R2 along with remaining methanol + catalyst at
atmospheric pressure and residence time of 1 hour. Here our conversions levels touch the
99% mark.
3.1.12 Centrifuge1 (C1)

The effluent of R1 goes to the centrifuge where the un-reacted oil and the biodiesel
produced are separated from the glycerol. This glycerol is not pure and needs treatment in
terms of solvent recycles and impurity removal.

The effluent of R2 is fed to the centrifugal separator where the un-reacted oil and the
biodiesel produced are separated from the glycerol. This glycerol is not pure and needs
treatment in terms of solvent recycles and impurity removal.
11
3.1.14 Mixing Tank1 (Wash Tank)
Now the biodiesel stream from the C2 is fed to the mixing tank and is washed with the
process wash water and HCL solution. This neutralizes the catalyst and converts any soap
to FFA.
3.1.15 Centrifuge 3 (C3)

The MT1 effluent is fed to the centrifuge where the biodiesel is recovered together with
small amounts of water.
3.1.16 Flash Tank (FT1)

Final purification of biodiesel is achieved in the flash drum that operates under vacuum. (5
kPa).
3.1.17 Mixing Tank2 (MT2)

Streams originating from C1, C2, C3 and the stream from the head of the FT end up in the
MT2. These contain methanol, glycerol, water as well as FFA, soaps and salts. This stream
is first treated with HCl to convert soaps into FFAs.

The effluent of MT2 then passes through the C4 and thus FFAs get removed. We get a
stream that is rich in methanol and glycerol.
3.1.19 Mixing Tank3 (MT3)

Glycerol and methanol rich stream is treated with NaOH to maintain pH. The resulting
stream is fed to the distillation columns D1.

The purpose of this heat exchanger is to bring the feed of the first distillation column to the
required temperature.
3.1.21 Distillation Column 1 (D1)

D1 operates slightly above atmospheric pressure. We get glycerol and water from bottom
which is 80% wt. /wt. glycerol & water. The top product consists of water and methanol.
12
3.1.22 Distillation Column 2 (D2)
D2 is operated at high pressure (50 kPa). We get almost pure 99.99 % methanol which is
then recycled as input stream from the top. Water is obtained from the bottom which can
be recycled as washing water.
3.2 Products
There are two main products of the transesterification process.
 Glycerin
 Biodiesel
3.1.23 Glycerine
To make the biodiesel plant economically attractive we have to make sure that anything
coming out of a product line other than the main product itself is sellable. For the most part
only two products are produced in a continuous biodiesel plant, its biodiesel and glycerol.
Excess methanol is reused or sold. However, there is a catch, glycerol produced during the
process is impure since it contains some quantities of methanol which make it highly unsafe
for a large sector of human consumable producing industries. It also has salts as well as
FFAs. Its physical appearance is also very undesirable. Hence the traditional markets are
off limits. To make the glycerol pure we generally flash or distil it but since it (glycerol) is
a high boiling component it can cause a strain on our financials. So, what ends up
happening is that this bio glycerol is used as a cattle feed supplement as it adds to the
cattle’s feed to weight gain ratio. This is because certain animals can handle toxic methanol
and its breakdown products. Another use for the bio glycerol is the cement industry. It is
added to various parts of the process such as in clinkering, kilning etc. to add to the cement
strength.
However, in our project the simulation indicates that the bottom product is essentially 80%
glycerol and 20% methanol. If this can be translated to reality, then the economic viability
of the process can surely be ever increased.
3.3 Testing of Used Oil

Chemically used oils contain triglycerides. When they are used for cooking purposes these
go through changes and the oil ends up having abundance of free fatty acids. It is these
13
acids that cause the acidity of the used oil. The problem is that when we try to make
biodiesel out of such oil and add KOH and alcohol for the purpose along with alcohol, it
ends up making soap. Soap is not what we want, we want biodiesel.
So, for that we have to measure the extra amount of KOH that needs to go in our batch of
waste oil. For this very purpose, we do a titration of our oil sample.
Prepare titration solution by mixing 1 gram of KOH in 1 L distilled water.
Prepare 3 beakers. Take1 ml of waste cooking oil and pour in beaker no. 1. Pour 10 ml of
isopropyl alcohol. Take your titrating solution in a third beaker.
Mix oil and alcohol. Add some indicator drops into the oil and alcohol mixture.
Now begin titrating. Slowly pour the titrating solution till pink colour appears and remains
so for 30 seconds.
It is generally considered that oil using 0-3 ml of the above-mentioned titrating solution
indicates a “good” cooking oil. Oil that uses 3-5 ml of the titration solution is average oil
while anything above that is harmful for human health since it has been heavily used and
has a lot of fatty acids. It is to be noted here that the presence of FFA greatly affects the
transesterification process. It has been noted that our oil must have a FFA value lower than
3% for the base catalysed reaction to produce favourable results. Ester yields are greatly
reduced in the presence of greater than three percent FFAs.
Since we are using a base catalysed process we have to debate on the Achilles heel of base
catalysed transesterification and that is be soap formation. The issue is not so relevant as
long as the FFAs are within the 3-4 % mark but waste or used cooking oils can contain up
to 15 % FFAs. Our catalyst NaOH doesn’t react well with triglycerides but reacts with
mono glycerides well and diglycerides to some extent. This results in soap which again
calls for even more purification. And with purification comes energy costs. To counter this
problem, we can use vacuum distillation to remove the FFAs from our triglycer ides
beforehand and sell them off either as animal feed or a separate esterification can be
arranged where different conditions can be perhaps used to convert these FFAs into
biodiesel. For smaller values of FFAs we can simply add in more catalyst and carry on with
removing the soap [9].
Now that we’ve calculated the catalyst to be used we can now proceed with the normal
biodiesel production. This is because we have effectively counteracted the free fatty acids.
14
Coincidentally this test can also be used to gauge how good our oil is for cooking purposes.
Used oil having a significant amount of free fatty acids is not a good choice. It is harmful
for health. This is precisely the reason that used cooking oil should not be reused rather it
should be waster in accordance with the laws of the country.
15
Chapter 4 MATERIAL BALANCE
Material balance is the backbone in the design and conceiving of a chemical plant along
with the energy balance. It helps us in conceiving the designs, in financial evaluation, in
process control and in optimizing the process. Let’s say for example a solvent is required
for the extraction of soya bean oil (which also happens to be our primary triolein) from the
its source. In order to calculate the arithmetic quantity of that solvent required we can apply
the material balance on that particular unit. But even better is that we can not only use that
information to calculate the amount of solvent required we can also use that informa tio n
for the design and development of the machines that extracts the soya bean oil. Hence in
every plant design we first go through the phase of the material balance. We can use the
processed information in the design of equipment or in the evaluation of the economics of
the process. Material balance can also help in deciding the raw material that we can use to
achieve the same end product. Quite a few different types of processing can achieve the
same end result, so that case studies (simulations) of the processes can assist materially in
the financial decisions that must be made. Material balances also helps in the hourly and
daily operating decisions of plant managers.
For the most part we’ve used stoichiometry for our balances especially in reactors. For
almost all separation processes in our process we were provided with figures.
4.1 Survey for Waste Cooking Oil Collection

We carried out an online survey to assess the amount of waste oil we could gather.
According to eatoye.com Lahore has 1000 restaurants from which you can order a
delivery... but the website has mostly branded places listed so we can only get but a rough
estimate from the website. I am going with an estimate that Lahore has three times the
places eatoye.com has listed. Exotic food is limited so I am going with a very low estimate.
The average waste vegetable oil generation column has been sourced from a study
[10]. Units are litres/month as also indicated in the paper from where the figures are
sourced. Most establishments seem to favour canola oil, while unspecified vegetable oil
and liquid shortening bring up a distant second and third respectively. The survey showed
that vegetable oils like sunflower oil and corn-mixes were the least common types of oils
being used in the group. Low responses in the Sunflower Oil, Corn/Soy Oil and
16
Corn/Canola Oil categories produced exceptionally high averages, skewing the data and
producing a total average volume significantly higher than the total average volume by
restaurant type.
3.1.24 Capacity Selection
Waste Cooling Oil Flow 30068.9043 kg/day OR 30.06 ton/day
4.2 Material Balance (Filter)

The composition of our crude oil after pre-treatment is as such.
Fin Calculatio Fout1 Calculatio Fout2(kg/hr.

Component
(Kg/hr.) n (Kg/hr.) n )
1220.296 1220.2963*
Oil 1220.2963 ~ ~
3 1
Palmitic. A 7.016 7.016*1 7.016 ~ ~
Moisture 3.13 3.13*1 3.13 ~ ~
Unsaponifie
55.87 ~ ~ 55.87*1 56.25
d
17
Ash .37586 ~ ~ .37586*1 .37586
Table 4.2-1 Material Balance (Filter)
4.3 Material Balance Reactor1 (R-1)

The reaction is as:
1𝑡𝑟𝑖𝑜𝑙𝑒𝑖𝑛 + 6𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 ⇔ 3𝐹𝐴𝑀𝐸 + 1𝑔𝑙𝑦𝑐𝑒𝑟𝑜𝑙 + 3𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙
𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡
 1 mole FFA consumes 1 mole of catalyst to produce 1 mole of soap + water.

 1𝐹𝐹𝐴 + 1𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡 ⇔ 1𝑠𝑜𝑎𝑝 + 1𝑤𝑎𝑡𝑒𝑟
𝑐𝑎𝑡𝑎𝑙𝑦𝑠𝑡
Reactor conditions and parameters are as such.
Figure 4.2.1 Material Balance (Filter)
Pressure Atmospheric
18
Temperature 60 °C
Conversion 90 %
Residence Time 1 hour
Table 4.3-1 Reactor1 Parameters
Calculation (90%
Component Fin (Kmol/hr.) Fout (Kmol/hr.)
Conv.)
1.3558 -
Oil 1.3558 .13558
(1.3558*.90)
Palmitic. A .025 .025 - .02255 .00250
Moisture (Water) .174 .174 + .0222 .1965
FAME ~ 3*(1.3558*.90) 3.660
Glycerol ~ 1.3558*.90 1.220
Methanol 7.32 3*(1.3558*.90) 3.6608
Catalyst .2929 .2929-(.0250-.0025) .2787
Soap ~ .0250*.90 .0225
Table 4.3-2 Material Balance (R-1)
Figure 4.3.1 Material Balance (R-1)
19
4.4 Material Balance (Reactor 2)
Reactor 2 has similar conditions as reactor 1. Overall conversion is 99%.
Temperature 60 °C
Conversion 90 %
Calculation (90%
Component Fin (Kmol/hr.) Fout(Kmol/hr.)
Conv.)
Oil .13558 .13558*.01 .001358
8.94E-06-(8.94E-
Palmitic. A 8.94E-06 8.94E-07
06*90%)
Moisture (Water) .001965 .0019 + .0002335 .00219
3.660 +
FAME 3.660 4.0269
(3*.13558*.90)
Glycerol ~ .13558*.90 .1220
2.196 + .7321 = (.13558*90%*3) +
Methanol 4.539
2.9281 2.9281
.0026 + .029 = .029-((8.94E-06)-
Catalyst .0301
.0316 .0000137)
.000225 + (8.94E-
Soap .000225 .0002335
06*.90)
Table 4.4-2 Material Balance (R-2)
20
Figure 4.4.1 Material Balance (R-2)
4.5 Material Balance (Centrifuge1)

 Centrifuges are assumed to achieve 99% recovery of the components.
 In Centrifuge1 and Centrifuge2 methanol is assumed to be distributed by 60% in
the biodiesel phase and 40% in the glycerol phase.
In Centrifuge3 methanol is assumed to distribute by 10% in the biodiesel phase and in

Centrifuge4 by 100% in the glycerol phase.
Recovery 99 %
60 % (With FAME)/40% (With
Methanol Distribution
Glycerol)
Table 4.5-1 Centrifuge1 Parameters
Componen Fin(kg/hr. Calculation Fout1(kg/hr. Calculation Fout2(kg/hr.

t ) s ) s )
FAME 1098.26 1098.26*1 1098.26 ~ ~
21
Glycerol 112.267 ~ ~ 112.267*1 112.267*1
Methanol 117.148 117.148*.60 70.28 117.148*.40 46.859
Palmitic. A .7016 0.7016*.01 0.00701 .7016*.99 .69
Catalyst 11.1502 11.1502*.01 0.108 11.1502*.99 11.03
Soap 6.76 6.76*.01 0.067 6.76*.99 6.69
Oil 122.02 122.02*1 122.02 ~ ~
Water 3.538 3.538*.01 0.035 3.538*.99 3.52
Table 4.5-2 Material Balance (C-1)
Figure 4.5.1 Material Balance (C-1)
4.6 Material Balance (Centrifuge 2)
Recovery 99 %
22
60 % (With FAME)/40% (With
Methanol Distribution
Glycerol)
Componen Fin(kg/hr. Calculation Fout1(kg/hr. Calculation Fout2(kg/hr.

t ) s ) s )
Palmitic. 1208.0934*
1208.0934 1208.0934 ~ ~
A 1
Glycerol 11.22 ~ ~ 11.22*1 11.22
145.2640*.6 145.2640*.4
Methanol 145.2640 87.1584 58.1056
0 0
.0002505*.0 .0002505*.9
FFA .0002505 1.37E-07 .0002480
1 9
Catalyst 1.2049 1.2049*.01 .011 1.2049*.99 1.160
Soap .07000 .07000*.01 .0007 .07000*.99 .06937
Oil 1.2202 1.2202*1 1.2202 ~ ~
Water .0395 .0395*.01 .000395 .0395*.99 .039
23
4.7 Material Balance (Mixing Tank 1)

The stream is fed to a mixing tank together with process (wash) water and HCl solution so
as to neutralize the catalyst and convert any soap to FFA. The wash and pH adjustment
tank effluent is fed to a centrifuge (C3) where biodiesel is recovered with small amounts
of water.
There are two reactions occurring in this mixer…
 SOAP + HCl  FFA + NaCl
 HCl + NaOH  H20 + NaCl
Wash Water Ratio (Wt.) 1:1 (For Every kg FAME)

HCl (Molar) 1:1 (For Every Mole Catalyst + Soap)
Table 4.7-1 Mixing Tank Parameters
24
Compone Fin1(kmol/ Calculatio Fin2(kg/h Fout1(kmol/
Calculation
nt hr.) ns r.) hr.)
FAME 4.0269 ~ ~ ~ 4.0269
Methanol 2.7237 ~ ~ ~ 2.7237
(3.19E-
Palmitic.
3.196E-11 ~ ~ 11+293E-03) 2.10E-06
A
*90%
.012049-
Catalyst .012049 ~ ~ 3.0122E-05
(.000293*90%)
2.33E-06-
Soap 2.33E-06 ~ ~ 2.33E-07
2.10E-06
Oil .0013 ~ ~ ~ .0013
(.00029*.90+2.3
Salt ~ ~ ~ .0002656
3E-6)
.00029+2.335E-
HCl ~ ~ .000300 ~
06
(1208.09/18)
Water 2.199E-05 ~ 65.25 67.11
+2.19E-05
Table 4.7-2 Material Balance (MT-1)
25
Figure 4.7.1 Material Balance (MT-1)
Recovery 99 %
Methanol Distribution 10 % (FAME) / 90% (Glycerol)
Compone Fin(kg/hr Fout1(kg/hr Fout2(kg/hr

Calculations Calculations
nt .) .) .)
FAME 1208.0934 1208.0934*1 1208.0934 ~ ~
Methanol 87.15 87.15*.10 8.715 87.15*.90 78.435
Palmitic.
.0005 .0005*.01 5.8E-06 .0005*.99 .0005
A
Catalyst .0012 .0012*.01 .000012 .0012*.99 .00188
9.314E- 9.314E-
Soap 9.314E-06 9.24E-08 9.34E-08
06*.01 06*.99
26
Oil 1.220 1.220*1 1.220 ~ ~
Salt .015 .015*.01 .00015 .015*.99 .015
1208.0992*.0 1208.0992*.9
Water 1208.0992 12.08 1196.9020
1 9
4.9 Material Balance (Flash Tank)

Final purification of biodiesel is achieved in the flash drum that operates under vacuum. (5
kPa)
27
Fin Fout1
Component Calculation Calculation Fout2(kg/hr.)
(Kg/hr.) (Kg/hr.)
FAME 1208.0934 ~ ~ 1208.0934*1 1208.0934
Methanol 8.7158 8.7158*1 8.7158 ~ ~
Oil 1.186 ~ ~ 1.186*1 1.186
Water 12.08 12.08*1 12.08 ~ ~
Table 4.9-1 Material Balance (FT)
Figure 4.9.1 Material Balance (FT)
28
Compo Fin1(kg/ Fin2(kg/ Fin3(kg/ Fin4(kg/ Fout(kg/
Calculations
nent hr.) hr.) hr.) hr.) hr.)
Glycero
109.155 10.91 ~ ~ 109.155+10.91 120
l
Methan 45.56+56.49+76.2
45.56 56.49 76.2 8.47 186
ol +8.47
Palmiti .6945+.00029+.00
.6945 .00029 .0005 ~ .6983
c. A 05
Catalys
10.70 1.16 .0116 ~ 10.70+1.16+.0116 11.8798
t
9.24E- 6.69+.069+9.24E-
Soap 6.69 .069 ~ 6.76
06 06
1162.86 3.502+.039+1162.
Water 3.502 .039 11.74 1178.15
3 8+11.74
29
Recovery 99 %
Methanol Distribution 100 % In Glycerol Phase
Compone Fin(kmol/h Calculatio Fout1(kmol/h Calculatio Fout2(kmol/h

nt r.) ns r.) ns r.)
Glycerol 1.30 1.30*1 1.30 ~ ~
Methanol 5.8 5.8*1 5.8 ~ ~
Palmitic. .0024+.022
.0024 ~ ~ .0250
A 55
Catalyst .2933 ~ ~ ~ ~
Soap .02255 ~ ~ ~ ~
Water 64.800 64.8+.315 65.11 ~ ~
HCl .315 .003*1 .003
.2933+.022
NaCl ~ ~ ~ .31588
55
30

Reaction taking place in the mixer 3 is as under…
 NaOH + HCl  H2O + NaCl
Compone Fin1(kmol/h Calculatio Fin2(kmol/h Calculati Fout1(kmol/h

nt r.) ns r.) on r.)
Glycerol 1.342 ~ ~ 1.342*1 1.342
Methanol 6.0038 ~ ~ 6.0038*1 6.0038
Water 66.96 ~ ~ 66.96*1 66.96
HCl .003 ~ ~ ~ ~
31
NaOH ~ .003*1 .003 ~ ~
NaCl ~ ~ ~ .003*1 .003
4.13 Material Balance (Distillation Column 1)

All glycerol is removed in the bottom product of D1 which is 80% w/w in glycerol and the
remaining is predominantly water.
Fin Fout
(Kg/hr.) 1(Kg/hr.)
Glycerol 123.49 ~ ~ 123.49*1 123.49
Methanol 192.123 192.123*1 192.123 ~ ~
Water 1205.40 1205.40*.90 1175.40 1205-1175 30
NaCl .1095 ~ ~ ~ ~
Table 4.13-1 Material Balance (D-1)
32
Figure 4.13.1 Material Balance (D-1)
4.14 Material Balance (Distillation Column 2)
Fin Fout
(Kg/hr.) 1(Kg/hr.)
Methanol 192.123 192.123*1 192.123 ~ ~
Water 1175.40 ~ ~ 1175.40*1 1175.40
Table 4.14-1 Material Balance (D-2)
33
Figure 4.14.1 Material Balance (D-2)
34
Chapter 5 ENERGY BALANCE
To properly utilize the energy that is consumed or produced within a chemical producing
industry the engineer must be familiar with the fundamentals of the energy balance. This
includes the know-how of the basic terminology associated with the subject. An engineer’s
main attention ought to be devoted to heat, work, enthalpy, and internal energy. Next, the
energy balance must be applied to the project. This can help in calculating the amount of
steam that our heater needs for heating purposes or the cooling water required for cooling
a stream to a required temperature.
In our project, we have used the standard enthalpy calculation formula that goes as.
𝑇
𝐻 = 𝑚 ∫ 𝐶𝑝 𝑑𝑇
𝑇𝑑
𝑘𝑚𝑜𝑙
𝑊ℎ𝑒𝑟𝑒 𝑚 = 𝑚𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 𝑖𝑛
ℎ𝑟
𝐽
𝑊ℎ𝑒𝑟𝑒 𝐶𝑝 = ℎ𝑒𝑎𝑡 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 𝑖𝑛
𝑘𝑚𝑜𝑙. 𝐾
𝑇𝑑 = 𝐷𝑎𝑡𝑢𝑚 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 𝑖𝑛 𝐾
𝑇 = 𝑆𝑝𝑒𝑐𝑖𝑓𝑖𝑒𝑑 𝑇𝑒𝑚𝑒𝑝𝑟𝑎𝑡𝑢𝑟𝑒 𝑖𝑛 𝐾𝑒𝑙𝑣𝑖𝑛
5.1 Cp Calculation
We know that value of Cp and specific enthalpy is a function of temperature and that
function can be written as an empirical power series equation. Now if we take this equation
and put in the above equation and integrate it, we’ll get something like below which we
can then use to calculate our enthalpy.
𝐶𝑝 = 𝑎 + 𝑏 ∗ 𝑇 + 𝑐 ∗ 𝑇 2 + 𝑑 ∗ 𝑇 3
𝑏 𝑐 𝑑
𝐻 = 𝑚 ∗ ( 𝑎 ∗ (𝑇 − 𝑇𝑑 ) + (𝑇 2 − 𝑇𝑑2 ) + (𝑇 3 − 𝑇𝑑3 ) + (𝑇 4 − 𝑇𝑑4 ))
2 3 4
𝑘𝑚𝑜𝑙
𝑊ℎ𝑒𝑟𝑒 𝑚 = 𝑚𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 𝑖𝑛
ℎ𝑟
𝐽
𝑊ℎ𝑒𝑟𝑒 𝐶𝑝 = ℎ𝑒𝑎𝑡 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 𝑖𝑛
𝑘𝑚𝑜𝑙. 𝐾
𝑇𝑑 = 𝐷𝑎𝑡𝑢𝑚 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 𝑖𝑛 𝐾 35
𝑇 = 𝑆𝑝𝑒𝑐𝑖𝑓𝑖𝑒𝑑 𝑇𝑒𝑚𝑒𝑝𝑟𝑎𝑡𝑢𝑟𝑒 𝑖𝑛 𝐾𝑒𝑙𝑣𝑖𝑛
The values of heat constants were used from the book “Perry’s Chemical Enginee rs’
Handbook”. However, some values were also obtained from other sources such as Coulson
Vol. 6 and internet. Some static Cp values were also used after appropriate unit conversion.
Energy balance Calculation

Steady state Law of conservation of energy applied on each equipment is applied by using
the following equation.
𝐻𝑖𝑛 − 𝐻𝑜𝑢𝑡 + 𝐶𝑜𝑛𝑠𝑢𝑚𝑝𝑡𝑖𝑜𝑛 + 𝐻𝑒𝑎𝑡 𝐴𝑑𝑑𝑖𝑡𝑖𝑜𝑛 = 0
5.2 Equipment
We are applying our energy balance on the following equipment…
 Heat Exchangers
 Reactors R1 and R2
 Distillation Column D1 and D2
 Flash Tank
Figure 5.2.1 Steam Properties
36
5.3 Energy Balance Heater (HE-1)
The heater is used for heating water that washes the FAME. For every kg biodiesel, we use
1 kg water, since hot water provides better washing we heat it to about 55 °C. Our reference
or datum temperature is 25 °C.
Figure 5.3.1 Energy Balance (HE-1)
So, as stated above we calculate the specific enthalpy of our feed and product stream using
the heat equation constants from the Perry’s. We then put it into the formula to calculate
our enthalpy.
Flow 𝑯𝒊𝒏 − 𝑯𝒐𝒖𝒕

Component a b c D T1 T2 𝑱
(kmol/h) =𝑸( )
𝒉𝒓.
Water 276370 -2090 8.125 - 298 333 79.11 1.72E+08
0.0141
Table 5.3-1 Energy Balance (HE-1)
𝑄 𝑘𝑔
𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑆𝑡𝑒𝑎𝑚 𝐹𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 (𝑚𝑠𝑡𝑒𝑎𝑚 ) = = 79.11
𝜆 ℎ𝑟.
𝑗𝑜𝑢𝑙𝑒𝑠
𝜆 = 𝐿𝑎𝑡𝑒𝑛𝑡 𝐻𝑒𝑎𝑡 𝑂𝑓 𝑉𝑎𝑝𝑜𝑟𝑖𝑧𝑎𝑡𝑖𝑜𝑛 𝑂𝑓 𝑆𝑡𝑒𝑎𝑚 = 2174000
𝑘𝑔
37
This heater is used to heat the entering methanol and caustic to 60 °C. this is because our
reaction in the reactor takes place at 60 °C.
Flow Heat Heat 𝑯𝒊𝒏 − 𝑯𝒐𝒖𝒕

Component a b c d e T1 T2 𝑱
(kmol/h) In Out =𝑸( )
𝒉𝒓.
Catalyst 883.47 - -3.01 - .0422 298 333 .071

2.49 .862
0E+00 2.3E+7 2.3E+7
Methanol 105800 - .9379 0 0 298 333 8.053
362.
𝑄 𝑘𝑔
𝜆 ℎ𝑟.
𝑘𝑔
38
Component a b c d e T1 T2 Flow Heat Heat 𝑯𝒊𝒏 − 𝑯𝒐𝒖𝒕

𝑱
(kmol/h) In Out =𝑸( )
𝒉𝒓.
Oil .45 .0007 .99 0 0 298 333 1120.646

FFA .43 0 0 0 0 298 333 7.01
1124.5 9.1E+7 9.13E+07
Water 276370 - 8.125 - 9e- 298 333 .174
2090 .014 6
𝑄 𝑘𝑔
𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑆𝑡𝑒𝑎𝑚 𝐹𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 (𝑚𝑠𝑡𝑒𝑎𝑚 ) == 42.02
𝜆 ℎ𝑟.
𝑘𝑔
39
Flow Heat 𝑯𝒊𝒏 − 𝑯𝒐𝒖𝒕

Component a b c d e T1 T2 Heat In 𝑱
(kmol/h) Out =𝑸( )
𝒉𝒓.
FAME 30060 206 6 0 0 328 333 3.9153

44E- 3.E- 9E-
Glycerol 8.242 0 328 333 0.11864
01 04 08
-
Methanol 105800 .9379 0 0 328 333 4.413
362.3
FFA .43 0 0 0 0 328 333 8.95E-07
9.25E+7 1.10E+8 1.73E+07
- - -
Catalyst 883.47 .0422 328 333 0.02928
2.495 3.013 .8621
Soap .56 0 0 0 0 328 333 0.000233
- - 9E-
Water 276370 8.125 328 333 0.002199
2090 0.014 06
Oil .45 .0007 .99 0 0 328 333 0.11864
40
𝑄 𝑘𝑔
𝜆 ℎ𝑟.
𝑘𝑔
5.7 Energy Balance (Reactor 1)

Conditions of our reactor are given below.
Temperature 60 °C
Conversion 90 %
Feed goes in at our datum temperature i.e. 25 °C and in the reactor, we maintain a
temperature of 60 °C in the reactor as per the kinetics study. We do this by cooling the
reactor with water. Supposing that the temperature of our water rises by a 30 °C when
cooling the reactor, we can calculate how much cooling water is required.
Figure 5.7.1 Energy Balance (R-1)
41
The values of our constants have been obtained from Perry’s Handbook.
𝑯𝒊𝒏 − 𝑯𝒐𝒖𝒕
Flow Heat
𝒉𝒓.
FAME 30060 206 6 0 0 298 333 3.5594
Glycerol 8.242 44E- 3.E- 9E- 0 298 333 1.1864
01 04 08
Methanol 105800 - .9379 0 0 298 333 3.559
362.3
FFA .43 0 0 0 0 298 333 .0701
1.12E+8 1.10E+8 5.25E+07
Catalyst 883.47 - - - .0422 298 333 .2704
2.495 3.013 .8621
Soap .56 0 0 0 0 298 333 6.7655
Water 276370 - 8.125 - 9E- 298 333 .1965
2090 0.014 06
Oil .45 .0007 .99 0 0 298 333 118.646
Table 5.7-2 Energy Balance (R-1)
∆𝑇 = 30 °C
𝐶𝑝 = 4120
𝑘𝑔°C
𝑄 𝑘𝑔
𝐶𝑜𝑜𝑙𝑖𝑛𝑔 𝑊𝑎𝑡𝑒𝑟 𝐹𝑙𝑜𝑤 = = 417.96
∆𝑇𝐶𝑝 ℎ𝑟.
5.8 Energy Balance (Reactor 2)

Conditions of our reactor are given below. Feed goes in at our datum temperature i.e. 25
°C and in the reactor, we maintain a temperature of 60 °C to maintain the optimal
conditions for our first reactor.
Temperature 60 °C
42
Conversion 90 %
Figure 5.8.1 Energy Balance (R-2)
The values of our constants have been obtained from Perry’s.

𝑯𝒊𝒏
Flow Heat − 𝑯𝒐𝒖𝒕
Component a b c d e T1 T2 Heat In
(kmol/h) Out 𝑱
=𝑸( )
𝒉𝒓.
FAME 30060 206 6 0 0 328 333 3.9153
Glycerol 8.242 44E- 3.E- 9E- 0 328 333 0.11864
01 04 08
Methanol 105800 - .9379 0 0 328 333 4.413
1.07E+8 1.11E+8 1.02E+07
362.3
FFA .43 0 0 0 0 328 333 8.95E-07
Catalyst 883.47 - - - .0422 328 333 0.02928
2.495 3.013 .8621
43
Soap .56 0 0 0 0 328 333 0.000233
Water 276370 - 8.125 - 9E- 328 333 0.002199
2090 0.014 06
Oil .45 .0007 .99 0 0 328 333 0.11864
Table 5.8-2 Energy Balance (R-2)
∆𝑇 = 30 °C
𝐶𝑝 = 4120
𝑘𝑔°C
𝑄 𝑘𝑔
5.9 Energy Balance (Flash Tank)

Flash tank is used for the purification of our biodiesel (FAME). The feed essentially
contains methanol, water and biodiesel. It operates at 5 kPa. A valve is used to reduce the
pressure while heat is provided to flash our mixture so that methanol goes into the upwards
stream while biodiesel is obtained from the bottom.
Figure 5.9.1 Energy Balance (FT)
44
Flow Heat 𝑯 𝒊𝒏 − 𝑯 𝒐𝒖𝒕
𝒉𝒓.
Water 276370 - 8.125 - 9E- 312.9 357.7 .67116

2090 0.014 06
Methanol 105800 - .9379 0 0 312.9 357.7 .27237 4.03E+8 1.84E+8 1.43E+08
362.3
FAME 30060 206 6 0 0 312.9 357.7 4.02
Table 5.9-1 Energy Balance (FT)
𝑄 𝑘𝑔
𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑆𝑡𝑒𝑎𝑚 𝐹𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 (𝑚𝑠𝑡𝑒𝑎𝑚 ) =
= 65.88
𝜆 ℎ𝑟.
𝑘𝑔
5.10 Energy Balance Condenser
Figure 5.10.1 Energy Balance (Condenser)
45
𝒉𝒓.
- - 9E-
Water 276370 8.125 357.7 328 .6526
2090 0.014 06 -
4.32E+6 2.31E+8
- 2.1E+06
Methanol 105800 .9379 0 0 357.7 328 .2648
362.3
Table 5.10-1 Energy Balance (Condenser)
∆𝑇 = 30 °C
𝐶𝑝 = 4120
𝑘𝑔°C
𝑄 𝑘𝑔

The purpose of this heat exchanger is to bring the feed of the first distillation column to the
required temperature i.e. 100 °C.
So, as stated above we calculate the specific enthalpy of our feed and product stream using
the heat equation constants from the Perry’s. We then put it into the formula to calculate
our enthalpy.
46
𝒉𝒓.
Glycerol 8.242 44E- 3.E- 9E- 0 328 333 1.3015

01 04 08
Methanol 105800 - .9379 0 0 328 333 5.8374
1.51E+8 3.82E+8 2.31E+8
362.3
Water 276370 - 8.125 - 9E- 328 333 65.1159
2090 0.014 06
𝑄 𝑘𝑔
𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝑆𝑡𝑒𝑎𝑚 𝐹𝑙𝑜𝑤 𝑅𝑎𝑡𝑒 (𝑚𝑠𝑡𝑒𝑎𝑚 ) =
= 106.18
𝜆 ℎ𝑟.
𝑘𝑔
47
5.12 Energy Balance Distillation Column (DC-1)
Feed going into the distillation column contains glycerol, water and methanol. Since
glycerol has a very high boiling point as compared to the other two, it is separated out firs t.
The following column separates the methanol from water. The first distillation column
operates at a bit higher pressure than atmospheric pressure. (101.3 kPa)
Figure 5.12.1 Energy Balance (DC-1)
48
Flow
Component a b c d e T1 T2 𝑸𝒃
(kmol/h)
Glycerol 8.242 44E- 3.E- 9E- 0 328 333 1.305
01 04 08
Methanol 105800 - .9379 0 0 328 333 0
1.18E+09
362.3
Water 276370 - 8.125 - 9E- 328 333 1.66
2090 0.014 06
Table 5.12-1 Energy Balance for Boiler of DC-1
𝑄𝑏 𝑘𝑔
𝜆 ℎ𝑟.
𝑘𝑔
Flow
Component a b c d e T1 T2 𝑸𝒄
(kmol/h)
Glycerol 8.242 44E- 3.E- 9E- 0 328 333 0
01 04 08
Methanol 105800 - .9379 0 0 328 333 5.8374
1.55E+09
362.3
Water 276370 - 8.125 - 9E- 328 333 63.4492
2090 0.014 06
Table 5.12-2 Energy Balance for Condenser of DC-1
∆𝑇 = 30 °C
𝐶𝑝 = 4120
𝑘𝑔°C
𝑄𝑐 𝑘𝑔
49
5.13 Energy Balance Distillation Column (DC-2)
The second distillation column operates at 50 kPa and separates methanol from water. 99.9
mole % methanol is obtained as the distillate.
Figure 5.13.1 Energy Balance (DC-2)
50
Flow
Component a b c d e T1 T2 𝑸𝒃
(kmol/h)
Water 276370 - 8.125 - 9E- 328 333 63.44
2090 0.014 06
4.04E+08
Methanol 105800 - .9379 0 0 328 333 0
362.3
Table 5.13-1 Energy Balance for Boiler of DC-2
𝑄𝑏 𝑘𝑔
𝜆 ℎ𝑟.
𝑘𝑔
Flow
Component a b c d e T1 T2 𝑸𝒄
(kmol/h)
Water 276370 - 8.125 - 9E- 328 333 0
2090 0.014 06
6.16E+07
Methanol 105800 - .9379 0 0 328 333 5.83
362.3
Table 5.13-2 Energy Balance for Condenser of DC-2
∆𝑇 = 30 °C
𝐶𝑝 = 4120
𝑘𝑔°C
𝑄𝑐 𝑘𝑔
51
Chapter 6 EQUIPMENT DESIGN
AFTER ALL the preliminary work, has been completed, the detailed design work can
begin. Equipment can be designed in its final form and full specification sheets prepared
for each item. Process flowsheet and equipment list can be checked and amended. Cost
estimates can also be revised to account for any significant changes from the preliminar y
design specifications.
6.1 Reactor Design
Parameter Value Units

Reactor Type CSTR Dimensionless
Temperature 60 / 333 °C/°K
Total Conversion 99 %
Residence Time 1 𝒉𝒐𝒖𝒓
Number of Reactors 2 Dimensionless
Configuration Series Dimensionless
Molar Flow of Oil (𝑭𝒂𝒐 ) 1.355 𝒌𝒎𝒐𝒍/𝒉𝒐𝒖𝒓
Volumetric Flow Rate of Oil (𝒗𝒂𝒐 ) 1.35 𝒎𝟑 /𝒉𝒐𝒖𝒓
Cao 1.0 𝒌𝒎𝒐𝒍/𝒎𝟑
Material of Construction SS Type 304 Dimensionless
Reactor volume can be calculated by the study of kinetics in our process. The study of
kinetics can lead us to the volume by algorithms specifically designed to calculate reactor
volume, conversion etc. kinetics for the transesterification reaction have been thoroughly
studied albeit with some confusion and contradiction. Despite this we were able to find a
paper that specifically studied the soya bean oil transesterification under our specified
conditions i.e. 6:1 methanol oil ratio. And 1 % of catalyst w.r.t the weight of our oil. The
temperature however was 50 °C [10]. the reactions are as such.
𝑇𝐺 + 𝑀𝑒𝑂𝐻 ⇔ 𝐷𝐺 + 𝐹𝐴𝑀𝐸
𝑘1/𝑘2
𝐷𝐺 + 𝑀𝑒𝑂𝐻 ⇔ 𝑀𝐺 + 𝐹𝐴𝑀𝐸
𝑘3/𝑘4
52
𝑀𝐺 + 𝑀𝑒𝑂𝐻 ⇔ 𝐺𝐿 + 𝐹𝐴𝑀𝐸
𝑘5/𝑘6
𝑇𝐺 + 3𝑀𝑒𝑂𝐻 ⇔ 𝐺𝐿 + 3𝐹𝐴𝑀𝐸
𝑘7/𝑘8
The rate equations used for volume calculation are given below.
𝑑[𝑇𝐺]
= −𝑘1 ∗ [𝑇𝐺][𝐴] + 𝑘2[𝐷𝐺 ][𝐴] − 𝑘7[𝑇𝐺 ][𝐴]3 + 𝑘8[𝐴][𝐺𝐿 ]3
𝑑𝑡
𝑑[𝐷𝐺]
= −𝑘1 ∗ [𝑇𝐺 ][𝐴] − 𝑘2[𝐷𝐺 ][𝐸 ] − 𝑘3[𝐷𝐺 ][𝐴] + 𝑘4[𝑀𝐺][𝐸]
𝑑𝑡
𝑑[𝑀𝐺]
= 𝑘3 ∗ [𝐷𝐺 ][𝐴] − 𝑘4[𝑀𝐺 ][𝐸 ] − 𝑘5[𝑀𝐺 ][𝐴] + 𝑘6[𝐺𝐿][𝐸]
𝑑𝑡
𝑑[𝐸]
= 𝑘1 ∗ [𝑇𝐺 ][𝐴] − 𝑘2[𝐷𝐺 ][𝐸] + 𝑘3[𝐷𝐺 ][𝐴] − 𝑘4[𝑀𝐺 ][𝐸 ] + 𝑘5[𝑀𝐺 ][𝐴] − 𝑘6[𝐺𝐿 [𝐸] + 𝑘7[𝑇𝐺 ][𝐴]3 − 𝑘9[𝐺𝐿][𝐸]
𝑑𝑡
𝑑[𝐺𝐿]
= 𝑘5 ∗ [𝑀𝐺 ][𝐴] − 𝑘6[𝐺𝐿][𝐸] + 𝑘7[𝑇𝐺 ][𝐴]3 − 𝑘8[𝐺𝐿][𝐸]3
𝑑𝑡
The mole balance equation for a CSTR is as under…
𝐹𝑇𝐺 − 𝐹𝑇𝐺𝑜
𝑉=
−𝑟𝑇𝐺
𝐹𝑇𝐺 ∗ 𝑋
𝑉=
−𝑟𝑇𝐺
𝑑[𝑇𝐺]
𝑤ℎ𝑒𝑟𝑒 → −𝑟𝑇𝐺 =
𝑑𝑡
53
We solved the differential equations in matlab for both the reactors. The program is
provided in Appendix A. Upon solving the equations, we got two volumes each. Reactor
𝑑2
𝑉 =𝜋∗ ∗ℎ
4
5.3 ∗ 4
= 𝑑2 ∗ ℎ
𝜋
6.3 ∗ 4
= 𝑑3
𝜋 ∗ 1.5
4.5 = 𝑑 3
𝑑 ≈ 1.7 𝑚
1 has a volume of 6.3 𝑚3 while theℎsecond 3
𝑚 has a volume of 1.42 𝑚 .
≈ 2.6reactor
Similarly, for the R-2 we can calculate the diameter and height.
𝑑2
𝑉 =𝜋∗ ∗ℎ
4
1.06 ∗ 4
= 𝑑2 ∗ ℎ
𝜋
.8 ∗4
= 𝑑3
𝜋 ∗ 1.5
. 7 = 𝑑3
𝑑 ≈ 1.06 𝑚
ℎ ≈ 1.6 𝑚
6.1.1 Reactor Selection

Following are the reasons for choosing CSTR for our project.
 Liquid phase reaction.
 Provides optimal mixing.
 The reactors can be operated at temperatures between -6.66 and 232 °C and at
pressures up to 7 atm.
 Relatively cheap to construct. Also, relatively easy to clean and maintain.
54
 Ease of control of temperature in each stage, since each operates in a stationary
state; heat transfer surface for this can be easily provided hence it is relatively
easy to maintain good temperature control with a CSTR.
 Can be readily adapted for automatic control in general, allowing fast response to
changes in operating conditions (e.g., feed rate and concentration).
 With efficient stirring and viscosity that is not too high, the model behavior can
be closely approached in practice to obtain predictable performance.
6.1.2 Rate Constants

Sourced from [10] the rate constants are as such.
Rate Constants (mole/dm^3*seconds) Value
k1 .049
k2 .102
k3 .218
k4 1.280
k5 .239
k6 .007
k7 7.84e-05
k8 1.58e-05
55
Since ours is a well-mixed vessel as stated per our primary source. We need to have a stirrer
involved which basically means that there is an impeller that needs be designed.
56
6.1.3 Reactor Impeller
It is quite common practice to have vessels with some form of mixing apparatus, it I
commonly referred to as an agitator. Especially in the case of a CSTR mixing plays an
important role as the constituents are considered to be well mixed. The basis of this
assumption is that the mixing is strong enough to provide enough mass transfer. Agitators
are chosen predominantly on the basis of reactor volumes and fluid properties mainly the
viscosity.
For the selection of the reactor impeller we need to know about the reactor volume and the
viscosity of the fluid. To calculate the volume of the reactor we simply need to use the
provided ratio of impeller diameter to the rector diameter. This ratio is given in the volume
6. [11]
6.1.4 Specifications Sheet

R-1 Volume 6.3 𝒎𝟑
R-2 Volume 1.4 𝒎𝟑
R-1 Diameter 1.7 𝒎
57
R-1 Height 2.6 𝒎
R-2 Diameter 1 𝒎
R-2 Height 1.6 𝒎
Impeller Type Turbine Dimensionless
R-1 Impeller Dia. 1.06 𝒎
R-2 Impeller Dia. .6 𝒎
6.1.5 Pressure Drop

In liquid-phase reactions, the concentration of reactants is insignificantly affected by even
relatively large changes in the total pressure. Consequently, we can totally ignore the effect
of pressure drop on the rate of reaction when sizing liquid phase chemical reactors.
However, in gas-phase reactions, the concentration of the reacting species is proportional
to the total pressure and consequently, proper accounting for the effects of pressure drop
on the reaction system can, in many instances, be a key factor in the success or failure of
the reactor operation.
6.2 Heat Exchanger Design

A heat exchanger is a device built for efficient heat transfer from one fluid to another,
whether a physical barrier separates the fluids so that they never mix, or the fluids are
directly contacted. It is used for heating of one fluid while cooling the other. Heat transfer
equipment is defined by the function it fulfils in a process. Exchangers recover heat
between two process streams.
6.2.1 Types with respect to Structure

Some major types are:
 Double pipe heat exchanger.
 Shell and tube heat exchanger.
 Compact heat exchanger.
58
Double pipe consists of two concentrically arranged pipes or tubes, with one fluid flowing
in the inner pipe and the other in the annulus between the pipes. The term double pipe
refers to a heat exchanger consisting of a pipe within a pipe, usually of a straight- le g
construction with no bends. Hairpin heat exchangers consist of two shell assemblies
housing a common set of tubes and interconnected by a return-bend cover referred to as
the bonnet.
6.2.2 Principal Parts

 Two sets of concentric pipes which constitutes;
i. Inner pipe.
Annulu
ii. Outer pipe. s
iii. Annulus.
Inner pipe
 Connecting tees.
 Return head.
 Return bend.
 Packing glands.
59
6.2.3 Working Principle of Double Pipe Heat Exchanger
The basic working principle of the heat exchanger is based on the law of conservation of
heat i.e.
As by law of nature heat tends to flow from higher potential to lower potential. It tends to
equalize the temperature of both streams. But physical barrier of good conductor prevents
the both streams from physical mixing and allows only heat to flow from one to other.
6.2.4 HEAT TRANSFER MODES

 Conduction
 Convection
 Radiation
6.2.5 Types of Double Pipe Heat Exchanger

Double pipe exchangers are divided into two major types:
 Single-tube
The Single-tube type consists of a single tube or pipe, either finned or bare, inside a
shell.
 Multi-tube
The Multi-tube type consists of several tubes, either finned or bare, inside a shell.
6.2.6 Double Pipe Heat Exchangers
Advantages
 The use of longitudinal finned tubes will result in a compact heat exchanger
for shell side fluids having a low heat transfer coefficient.
 Counter current flow will result in lower surface area requirements for
60
services having a temperature cross.
 Potential need for expansion joint is eliminated due to U-tube construction.
 Shortened delivery times can result from the use of stock components that can
be assembled into standard sections.
 Modular design allows for the addition of sections at a later time or the
rearrangement of sections for new services.
 Simple construction leads to ease of cleaning inspection and tube element.
Disadvantages
 Hairpin sections are specially designed units which are normally not built to
any industry standard other than ASME Code. However, TEMA tolerances
are normally incorporated wherever applicable.
 Multiple hairpin sections are not always economically competitive with a

single shell and tube heat exchanger.
 Proprietary closure design requires special gaskets.
6.2.7 Operation of Double Pipe Heat Exchanger
Double pipe exchangers are usually assembled in 12-, 15-, or 20-ft effective lengths
(the distance in each leg over which heat transfer occurs).
When hairpins are employed in excess of 20ft, the inner pipe tends to sag and touch the
outer pipe causing a poor flow distribution in the annulus.
 The best-known use of the hairpin is its operation in true counter current flow
which yields the most efficient design for processes that have a close
temperature approach or temperature cross. However, maintaining counter
current flow in a tubular heat exchanger usually implies one tube pass for each
shell pass.
61
 The double-pipe exchanger is very flexible: vaporization, condensation, or
single-phase convection can be carried out in either channel.
 The exchanger can be designed for very high pressures or temperatures if

required.
 By proper selection of diameters and flow arrangements, a wide variety of

flow rates can be handled.
Design Calculation
The purpose of this equipment is to heat the waste vegetable oil to the required temperature.
6.2.8 Heat Exchanger Design

Assumed Calculations:
𝑄
A=
𝑈 ∗ ∆𝑇
By Assuming U = 300 W/m2 O C
Q = 90481300 J/Kg (25133 Watt)
A = 3.055 m2
As our area is not much big so we will use Double Pipe Heat Exchanger.
𝑄
m=
𝐶𝑝 ∗ ∆𝑇
m = 429.95 Kg/hr
Pipe Side (Hot Water)
Inlet temp = 90 o C
Outlet temp = 50 o C
Mass flow rate of hot water = 947.899 lb/hr
Annulus side (WVO)
Inlet temp = 25o C

62
Outlet tem = 60o C
Mass flow rate of oil = 1217.44 Kg/hr
Pipe Dimensions
We are using 20ft length of the pipe. If the length of the pipe will be greater than 20-feet,
the inner pipe tends to sag and it will touch the outer pipe and causes a poor flow
distribution in the annulus.
D2 = 0.0525 m
D1 = 0.0420 m
D = 0.0350 m
Calculation of LMTD
∆𝑇1 − ∆𝑇2
LMTD =
∆𝑇1
ln(∆𝑇2)
LMTD = 11.18 °C
PHYSICAL PROPERTIES
PHYSICAL PROPRTIES INNER PIPE ANNULUS
Hot Water WVO
Viscosity µ (Cp) 0.014 0.357
Thermal Conductivity
(k)(W/m.K) 0.636 0.243
Heat capacity(Cp) (KJ/Kg.°C) 0.221 3.818
Density ρ(kg/m3 ) 965 908
63
Annulus Side (WVO)
D 2 = 0.0525 m
D 1 = 0.0420 m
aa = 3.14(D 2 2- D1 2 )/4
aa = 0.00076 m2
Equivalent Diameter
Deq = (D2 2- D1 2 )/ D 1
Deq = 0.023 m
Mass Velocity
Ga = W/ aa
Ga = 1586494.5 Kg/hr.m2
Reynolds Number
Re = DeGa/ µ
Re = 28657.8558
L/D = 262.4
Jh = 100
Pr = Cp µ/k
Pr = 5.593063265
ho = 1853.26 W/m2 .OC
Inner pipe (Hot Water)
D = 0.0350 m
ap = 0.00096 m2
64
Gp = W/ ap
Gp = 445005.07 Kg/hr.m2
Rep = DG p / µ
Rep = 11706.02989
L/D = 175
Jh = 60
Pr = Cp µ/k
Pr = 0.129183469
hi = 97.72362084 W/m2 .OC
hio = 81.24011853
Uc = hio *ho /hio +ho
Uc = 369.12 W/m2 .OC
1/UD = 1/Uc + Rd (Rd is assume as 0.002 hr.ft2 .OF/Btu)
UD = 326.62 W/m2 .OC
Required Area
A = Q/UD∆T
A = 2.80 m2
Required Length
Required Length = Surface Area/0.435Ft2
L = 21.14 m
Actual Length
L = 24.38 m
Hairpin = 2
Actual Area will be:
65
Form table for 1.25- in we have 0.435 Ft2 of external surface per foot length.
Actual Length * 0.435
Actual Area (A) 3.23 m2
This area is close to the assumed calculation area (3.05 m2 )
The surface apply will actually be
UD = 328.771447 W/m2 OC
The overall heat transfer coefficient is close to the assumed calculation
Rd = 0.001897 m2 .OC/W
Pressure Drop (Annulus)
1) De’ = (D2 – D1 )
De’ = 0.01 m
Re’a = De’ Ga/µ
Re’a = 12520.00405
f = 0.0035 + 0.246 /( Re’a)0.42
f = 0.0085
ρ = 56.75
2) ∆Fa = 4f Ga2 L/2g ρ2 De’
∆Fa = 0.94 m.
V = G/3600 ρ
V = 1.590 FPS
3) Ft = 3(V2 /2g’)
Ft = 0.117
66
4) ∆Pa = 1.2676 Psi
Inner Pipe
1) Rep = 35030
f = 0.0035 + 0.246 /( Rep )0.42
f = 0.00675791
ρ = 60.31
2) ∆Fp = 4f Ga2 L/2g ρ2 De’
∆Fp 0.015 m.
∆Pp = 1.052 Psi
6.2.9 Mechanical Design
Selection of material
Inner pipe material : Carbon steel (approximately 0.30–0.59% carbon content)
Whose density is = 7877.61 kg/m3 (table 2-118 Perry chemical Engineering 8th edition)
The permissible stress is ft = 0.788 kg/m2
% Elongation = 28
Characteristics of material
 available in a wide range of standard forms and sizes
 good tensile strength and ductility
 not resistant to corrosion
67
6.3 Flash Tank
1. Final purification of biodiesel is achieved in the flash drum that operates under
vacuum (5 kPa).
2. Modelling of the flash tank was performed on Aspen Hysys. Material balance &
construction sheet is given in Appendix B.
3. The feed rates were taken from the material balance.
4. Pressure was provided in our primary source.
5. Temperature was set around the boiling point of water.
6. Components present in too low an amount were neglected for the ease.
7. Multiple fluid packages were used which gave similar results. These include NRTL
Ideal.
Figure 6.3.1 Flash Tank
Operating Conditions of the flash tank are given as under.

Flash Tank Conditions
Liquid Residence Time 720 𝒔𝒆𝒄𝒐𝒏𝒅𝒔
Operating Pressure 5 Kilo Pascals
Package Used NRTL Ideal Dimensionless
Valve IN Conditions
Temperature 55 °C
68
Operating Pressure 101.3 kPa
Total Feed (Molar Flow) 5 kmol/h
Mole Fraction (Triolein) .003 Dimensionless
Mole Fraction (Methanol) .0548 Dimensionless
Mole Fraction (H2O) .1350 Dimensionless
Mole Fraction (FAME) .1350 Dimensionless
Flash IN Conditions
Temperature 53.32 °C
Operating Pressure 5 kPa
Total Feed (Molar Flow) 5 kmol/h
Mole Fraction (Triolein) .003 Dimensionless
Flash UP Conditions
Temperature 110 °C
Total Feed (Molar Flow) .8359 kmol/h
Mole Fraction (Triolein) 0 Dimensionless
Mole Fraction (FAME) 0 Dimensionless
Flash DOWN Conditions
Temperature 110 °C
Total Feed (Molar Flow) .4.164 kmol/h
Mole Fraction (Triolein) 0.0004 Dimensionless
69
Table 6.3-1 Streams from Flash Tank
Design Specifications of the flash tank are given as under.

Diameter .609 𝒎
Total Length (Height) 3.353 𝒎
L/D Ratio 5 Dimensionless
Material Type Carbon Steel Dimensionless
Shell Thickness 6.350 𝒎𝒎
Corrosion Thickness 3.175 𝒎𝒎
Table 6.3-2 Design Specifications of Flash Tank
6.4 Distillation Column Design (D-1)

In industry, it is common practice to separate a liquid mixture by distillation of the
components, which have lower boiling points when they are in pure condition from those
having higher boiling points. This process is accomplished by partial vaporizat ion and
subsequent condensation
6.4.1 Choice between Plate and Packed Column

Vapor liquid mass transfer operation may be carried out either in plate column or packed
column. These two types of operations are quite different. A selection scheme considering
the factors under four headings.
Factors that depend upon the system i.e. scale, foaming, fouling factors, corrosive
systems, heat evolution, pressure drop, liquid holdup.
Factors that depend upon the fluid flow moment.
Factors that depends upon the physical characteristics of the column and its internals
i.e. maintenance, weight, side stream, size and cost.
Factors that depend upon mode of operation i.e. batch distillation, continuous
distillation, turndown, and intermittent distillation.
70
The relative merits of plate over packed column are as follows:
Plate column are designed to handle wide range of liquid flow rates without flooding.
If a system contains solid contents, it will be handled in plate column, because solid
will accumulate in the voids, coating the packing materials and making it ineffective.
Dispersion difficulties are handled in plate column when flow rate of liquid are low
as compared to gases.
For large column heights, weight of the packed column is more than plate column.
If periodic cleaning is required, man holes will be provided for clea ning. In packed
columns packing must be removed before cleaning.
For non-foaming systems, the plate column is preferred.
Design information for plate column are more readily available and more reliable
than that for packed column.
Inter stage cooling can be provide to remove heat of reaction or solution in plate
column.
When temperature change is involved, packing may be damaged.
Plates are mostly used for large diameter more than 0.6 m
For this particular process, “Methanol, DME, Water” plate column is selected because:
System is non-foaming.
Temperature is high.
Diameter is greater than 0.6 meter.
6.4.2 Choice of Plate Type

There are three main plate types, the bubble cap, sieve plates, ballast or valve plates. Sieve
plate is selected because:
They are lighter in weight and less expensive. It is easier and cheaper to install.
Pressure drop is low as compared to bubble cap trays.
Peak efficiency is generally high.
Maintenance cost is reduced due to the ease of cleaning.
6.4.3 Design Steps for A Distillation Column

Calculation of Minimum number of plates
Calculation of optimum reflux ratio
71
Calculation of theoretical number of stages
Calculation of actual number of stages
Calculation of diameter of the column
Calculation of the height of the column
Design Calculations:
Components mass %
Feed Top Bottom
Glycerol 0.08319 0.00 0.4401
Methanol 0.102 0.08416 0.00
Water 0.814 0.9158 0.5598
Stream Temperature Flow rate Pressure
℃ Kg/hr psi
Feed 100 1485.35 49.3128 (3.35 atm)
Top 98.1 1334.78 14.6488 (1atm)
Bottom 250.3 150.71 15.95 (1.019atm)
Pressure of feed = P = 49.31 psia

Temperature of feed = T = 100 oC = 373K
Boiling point of water = Tw = 101.1 °C = 374.1 K
Boiling point of Methanol= Tm = 64.8 °C = 337.8 K
Heat of Vaporization of methanol = ΔHvap = 35200 J/mol
Relative Volatility Calculation
−ΔHvapL 1 1
α =exp [ (T − T )]
R w m
72
“integratedClausius-Clapeyron equation”
−35200 1 1
α =exp [ (374 .1 − 337.8 )]
8.314
α = 3.37
6.4.3.1.1.1.1.1.1 Reflux Ratio (RD)
Colburn’s method for minimum reflux
1 x 1−x
RM = α−1 [ xdA − α ( 1−xdb )]
fA fb
1 0.08416 1−0.00
RM = [ − 3.37 ( )]
3.37−1 0.102 1−0.08319
RM = 1.5
R = 1.2 RM
R = 1.2 x 1.5
R = 1.8
73
Minimum Number of Stages
Minimum number of Stages can be found Fenske relation.
6.4.3.1.1.1.1.1.2 where:
N is the minimum number of theoretical plates required at total reflux
(of which the
reboiler is one),
Xd is the mole fraction of more volatile component in the overhead
distillate,
Xb is the mole fraction of more volatile component in the bottoms,
𝜶𝒂𝒗𝒈 is the average relative volatility of the more volatile component
to the less volatile component
N min = 4 (reboiler is excluded)
Plate Efficiency
Using O’Connell relation

Eo = 51 − 32.5 log 10 (μa αa )
µa = Molar average liquid viscosity mNs/m2 = 0.1553 mNs/m2
αa = average relative volatility = 3.37
Eo = 50.3(αa µa)-0.226
Eo = 68.226 %
Theoretical no. of Plates:
Gilliland related the number of equilibrium stages and the minimum reflux ratio and the
no. of equilibrium stages with a plot that was transformed by Eduljee into the relation:
74
𝑵 − 𝑵𝒎𝒊𝒏 𝑹 − 𝑹𝒎𝒊𝒏 𝟎.𝟓𝟔𝟔
= 𝟎. 𝟕𝟓[ 𝟏 − ( ) ]
𝑵+𝟏 𝑹+𝟏
6.4.4 From which the theoretical no. of stages to be 7
(calculated by aspen see appendix C)

6.4.5 Feed plate location
Using Kirkbride’s relation
NR 0.0831 0.00075 2 1328.75

𝑙𝑜𝑔 = 0.206log [( )( ) ]
NS 0.102 0.00662 151
NR
= 0.611
NS
R = 1.8, N=7
N r+N S = 6
NS = 6 - Nr
N s = 7 - 0.61N s Ns = 4.3
Feed plate = 4
6.4.6 Column Diameter
𝝆𝑳 −𝝆𝒗 1⁄2
𝐮𝐕 = (−𝟎. 𝟏𝟕𝟏𝒍𝟐𝒕 + 𝟎. 𝟐𝟕𝒍𝒕 − 𝟎. 𝟎𝟒𝟕)[ ]
𝝆𝒗
75
Where uv = maximum allowable vapour velocity based on the gross total column cross-
sectional area.
Lt = plate spacing, m, (range 0.5 to 1.5)
The column diameter, Dc can be calculated by
𝟒𝐯𝐰
𝐃𝐜 = √
𝛑𝛒𝐯 𝒖𝒗
Where as Vw = is maximum vapour rate, m3 /s
𝑫𝒄 = 𝟎. 𝟗𝟏𝟒𝟒𝒎
Provisional Plate Design

Column diameter = 0.914 m
Column Area A
 2
 d
4
Side DC Top Width = 120.7mm
Side DC Btm Width =120.7mm
Side DC Top Length = 0.6189m
Side DC Btm Length = 0.6189m
Net area An = Ac – Ad
= 0.6567m2
Active area Aa = Ac – 2Ad
= 0.5542m2
Hole area Ah take 10% Aa = 5.584 × 10-2 m2
Pressure drop per plate
Assume 100 mm water pressure drop per plate,
Columnpressuredrop = 100 ∗ 10−3 ∗ 1000 ∗ 9.81 ∗ 18
76
= 17658 Pa
TopPressure = 14 Psia
Estimatedbottompressure = 15.5 psia
Total Pressure Drop
ht = hd + (hw + how) + hr
Max delta P( ht of liq) = 3.871kpa ( aspen, see appendix)
Height of Column
No. of plates = 7
Tray spacing = 0.906 m
Distance between 51 plates = 0.906  7 = 3.9 m
Top clearance = 0.5 m
Bottom clearance = 0.5 m
Tray thickness = 575.1mm/plate
Total height of column = 4.267m (aspen, see appendix)
77
SPECIFICATION SHEET OF DISTILLATION COLUMN
Identification
Item Distillation Column
Item # T-501
Type Sieve Tray
Function
The separation of methanol from glycerol
Design data
No. of trays 7
Operating Pressure Slightly above than atm
Operating Temperature 101 °C
Tray spacing 079069 m
Tray thickness 3.175 mm
Height 4.267 m
Diameter 0.9144 m
Max Flooding 59%
Total Weir Length 618.9mm
Max weir load 12.63m3 /h.m
DC Clearance 38.10mm
Reflux ratio 1.8
Sieve hole Diameter 6.350mm
Sieve hole Area 5.58 ×10-2 m2
No. of Holes(estimated) 1763
Liquid density 959.119Kg/m3
Vapor density 0.5881 Kg/m3
Material of Construction Stainless steel 18Cr/8Ni Ti stabilized
(aspen, see appendix )
78
6.5 DISTILLATION COLUMN DESIGN
Feed = 1367.5263 Kg/hr = 71.3039 K.mole/hr
Components Kg/hr Mol. Wt K.mole Mole%

wt%
CH3 OH 192.1234601 32 6.0038 8.42001
H2 O 1175.402976 18 65.10036 91.2998
About (8.42001+ 91.2998) = 99.71%) of the feed consists of methanol and water. Thus
binary distillation can be assumed.
Distillate = 192.1234601 Kg/hr = 6.0038 K.mole/hr
Component Kg/hr Mol. Wt k.mole Mol. Wt

wt%
CH3 OH 192.1234601 32 5.854 99.99
H2 O 0.26964 18 0.1498 0.01
Bottom = 1175.402976 Kg/hr = 65.10036 K.mole
Component Kg/hr Mol. Wt k.mole Mol. Wt

wt%
CH3 OH 0.02688 32 0.00084 0.01
H2 O 1175.402976 18 65.10036 99.9
We get
Xf = 0.084
Xd = 0.9999
Xw = 0.01
79
(Equlibrium data from the compilation by Gmehling, J. and Onken, U. 1977. Vapor-
Liquid Equilibrium Data Collection, Dechema, Frankfurt, Germany, vol. 1, p. 60.)
from Chemical Engineering Design and Analysis: An
Introduction
T. M. Duncan and J. A. Reimer, Cambridge University Press,
1998.
Equilibrium Data for Methanol – Water is given as follows

Temp Temp x y y_calc Diagonal
(oF) (oC) (mole (mole
f) f)
212 100 0 0 0 0
209.12 98.4 0.012 0.068 0.164522 0.012
206.42 96.9 0.02 0.121 0.203265 0.02
204.44 95.8 0.026 0.159 0.226586 0.026
203.18 95.1 0.033 0.188 0.250089 0.033
201.38 94.1 0.036 0.215 0.259262 0.036
197.96 92.2 0.053 0.275 0.304281 0.053
194 90 0.074 0.356 0.349368 0.074
191.48 88.6 0.087 0.395 0.373577 0.087
188.42 86.9 0.108 0.44 0.408558 0.108
185.72 85.4 0.129 0.488 0.439742 0.129
182.12 83.4 0.164 0.537 0.485687 0.164
179.6 82 0.191 0.572 0.517318 0.191
174.38 79.1 0.268 0.648 0.595187 0.268
172.58 78.1 0.294 0.666 0.618443 0.294
169.7 76.5 0.352 0.704 0.666301 0.352
167.54 75.3 0.402 0.734 0.703963 0.402
165.56 74.2 0.454 0.76 0.740321 0.454
163.76 73.2 0.502 0.785 0.771772 0.502
161.6 72 0.563 0.812 0.809295 0.563
159.62 70.9 0.624 0.835 0.844504 0.624
156.56 69.2 0.717 0.877 0.894496 0.717
154.58 68.1 0.79 0.91 0.931129 0.79
152.96 67.2 0.843 0.93 0.956498 0.843
152.42 66.9 0.857 0.939 0.963042 0.857
150.26 65.7 0.938 0.971 0.999729 0.938
149 65 1 1 1.026572 1
Where X = Mole fracti

on of M.V.C in Liquid phase
Y = Mole fraction of M.V.C in Vapor phase
80
VLE for MeOH/H2O system
Equilibrium Diagonal
1
0.9
0.8
0.7
y (m ole frac MeOH)
0.6
0.5
0.4
0.3
0.2
0.1
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
x (m ole frac MeOH)
Now after drawing equilibrium curve
(11.49) Coulson and Richardson Vol.2

𝑥𝑑− 𝑦
𝑓
Minimum Reflux Ratio = R m = 𝑦
𝑓 −𝑥 𝑓
= (0.9999 – 0.391)/(0.391 – 0.084)= 1.98

Reflux Ratio = R = 1.5* R m = 1.5 * 1.98=2.97
6.5.1 Top Operating Line
F = 71.23kmol/hr D = 5.854 kmol/hr
W = 71.05 kmol/hr
D = 5.854Kmol/hr, XD = 0.99, xf =0.084
Ln = 17.79 Kmol/hr Vn = 23.456 Kmol/hr
𝐋𝐧 𝐃
yn = 𝐱 𝐧+𝟏 + 𝐱𝐃
𝐕𝐧 𝐕𝐧
17.79 5.864×0.999
yn = xn+1 +
23.456 23.456
yn = 0.75 xn+1 + 0.249
81
6.5.2 Bottom Operating Line
F = 71.23 Kmol/hr, xw = 0.001,
Lm = 89.09 Kmol/hr Vm = 23.655 Kmol/hr

𝐋𝐦 𝐁
Ym = 𝐱 𝐦+𝟏 − 𝐱𝐖
𝐕𝐦 𝐕𝐦
89.09 65.435×0.001
yn = xn+1 −
23.65 23.655
ym = 3.8012xm+1 −0.00276
The Points Of Top Operating Line

𝐃
(0 , 𝐱 𝐃)) ; (Xf , Xd)
𝐕𝐧
(0 , 0.249) ; (0.084 , 0.999)

The Bottom Operating Line Points
𝐁
(0 , 𝐱 𝐰 ) ; (Xf , Xw)
𝑽𝒎
(0 ,0.00276) ; (0.084 , 0.01)
82
6.5.3 Ideal no of trays is 8
6.5.4 Efficiency And Total Number Of Real Stages
Coulson and Richardson’s volume 6( page549)

Eo = 51 – 32.5 Log μ a, aa
Where
Eo = Overall column efficiency percent.
Average temperature of column = 87.5 o C = 189.5 o F
(Kaye & Laby, Engineers Edge, RoyMech and Dynesonline)

Viscosity of Methanol = 0.257 cp
Viscosity of Water = 0.325 cp

μ = (0.7108 * 0.257) + (0.2843 * 0.325)
= 0.257 cp
Eo = 51 – 32.5 Log (0.257)
= 70 %
83
Actual number of trays in column = 8 / 0.7
= 12
Feed should be entered on plate # 6
Maximum vapor flow rate in rectifying section = Vn = 23.456 kg mole/hr
Maximum liquid flow rate in rectifying section = Ln = 17.592 kg mole/hr
Maximum vapor flow rate in stripping section = Vm = 23.655kg mole/hr
Maximum liquid flow rate in stripping section = Lm = 89.09kg mole/hr
Plate spacing initial estimate = T_S= 0.5m = 18in
Calculation of column diameter based on flooding velocity
Calculate FLV = liquid vapor flow factor
LW V
FW 
VW L
LW = liquid mass flow rate kg/s
VW = vapor mass flow rate, kg/s
17.592 1.15
FWT OP =23.655 √ 750 =0.039
89 .09 .5
FWbotom =23.655 √962 =0.022
From figure 11.27 Coulson and Richardson vol.6)
t 1 = a constant obtained from fig 11.27
84
K1 Top = 0.08 K1 Bottom = 0.085
Flooding Velocity:
U f = flooding velocity
 L  V   
0.2
U f  K1  
 V  20 
962  0.5  58 
0.2
U f bottom  0.085  
0.5  20 
= 4.3 m/s
750  1.15  19 
0.2
U f Top  0.08  
1.15  20 
= 2.17 m/s
Based on 85% flooding velocity

6.5.5 Superficial Vapor Velocity
Uˆ base  4.3  0.85  3.5 7 m/s
Uˆ v,top  2.17  0.85  1.9 m/s
Maximum volumetric Flow rate = V/  V
Top = 0.573 m3 /sec
Bottom = 1.147 m3 /sec
6.5.6 Net Area Required

Maximum volume metric flow rate / superficial velocity
Top = 0.5735/1.9 = 0.30m2
Bottom =- 1.471/3.57 = 0.41m2

85
As first trial take down comer area as 12% of the total.
Column cross sectional area
Base = 0.41/0.88 = 0.46 m2
Top = 0.30/0.88 = 0.34 m2
6.5.7 Column Diameter
Diameter =√ (4 × Area /0.88  )
 2
Area =  d
4
3.14(00.34) 2 3.14(0.46) 2
Top= 4
, = 0.090 m Bottom = 4
= 0.166m
Diameter top =0.362m diameter bottom = 0.490 m

6.5.8 Height of the column :
Hc=1.2 *T_S*(N-1) taken from paper
1.2(0.5)(16-1)=9 m
Provisional Plate Design
Column diameter (base) = 0.4827 m
 2
Column Area Ac  d
4
Ac = 0.182 m2
Downcomer area Ad = 0.12(0.182)
= 0.021m2
Net area An = Ac – Ad
= 0.182– 0.021
= 0.161m2
Active area Aa = Ac – 2Ad
= 0.182 – 2(0.021)
86
= 0.14 m2
Hole area Ah take 10% Aa = 0.1 × 14 = 0.014m2
Weir length
Ad / Ac = 0.021 / 0.182 = 0.115
(From figure 11.31 vol.6)
lw / dc = 0.76
lw  1.6  0.76
lw = 1.22 m
Take weir height , hw = 50 mm
Hole diameter, dh = 5 mm
Plate thickness = 5 mm
Maximum liquid rate Lm’ = 89.09× 18 / 3600 = 0.4454 kg/sec
Minimum liquid rate at 70% turn down 0.7*0.4454
= 0.31178s kg/sec
𝑜.4454
Maximum h0w =750( )2/3 =3.9313 mm liquid
962∗1.22
𝑜 .31174
Minimum how =750(962 ∗1.22 )2/3 =3.096 mm liquid
At minimum hw + how = 50 + 3.096
= 53.096 mm liquid
From fig 11.30, Coulson and Richardson Vol.6
K2 = 30.4
87
 K  0.925 .4  d h 
U m in  2
v 1 / 2
 30 .4  0.925 .4  5
U m in 
0.51 / 2
= 14.2 m/s
min. vapour rate

Actual minimum vapour velocity 
Ah
0.70 6.5

0.155
= 28.1 m/s
So minimum vapor rate will be well above the weep point.
6.5.9 Plate Pressure Drop
Dry Plate Drop
Max. Vapour velocity through holes
Û h = Volumetric Flow Rate / Hole Area
1.417
Uh =0.155 =9.14 m/s
Fom fig. 11.43 Coulson and Richardson Vol.6
for plate thickness/hole dia = 5/5 = 1
Ah Ah .155
and    0.1
Ap Aa 1.55
Co = 0.84
From Eq.11.88 Coulson vol.6
88
2
Uˆ  
hd  51 h  V
 Co   L
9.14 0.5
hd=51[0.84 ]2 962 =3.13 mm liquid
6.5.10 Residual Head
12 .5 10 3
hr   12 .9mm liquid mm liquid
962
Total Pressure Drop
ht = hd + (hw + how) + hr
Total pressure drop = 3.12+ (50 + 3.096) + 12.9
ht = 69.116 mm liquid
6.5.11 Check Residence Time
Ad  hbc   L
tr 
Lwd
0.23  0.218  962

tr 
2.48
= 12.8 sec
> 3 sec. so, result is satisfactory

6.5.12 Check Entrainment
Uv = Maximum Volumetric Flow Rate of vapors/Net Area
UV = 1.147/ 1.78 = 0.644 m/s
89
No of Holes
Area of one hole  1.964 105

Number of Holes = Hole Area / Area of one hole
0.155
No. of holes  = 6620
1.964  105
Specification Sheet
Equipment Distillation Column
Actual No.of Trays 12
Efficiency 70 %
R 2.97
Diameter top 0.362 m
Bottom diameter 0.49 m
Height 9m
No. of holes 6620
Superficial velocity 80 % of flooding velocity
Pressure Drop 69.116 mm liquid
90
Tray Thickness 5mm
Tray spacing 0.5 m
6.6 Mixing Tank Design
6.6.1 Volume Calculation

we can calculate volume of tank by this formula
𝑄
v= τR 0.8
residence time= τR = 1 hr., volumetric flow rate

Q=2.86862 m3
3
v = 3.582 m
now we have
𝜋
V= D2L (1)
4
D= internal diameter
L=height or length
suppose
𝐿
=3 0r L=3D
𝐷
putting values of L in equation…. (1)
𝜋
v=4 D2 (3D)
3.14
3.582 = 3D3
4
3.582(4)=9.42 D3
D=1.521 m
L=3(1.521)
L = 4.563 m
6.6.2 Thickness
Pressure in tank =1 atm
91
Pressure in guage = 1-1=0
𝑁 𝑁
Design pressure=Pi=0+10% =0.1 = 0.01 𝑚𝑚2
𝑚2
Material of construction= strainless steel 18cr/8Ni

Design temperature = 55 °C
𝑁
Typical design stress at this temperature =f =160 𝑚𝑚2 (from table 13.2)
Joint factor = 1 , diameter of tank Di = 1.521 m

Thickness for cylindrical shell ‘e’
𝑃𝑖 𝐷𝑖
e=2 𝐽 𝑓−𝑃𝑖
e=0.0000475 mm
Corrosion allowance = 2mm
e=2.0000475 mm
2.2 Thickness for head section
Most standard ellipsoidal heads are manufactured with a major and minor axis ratio of 2 :
1. For this ratio, the following equation can be used to calculate the minimum thickness
required:
𝑃𝑖 𝐷𝑖
e=
2 𝐽 𝑓−0.2𝑃𝑖
𝑜.𝑜1(1.521)
e=2(1)(160)−0.2(0.01) = 0.0000475 m
Add corrosion allowance = 2mm

e = 2.0000475 mm
6.6.3 choice of closure :-

torispherical heads are used when internal pressure 0-15 bar
Pi Rc Cs
e = 2𝑓𝐽+𝑃𝑖 (𝐶𝑠−0.2)
where Cs = stress concentration factor for torispherical head

1 𝑅𝑐
cs= (3+√ )
4 𝑅𝑘
92
Rc =crown radius
Rk = knuckle radius
 (The ratio of the knuckle to crown radii should not be less than 0.06, to avoid
buckling; and the crown radius should not be greater than the diameter of the
cylindrical section. For formed heads (no joints in the head) the joint factor J is
taken as 1.0)
Rc =Rk (0.06) equal to dia of vessel
RC= (1.52)(0.06) =0.0912
Cs=0.8075
Now put the values in the main equation ..
0.01(0.0912)(0.8075)
e= =0.0000023
2(160)(1) +0.01(0.0912−0.2)
add corrosion allowance =2 mm

e = 2.0000023 mm
6.6.4 Impeller design

Type = pitched-blade turbine impeller
93
It is used when fluid is low viscous it gives radial as well as axial mixing .
Standard properties for impeller
D a = impeller diameter
D t = tank diameter =1.521 m
Impeller dia
𝑫𝒂 𝟏
=
𝑫𝒕 𝟑
1.521
Da = =0.507 m
3
94
Depth of liquid
𝐻
=1
𝐷𝑡
H=1.521
Width of impeller blades
𝑤 1
=5
𝐷𝑎
𝐷
W= 5𝑎 = 0.104 m
Length of impeller
𝐿 1
=
𝐷𝑎 4
𝐷𝑎 0.507
L= = =0.1267 m
4 4
Clearance
𝐸 1
=
𝐷𝑡 3
1.521
=0.507 m
3
Power calculation :-
In impeller design rpm is taken as 20-150.For low viscous fluid it will be 90rpm.
𝐷2 𝑁𝑝
Reynold's number=
μ
Reynold's number >10,000 so Np=KT

Np=Power number, KT=Constant for turbulent flow
For pitched blade
KT=1.27
𝑘𝑤
P = 0.04-0.10 𝑚3
D=0.507 ,N=90 rpm 0r 1.5 rps ,

𝐤𝐠
ρ= 1060.8 𝐦𝟑
𝑃
Np=𝐷5 𝑁3 𝛒
Power for impeller is given by,

P=kT N3 Da5
P=152 W = 0.152 kW
95
6.6.5 Design Data
Volume 3.582 𝒎𝟑
Internal diameter 1.512 𝒎
Height 4.563 𝒎
𝑁
Total pressure .01
𝑚𝑚2
Operating temperature 55 °C
Wall Thickness 2 𝒎𝒎
Closure Torri Spherical Dimensionless
Impeller Type Pitch Blade Turbine Dimensionless
Power for Impeller .152 kW
96
Chapter 7 INSTRUMENTATION & PROCESS
CONTROL
7.1 Introduction
Process control is an inherent requirement for any process industry in one way or the other.
Instrumentation implement in the form of actual hardware. In our project, we are to propose
the elements of instrumentation that will render control to our process. We have done that
by applying process control on the common types of equipment in our process such as the
reactor, heat exchanger and the distillation column.
7.1.1 Requirements of Control

During the operation of chemical plant, the control system must satisfy several
requirements and it must accomplish certain objectives, these are as following.
7.1.2 Safety
The safe operation of chemical process is a primary requirement for the wellbeing of the
people in the plant, thus the operating pressure, temperature and concentration of chemical
should always be within allowable limits.
7.1.3 Product Specification

To achieve the desired quantity and quality of our product we must put in place some
appropriate instrumentation. This will ensure proper production.
7.1.4 Environmental Regulation

Various laws may specify that temperatures, concentration of chemicals and flowrates of
the effluents from a plant must be within certain limits.
7.1.5 Operational Constraints

The various types of equipment’s used in a chemical plant have constraints inherent to their
operations.
97
7.1.6 Economics
The operation of a plant must conform with the market conditions, that is the availability
of raw material and the demand of the final product. Furthermore, it should be as
economical as possible in its utilization of raw materials, energy, capital and human labour.
Thus, it is required that the operating conditions are controlled at given optimum levels of
minimum operating costs and maximum profit. All the requirements above dictate the need
for continuous monitoring of the operation of a chemical plant and external control to
ensure the satisfaction of operational objectives.
Generally, a control system satisfies the following
1. Suppressing the influence of external disturbances.
2. Ensuring the stability of chemical process.
3. Optimizing the performance of chemical process.
7.2 Reactors
Measured Variable(s) 𝑭𝒐𝒊𝒍 , 𝑭𝑵𝒂𝑶𝑴𝒆 , 𝑻𝑹−𝟏

Manipulated Variable 𝐹𝑁𝑎𝑂𝑀𝑒 , 𝐹𝐶𝑜𝑜𝑙𝑖𝑛𝑔 𝑊𝑎𝑡𝑒𝑟
Controlled Variable 𝑇𝑅−1, 𝑭𝒐𝒊𝒍 /𝑭𝑵𝒂𝑶𝑴𝒆

Name of Control System Applied for
Ratio Control
Flow Control
Name of Control System Applied for
Cascade Control System
Temperature Control
Table 7.2-1 Measured, Control & Manipulated Variables for R-1
98
For the control of feeds into the CSTRs we use ratio control which divides the feed
Figure 7.2.1 Reactor Control
according to flowrate of the oil input into the CSTR. While for temperature control we use
a cascade feedback control system. A cascade control system is one which uses temperature
as a secondary measurement. We have to supply cooling water to the reactors in order to
keep the reaction temperature around the optimum (60 °C).
7.3 Heat Exchanger

The objective of this heat exchanger with this instrumentation is to keep the exit
temperature of waste vegetable oil constant by manipulating the hot water flow. There are
two principal disturbances (loads) that are measured for feed forward control: WVO flow
rate and WVO inlet temperature.
99
Figure 7.3.1 Heat Exchanger Control
7.4 Distillation Column
100
Figure 7.4.1 Distillation Column Control
101
Chapter 8 COST ESTIMATION
8.1 Introduction
Before the plant is put into production we must together some rough estimates of financia ls.
The capital needed to supply the necessary plant facilities is called fixed capital investme nt
while that for the operation of the plant is called the working principal and sum of two
capitals is called total capital investment.
An acceptable plant design must present a process that is capable of operating under
conditions which will yield a profit. Since, Net profit total income-all expenses it is
essential that chemical engineer be aware of the many different types of cost involved in
manufacturing processes. Capital must be allocated for direct plant expenses; such as those
for raw materials, labour, and equipment. Besides direct expenses, many other indirect
expenses are incurred, and these must be included if a complete analysis of the total cost is
to be obtained. Some examples of these indirect expenses are administrative salaries,
product distribution costs and cost for interplant communication.
Source for cost indices used is provided in Appendix F.
102
8.2 Equipment Cost Estimation
8.1.1 Reactor Cost Estimation
For A CSTR Cylindrical Vessel We Have:
𝐶 = 𝐹𝑚 exp(2.631 + 1.3673(lnV) − .06309(𝑙𝑛𝑉 2 ))
𝑭𝒎 2.4 Dimensionless
Volume 1644.06 𝑼𝑺 𝑮𝒂𝒍𝒍𝒐𝒏𝒔
Purchase Cost 26155 $
𝑪𝒊𝒏𝒔𝒕𝒂𝒍𝒍𝒆𝒅 (∗ 𝟏. 𝟔) 41848 $
𝑊ℎ𝑒𝑟𝑒 𝐼𝑛𝑑𝑒𝑥 𝐼𝑛 1985 = 333.3

668.1
𝐶𝑜𝑠𝑡 𝐼𝑛 2016 = 26155 ∗ = 52427.7 $
333.3
8.1.2 Flash Tank Cost Estimation
For A CSTR Cylindrical Vessel We Have:
𝐶 = 𝐹𝑚 𝐶𝑏 + 𝐶𝑎
103
𝑭𝒎 1.7 Dimensionless
Volume 34.55 𝑓𝑡 3
Purchase Cost 4562.86 $
𝑪𝒊𝒏𝒔𝒕𝒂𝒍𝒍𝒆𝒅 (∗ 𝟏. 𝟓) 6844.30 $

668.1
𝐶𝑜𝑠𝑡 𝐼𝑛 2016 = 4562.86 ∗ = 9146.2549 $
333.3
8.1.3 Heat Exchanger Cost Estimation
For Double Pipe Heat Exchanger: [12]
𝐶 = 900 ∗ 𝑓𝑚 ∗ 𝑓𝑝 ∗ 𝐴.18
𝒇𝒎 1 Dimensionless
𝒇𝒑 1 Dimensionless
Area 34.8 𝒇𝒕𝟐
Purchase Cost 1705 $
𝑪𝒊𝒏𝒔𝒕𝒂𝒍𝒍𝒆𝒅 (∗ 𝟐. 𝟎) 3410 $
104
650.9
𝐶𝑜𝑠𝑡 𝐼𝑛 2016 = 1705 ∗ = 3329.68 $
333.3
8.1.4 Centrifuge Cost Estimation
For Centrifuge:
𝐶 = 𝑎 +𝑏 ∗𝑊
𝒂 98 Dimensionless
𝒃 5.06 Dimensionless
W 1.344 𝒕𝒐𝒏𝒔/𝒉𝒓
Purchase Cost 104804.78 $
𝑪𝒊𝒏𝒔𝒕𝒂𝒍𝒍𝒆𝒅 (∗ 𝟏. 𝟐) 125765.74 $

668.1
𝐶𝑜𝑠𝑡 𝐼𝑛 2016 = 104804.78 ∗ = 210081.228 $
333.3
105
8.1.5 Distillation Column Cost Estimation (D-1)
For Distillation Column:
𝐶𝑡 = 𝑓1 ∗ 𝐶𝑏 + 𝑁𝑓2 𝑓3 𝑓4 𝐶𝑡 ∗ 𝐶𝑝1
𝐿 𝑇
𝐶𝑏 = exp(7.123 + .1478(𝑙𝑛𝑊 ) + .0248(𝑙𝑛𝑊 ) + .0158( )( 𝑏 )
𝐷 𝑇𝑝
9020 < 𝑊 < 2470000, 2 < 𝐷 < 16 𝑓𝑡. 𝑡𝑟𝑎𝑦 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟
𝑁 = 𝑁𝑢𝑚𝑏𝑒𝑟 𝑂𝑓 𝑇𝑟𝑎𝑦𝑠
𝐶𝑝1 = 204.9𝐷 .6332 𝐿.8016
2 < 𝐷 < 24
57 < 𝐿 < 170 𝑓𝑡
Material 𝑭𝟏 𝑭𝟐
Stainless steel, 304 1.7 1.189+.05770D
Carpenter (20CB-3) 3.2 1.525+.07880D
Nickel-200 5.4
Monel-400 3.6 2.306+.1120D
Inconel-600 3.9
lncoloy-825 3.7
Titanium 7.7
106
Tray Types 𝑭𝟑
Valve 1.00
Grid .80
Bubble Cap 1.59
Sieve .85
𝑭𝟏 1.7 Dimensionless
𝑪𝒃 11540 $
𝑭𝟐 1.27 Dimensionless
𝑭𝟑 .85 Dimensionless
𝑭𝟒 1.693 Dimensionless
𝑪𝒕 285.4 $
𝑪𝒑𝟏 4170.6 $
𝑪𝒑𝒖𝒓𝒄𝒉𝒂𝒔𝒆𝒅 67732.96 $

668.1
𝐶𝑜𝑠𝑡 𝐼𝑛 2016 = 67732.96 ∗ = 135770.74$
333.3
107
8.1.6 Distillation Column Cost Estimation (D-2)
For Distillation Column:
𝐶𝑡 = 𝑓1 ∗ 𝐶𝑏 + 𝑁𝑓2 𝑓3 𝑓4 𝐶𝑡 ∗ 𝐶𝑝1
𝐿 𝑇
𝐶𝑏 = exp(7.123 + .1478(𝑙𝑛𝑊 ) + .0248(𝑙𝑛𝑊 ) + .0158( )( 𝑏 )
𝐷 𝑇𝑝
9020 < 𝑊 < 2470000, 2 < 𝐷 < 16 𝑓𝑡. 𝑡𝑟𝑎𝑦 𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟
𝑁 = 𝑁𝑢𝑚𝑏𝑒𝑟 𝑂𝑓 𝑇𝑟𝑎𝑦𝑠
𝐶𝑝1 = 204.9𝐷 .6332 𝐿.8016
2 < 𝐷 < 24
57 < 𝐿 < 170 𝑓𝑡
Material 𝑭𝟏 𝑭𝟐
Carpenter (20CB-3) 3.2 1.525+.07880D
Nickel-200 5.4
Monel-400 3.6 2.306+.1120D
Inconel-600 3.9
lncoloy-825 3.7
Titanium 7.7
108
Tray Types 𝑭𝟑
Valve 1.00
Grid .80
Bubble Cap 1.59
Sieve .85
𝑭𝟏 1.7 Dimensionless
𝑪𝒃 11540 $
𝑭𝟐 1.9 Dimensionless
𝑭𝟑 .85 Dimensionless
𝑭𝟒 1.224 Dimensionless
𝑪𝒕 285.4 $
𝑪𝒑𝟏 4170.6 $
𝑪𝒑𝒖𝒓𝒄𝒉𝒂𝒔𝒆𝒅 32253.96 $

668.1
𝐶𝑜𝑠𝑡 𝐼𝑛 2016 = 32253.96 ∗ = 64653.077$
333.3
109
8.3 Total Equipment Cost
Serial No. Equipment Cost ($)
1 Reactor (*2) 17869
2 Heat Exchanger (*5) 17869
3 Distillation Column (*2) 69176.95
4 Centrifuge (*4) 419219
5 Flash Tank 6844
7 Mixing Tank (*3) 97140
Total 536984
8.4 Total Physical Plant Cost (PPC)
1 f1 Equipment Erection .4
2 f2 Piping .7
3 f3 Instrumentation .2
4 f4 Electrical .1
5 f5 Utilities .5
6 f6 Storage .15
110
𝑃𝑃𝐶 = 𝑃𝐶𝐸 ∗ (1 + 𝑓1 + 𝑓2 + 𝑓3 + 𝑓4 + 𝑓5 + 𝑓6)
𝑊ℎ𝑒𝑟𝑒 𝑃𝐶𝐸 = 𝑃𝑢𝑟𝑐ℎ𝑎𝑠𝑒𝑑 𝐸𝑞𝑢𝑖𝑝𝑚𝑒𝑛𝑡 𝐶𝑜𝑠𝑡
𝑊ℎ𝑒𝑟𝑒 𝑃𝑃𝐶 = 𝑇𝑜𝑡𝑎𝑙 𝑃ℎ𝑦𝑠𝑖𝑐𝑎𝑙 𝑃𝑙𝑎𝑛𝑡 𝐶𝑜𝑠𝑡 = 1637801.19 $
Fixed Capital
1 f7 Designing & Eng. .3
2 f8 Contingencies .1
𝐹𝑖𝑥𝑒𝑑 𝐶𝑎𝑝𝑖𝑡𝑎𝑙 = 𝑃𝑃𝐶 ∗ (1 + 𝑓7 + 𝑓8)

𝑊ℎ𝑒𝑟𝑒 𝑃𝑃𝐶 = 𝑃ℎ𝑦𝑠𝑖𝑐𝑎𝑙 𝑃𝑙𝑎𝑛𝑡 𝐶𝑜𝑠𝑡 = 1637801.19 $
𝐹𝑖𝑥𝑒𝑑 𝐶𝑎𝑝𝑖𝑡𝑎𝑙 = 𝐸𝑞𝑢𝑖𝑝𝑚𝑒𝑛𝑡 𝐶𝑜𝑠𝑡 = 2292921.66 $
8.5 Total Investment

Working Capital (5% of fixed capital) = 114646.08 $
𝑇𝑜𝑡𝑎𝑙 𝐼𝑛𝑣𝑒𝑠𝑡𝑚𝑒𝑛𝑡 𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝐹𝑜𝑟 𝑃𝑟𝑜𝑗𝑒𝑐𝑡 = 𝐹𝑖𝑥𝑒𝑑 𝐶𝑎𝑝𝑖𝑡𝑎𝑙 + 𝑊𝑜𝑟𝑘𝑖𝑛𝑔 𝐶𝑎𝑝𝑖𝑡𝑎𝑙
𝑇𝑜𝑡𝑎𝑙 𝐼𝑛𝑣𝑒𝑠𝑡𝑚𝑒𝑛𝑡 𝑅𝑒𝑞𝑢𝑖𝑟𝑒𝑑 𝐹𝑜𝑟 𝑃𝑟𝑜𝑗𝑒𝑐𝑡 = 2407567.75 $
8.6 Annual Operating Cost
Annual Fixed Cost
1 Maintenance Cost 7% of Fixed Capital 2272983.43 $
2 Operating Labour Depend on Market 159108.84 $
111
20 % of Operating
3 Laboratory Cost 1820437.50 $
Labour
20 % of Operating
4 Supervision 364087.50 $
Labour
5 Plants Overheads 50% of Operating Labour 910218.75 $
6 Capital Charges 10% of Fixed Capital 227298.34 $
7 Insurance 1% of Fixed Capital 45459.67.67 $
8 Local Taxes 2% of Fixed Capital 3913427.94 $
Total Fixed Cost 3917415.58 $
Annual Variable Cost
1 Raw Materials Depends on Market Rate 9385819.61 $
2 Miscellaneous 10 % of Maintenance Cost 15910.88 $
Total Variable Cost 9401870.06 $
8.7 Direct Production Costs

Direct Production Cost = Total Fixed Cost + Total Variable Cost = 13319285.65 $
112
8.8 Annual Production Cost
R & D Cost = 25 % of Direct production Cost
Annual Production Cost = Direct Production Cost + R & D = 16,6,49,107.06 $
Annual Production Cost (In Rs. ) = 1,744,410,192.21 𝑅𝑠.
8.9 Production Cost
Operating hours of plant per annum = 8000/ year

kg 𝑘𝑔
Product Rate = X = 10512000
hr 𝑦𝑒𝑎𝑟
Annual Production Cost 16649107 $
Production Cost = = = 1.72
Annual Production Rate 9654336 𝑘𝑔
$
Production Cost (in Rs. ) = 180.21
𝑘𝑔
113
Chapter 9 SITE & MATERIAL SELECTION
9.1 The Project
Our project deals with the production of waste cooking oils (preferably soybean oil) via
the method of base catalysed transesterification. We are to design a viable continuo us
method of production of our product using the cheapest resources possible while
maintaining little to no compromise on quality.
9.2 Proposal for Site Location

The criteria most important for the selection of our site location are as listed.
1. Raw Materials
2. Market
3. Energy Availability
4. Climate
5. Transport
6. Water Supply
7. Waste Disposal
8. Labor Supply
9.2.1 Raw Materials
The raw materials for our project are as follows.
1. Waste Cooking Oil
2. KOH
3. Methanol
Possible route for the cheapest waste oil for our product is perhaps through food markets
or at ports near Karachi where waste oil from abroad is dumped. A setup near edible
markets would be really profitable if their presence is limited to a smaller area. In this way,
our transportation cost would be massively cut down which will eventually cheapen our
fuel making it more viable for the masses. Hence it is recommended that the plant be set
near an area which deals with food items on regular basis and in large volumes.
114
9.2.2 Climate
FAMEs have an approximate pour pt. between -10 to -20 degree centigrade. It is therefore
essential that our site not be located in an area with temperatures lower than 0 degree
centigrade. This will cause the biodiesel flow to hinder and in turn the energy consumptio n
will increase.
9.2.3 Market
Our end product may be sold at conventional fuel pumps in the form of mixing of the diesel
reservoir with manufactured biodiesel in proportionate amount. However, the governme nt
must enforce stricter laws regarding air pollution prior to that. An example would be the
environmental protection laws of Europe and the United States.
9.2.4 Waste Disposal

1. Salts
2. Filter Residue
Main wastes from our production unit would be salts and filter residue. Both of these are
not that harmful for human health. Filter residue, since it is organic waste can be sold as
manure for crops. The salt can also be sourced to the preferable industries. Hence, waste
disposal is not the most critical of issues.
9.2.5 Transport
It is essential for any industry to have a sound means for both transferal of its raw materials
and its products. It is highly recommended that our project be located near a busy route. It
will also ensure the quick availability of our product to the masses. Since we’ve already
established that our project needs to be in the vicinity of a cluster of food outlets, the issue
has been resolved to a greater extent.
9.2.6 Water Supply

In biodiesel production, it is quite necessary that we have a reasonable water supply means.
This is because it is often required by the biodiesel manufacturers to wash their fuel. This
is done in order to remove the impurities. Hence a sustained water supply is necessary for
a biodiesel plant.
115
9.2.7 Labour Supply
In a country like Pakistan labour is not really an issue especially since our project is to be
located in a populous city.
9.3 Conclusion
So, a few points’ important tips for the site selection for our project are.
1. Plant should be near a mass food market.
2. Should have adequate storage facilities for waste oil collected from the above-
mentioned outlets.
3. Should be near a main road for easy transportation of raw materials and finis hed
goods.
4. It is necessary that the plant be installed in a place with a weather that is not too
cold. Else we will have to invest a lot of resources on the pumping of our finis hed
product.
5. Also, provision of energy is a key factor to our project since we will be using steam
for the removal of methanol from our (ester + methanol) mixture. We can use
natural gas for this purpose or wood which is locally sourced for winters when there
is a shortage of gas utility.
116
Chapter 10 HAZOP STUDY
A hazard and operability study is a procedure for the systematic, critical,
examination of the operability of a process. When applied to a process design or an
operating plant, it indicates potential hazards that may arise from deviations from the
intended design conditions. HAZOP is basically for safety and hazards are the main
concern. Operability problems degrade plant performance (product quality, production
rate, profit). For HAZOP, considerable engineering insight is required - engineers working
independently could develop different results.
10.1 HAZOP On Double Pipe Heat Exchanger
Guide Word Deviation Causes Consequences Action
Temperature of Low
Less flow of
Less Pipe blockage oil remains temperature
heating water
constant alarm
Temperature of High
More flow of Failure of hot
More oil increase from temperature
heating water water valve
set point alarm
117
10.2 HAZOP On Distillation Column (Parameter Pressure)
Inlet Pipe Check Inlet

NO
Deviation Rupture/Inlet No Separation Pipeline &
Valve Closed Valve
Check Inlet
Less Separation,
Leakage in Pipe Condition,
No Pressure Off Specified
LESS Column Check Tower
Product
Walls
Temperature Both
Install PIC at
Low Pressure Too High Components
MORE Inlet & TIC in
Inside the Methanol &
Column
Column Water Vaporize
118
10.3 HAZOP On Distillation Column (Parameter Temperature)
Temperature Reboiler Not No Separation of Install Flow

Higher Than Working The Components Control Valves
MORE
Required Properly Both Vaporize at Steam Inlet
to The Reboiler
119
10.4 Hazard Analysis
The Process of Hazard Identification is the procedure to assess all the hazards that could
directly and indirectly affect the safe operation of that plant and or system, and is referred
to as the Hazard Identification procedure or HAZAD. The Plant of fame having differe nt
hazards which could cause an Event (release of toxic, flammable or explosive chemica ls,
or any action) that could result in injury to personnel or harm to the environment. That
Hazards are listed in the table below:
Hazard/Threat Causes Consequence Possible

Safeguards
Exposure of Possible leak in May cause eye Flush eyes with

glycerol glycerol storage irritation. May plenty of water for
tank or line. cause skin irritation. at least 15 minutes.
Can cause Flush skin with
gastrointestinal plenty of water for
irritation. at least 15 minutes
while removing
contaminated
clothing and shoes.
Never give
anything by mouth
to an unconscious
person. Do NOT
induce vomiting
Exposure of FAME Possible leak in Severely irritation Irrigate eyes with a

biodiesel storage to skin and eyes, heavy stream of
tank or line. Inhalation cause water for at least 15
irritation of to 20 minutes.
120
respiratory tract. Wash exposed
May cause central areas of the body
nervous system with soap and
depression with water. Remove
symptoms of from area of
dizziness, headache, exposure; seek
nausea, vomiting, medical attention if
and drowsiness. symptoms persist.
Give one or two
glasses of water to
drink. If gastro-
intestinal symptoms
develop, consult
medical personnel.
(Never give
anything by mouth
to an unconscious
person.)
Fire/Explosion due Heating or any May result in loss of Storage should be

to biodiesel ignition source in human lives and designed according
storage or auto material and to internationally
ignition due to equipment loss recognized
high temperature guidance and
Flash Point requirements. Use
(Method Used): water spray to cool
130.0 C or 266.0 drums exposed to
F min (ASTM 93) fire. Dry chemical,
foam, halon (may
not be permissible
in some countries),
121
CO2, water spray
(fog). Water stream
may splash the
burning liquid and
spread fire.
Exposure of Possible leak in High concentrations If vapours or mists

biodiesel biodiesel tank in air causes frost are generated, wear
burns to eyes a NIOSH approved
irritating, to organic vapor/mist
respiratory system. respirator. Safety
Causes burns. May glasses, goggles, or
cause cancer. face shield
Harmful to aquatic recommended to
organisms. protect eyes from
mists or splashing.
PVC coated gloves
recommended to
prevent skin
contact. Employees
must practice good
personal hygiene,
washing exposed
areas of skin
several times daily
and laundering
contaminated
clothing before re-
use
122
Exposure of Possible leak of Hazardous in case Check for and
methanol methanol from of skin contact remove any contact
cylinders or pipe (irritant), of eye lenses. Immediately
lines contact (irritant), of flush eyes with
ingestion, of running water for at
inhalation. Slightly least 15 minutes,
hazardous in case of keeping eyelids
skin contact open. Cold water
(permeator). Severe may be used. Get
over-exposure can medical attention,
result in death. Cold water may be
used. Get medical
attention if inhaled,
remove to fresh air.
If not breathing,
give artificial
respiration. If
breathing is
difficult, give
oxygen. Get
medical attention
immediately
123
Appendix A Matlab Program
124
125
126
127
Appendix B Flash Tank Data
128
129
Appendix C D-1 Data
130
131
132
133
134
Appendix D D-2 Data
135
136
137
138
Appendix E Heat Exchanger Charts & Graphs
139
140
141
142
Appendix F Costing Indices
143
144
References
[1] M. A. H. b. Fangrui Ma, “Biodiesel production: a review,” Nebraska, 1999.
[2] L. W. JR., Orgainc Chemistry, Pearson.
[3] G. Knothe, Dependence of biodiesel fuel properties on the structure of fatty acid alkyl
esters, 2005.
[4] M. S. C. HUNG, “PROSPECT OF BIODIESEL PRODUCTION FROM WASTE OIL AND FAT IN
MALAYSIA,” 2010.
[5] C. M. T. S. M. L. L. &. S. Garcia, Transesterfication of soybean oil catalyzed by sulfated

zirconia, 2008.
[6] W. Y. &. B. Zhou, “Phase behavior of the base-catalyzed transesterification of soybean oil,”
Journal of the American Oil Chemists Society, 2006.
[7] Moser, “Biodiesel production, properties, and feedstocks,” In Vitro Cellular &
Developmental Biology-Plant, 2009.
[8] Y. Zhang, “Biodiesel production from waste cooking oil: 1. Process design and
technological assessment,” Elsevier, 2002.
[9] M. J. V. G. H. M. W. G. Canakci, “Used and Waste Oil and Grease for Biodiesel,” 16
December 2015. [Online]. Available: http://articles.extension.org/pages/28000/used-and-
waste-oil-and-grease-for-biodiesel. [Accessed 22 February 2016].
[10] D. Z. H.Noureddini, “Kinteic of Transesterification of Soyabean Oil,” Nebraska, 1997.
[11] R. K. Sinnot, Chemical Engineering Design, Coulson & Richardson’s Volume 6, 2005.
[12] S. M. Walas, Chemical Process Equipment (Selection & Design).
[13] J. H. Marco Aurélio, BIOFUEL PRODUCTION RECENT DEVELOPMENTS AND PROSPECTS,

Petra Zobic, 2011.
[14] D. Kern, Process Heat Transfer, McGraw Hill, 1950.
145

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Final Year Design Project

A Plant Design Report on The Production of

Department of Chemical Engineering

A report submitted in partial fulfilment of the

Department of Chemical Engineering

is not concurrently submitted in candidature of any other degree.

Chapter 1 INTRODUCTION ___________________________________________ 1

1.1 Biofuels _______________________________________________________ 1

1.2 What Is Biodiesel? _______________________________________________ 1

1.3 Advantages & Disadvantages_______________________________________ 2

1.4 What Are Oils? __________________________________________________ 3

1.5 Vegetable Oils as Fuels (Properties) _________________________________ 3

Chapter 2 LITERATURE REVIEW ______________________________________ 4

2.1 Process Selection ________________________________________________ 4

2.2 Transesterification _______________________________________________ 4

2.3 Pre-treatment ___________________________________________________ 4

2.4 Standard Practices & Their Flowsheets _______________________________ 5

2.5 Raw Materials __________________________________________________ 6

2.5.1 Choice of Oil ________________________________________________ 6

2.5.2 Catalyst ____________________________________________________ 6

2.5.3 Alcohol ____________________________________________________ 7

2.5.4 Factors Affecting the Transesterification Process ___________________ 7

Chapter 3 PROCESS DESCRIPTION & FLOWSHEET ______________________ 9

3.1 Process Flow Diagram & Description ________________________________ 9

3.1.1 Filter ______________________________________________________ 9

3.1.2 Heat Exchanger (HE-1)_______________________________________ 10

3.1.3 Pre-Treatment Reactor _______________________________________ 10

3.1.4 Heat Exchanger (HE-2)_______________________________________ 10

3.1.5 Heat Exchanger (HE-3)_______________________________________ 10

3.1.7 Pre-treatment Heat Exchanger (PT_HE-2) ________________________ 10

3.1.8 Pre-treatment Distillation (P_D) ________________________________ 11

3.1.9 Reactor1 (R1) ______________________________________________ 11

3.1.10 Heat Exchanger (HE-4)_______________________________________ 11

3.1.11 Reactor2 (R2) ______________________________________________ 11

3.1.12 Centrifuge1 (C1) ____________________________________________ 11

3.1.13 Centrifuge2 (C2) ____________________________________________ 11

3.1.14 Mixing Tank1 (Wash Tank) ___________________________________ 12

3.1.15 Centrifuge 3 (C3) ___________________________________________ 12

3.1.16 Flash Tank (FT1) ___________________________________________ 12

3.1.17 Mixing Tank2 (MT2) ________________________________________ 12

3.1.18 Centrifuge4 (C4) ____________________________________________ 12

3.1.19 Mixing Tank3 (MT3) ________________________________________ 12

3.1.20 Heat Exchanger (HE-5)_______________________________________ 12

3.1.21 Distillation Column 1 (D1) ____________________________________ 12

3.1.22 Distillation Column 2 (D2) ____________________________________ 13

3.2 Products ______________________________________________________ 13

3.1.23 Glycerine __________________________________________________ 13

3.3 Testing of Used Oil _____________________________________________ 13

Chapter 4 MATERIAL BALANCE _____________________________________ 16

4.1 Survey for Waste Cooking Oil Collection ______________________________ 16

3.1.24 Capacity Selection___________________________________________ 17

4.2 Material Balance (Filter) _________________________________________ 17

4.3 Material Balance Reactor1 (R-1) ___________________________________ 18

4.5 Material Balance (Centrifuge1) ____________________________________ 21

4.6 Material Balance (Centrifuge 2)____________________________________ 22

4.7 Material Balance (Mixing Tank 1) __________________________________ 24

4.8 Material Balance (Centrifuge 3)____________________________________ 26

4.9 Material Balance (Flash Tank) _____________________________________ 27

4.10 Material Balance (Mixing Tank 2) ________________________________ 28

4.11 Material Balance (Centrifuge 4) __________________________________ 29

4.12 Material Balance (Mixing Tank 3) ________________________________ 31

4.13 Material Balance (Distillation Column 1) __________________________ 32

4.14 Material Balance (Distillation Column 2) __________________________ 33