Group 21 Thesis

Identification of novel heterogeneous catalysts for the extraction of
potassium hydroxide (KOH) for biodiesel production
Supervised by
Mr. Tahir Asif
Submitted by
Registration NumberNumber Student Namedent
Name
2018-ME-360 Mohammad Tayyab Bin Bilal
2018-ME-367 Ahmad Sarwar
2018-ME-368 Hafiz Abdulrehman
Department of Mechanical Engineering,

University of Engineering and Technology, Lahore
A thesis submitted in partial fulfilment of the requirements of the

Degree of Mechanical Engineering at University of Engineering
and Technology, Lahore
1
10th April, 2022
Declaration
We, Mohammad Tayyab Bin Bilal, Ahmad Sarwar and Hafiz Abdulrehman, confirm that
the research included within this thesis is my own work or that where it has been carried out in
collaboration with, or supported by others, that this is duly acknowledged below, and my
contribution indicated. Previously published material is also acknowledged below.
I attest that I have exercised reasonable care to ensure that the work is original, and does not to
the best of my knowledge infringe any third party’s copyright or other Intellectual Property
Right, or contain any confidential material.
I accept that the University has the right to use plagiarism detection software to check the
electronic version of the thesis.
I confirm that this thesis has not been previously submitted for the award of a degree by this or
any other university.
The copyright of this thesis rests with the author and no quotation from it or information derived
from it may be published without the prior written consent of the author.
Print Name:
Registration NumberNumber Student Namedent Name

2018-ME-360 Mohammad Tayyab Bin Bilal
2018-ME-367 Ahmad Sarwar
2018-ME-368 Hafiz Abdulrehman
Signature: .....................................................................
Date: ..................................................................................
2
Preface
The work presented in this dissertation was undertaken at the Department of Mechanical Engineering,
University of Engineering and Technology, Lahore between October 2006 and February 2010. This
dissertation is the result of my own work and includes nothing which is the outcome of work done in
collaboration except where specifically indicated in the text. Neither the present dissertation, nor any part
thereof, has been submitted previously for a degree to this or any other university. The main text of this
dissertation-chapters one through eight-including appendix, bibliography, tables, and equations contains
approximately 12199 words. Additionally, 28 figures and 07 tables are included.
Some of the works in this dissertation have been published:
3
Abstract
The research focused towards the utilization of agriculture waste and agricultural products for
extracting the novel, low-cost, green, and highly efficient heterogeneous catalyst for biodiesel
production. Heterogeneous catalyst (KOH) is extracted by the calcination of potatoes and
spinach. Calcination has been done for 2 hours. Biodiesel was produced by transesterification
process using these catalysts (Temperature 65◦C, Reaction time 2 hours, catalyst concentration
2%wt and methanol to oil ratio 15:1). The yield of biodiesel produced from potatoes origin
catalyst was about 93.3% and from spinach origin catalyst was about 89.5%. Potato origin
heterogeneous catalyst was recommended for biodiesel production. The yield of biodiesel can
further be optimized by using RSM (Response Surface Methodology) technique.
4
Table of Contents
1. Introduction..........................................................................................................................10
1.1 Quickly reduction of fossil fuels.....................................................................................10
1.2 Effects of traditional fossil fuels.....................................................................................11
1.3 Biodiesel the best alternative source...............................................................................11
1.4 Aim and Objectives.........................................................................................................13
2 Literature Review................................................................................................................14
2.1 Background of biofuel....................................................................................................14
2.1.1 Rudolph Diesel discovery........................................................................................14
2.1.2 Henry Ford thoughts on biodiesel............................................................................14
2.1.3 Germany and allices utilization in biofuel...............................................................14
2.1.4 The international biofuels forum.............................................................................14
2.1.5 Development in South African region.....................................................................15
2.1.6 Sustainable development commission (SDC) report...............................................15
2.1.7 How South Africa overcome their problems?.........................................................15
2.1.8 Expedito Parente making biofuel.............................................................................16
2.2 Feedstocks used for biodiesel making............................................................................17
2.2.1 Availability and classification of biodiesel..............................................................17
2.3 Processes for the making of biodiesel.............................................................................20
2.3.1 Direct blending........................................................................................................20
2.3.2 Thermal cracking (Pyrolysis)..................................................................................20
2.3.3 Micro emulsion process...........................................................................................21
2.3.4 Transesterification process......................................................................................22
2.4 Base catalyst transesterification process.........................................................................23
2.5 Acid catalyst transesterification process.........................................................................24
2.5.1 Significance of transesterification process..............................................................25
2.6 Experimental procedure..................................................................................................25
2.7 Selection of alcohols.......................................................................................................26
2.7.1 Methanol..................................................................................................................26
2.7.2 Why methanol could be preferred...........................................................................26
2.8 Catalysts..........................................................................................................................27
2.9 Efficiency of acid catalyzed reaction..............................................................................27
5
2.9.1 Difficulties in acid catalyzed reaction.....................................................................27
2.9.2 Agricultural wastes used as catalysts.......................................................................28
2.10 . Reaction parameters (For homogeneous catalyst)....................................................30
2.10.1 Catalyst....................................................................................................................30
2.10.2 Methanol to oil ratio................................................................................................31
2.10.3 Time.........................................................................................................................32
2.10.4 Temperature.............................................................................................................33
2.11 Parameters (For heterogeneous catalyst).....................................................................33
2.11.1 Catalyst....................................................................................................................33
2.11.2 Methanol to oil ratio................................................................................................34
2.11.3 Reaction time...........................................................................................................35
2.11.4 Reaction temperature...............................................................................................37
3 Materials and Methods........................................................................................................38
3.1 Production of biodiesel using homogenous catalyst (KOH)...........................................38
3.1.1 Defects in reaction...................................................................................................39
3.1.2 Titration process......................................................................................................39
3.1.3 Esterification process...............................................................................................39
3.1.4 Second time esterification process performed.........................................................39
3.1.5 Perform second titration process.............................................................................39
3.1.6 Perform transesterification process..........................................................................39
3.2 Production of biodiesel using heterogeneous catalyst (spinach)....................................41
3.2.1 Extraction of KOH from spinach.............................................................................41
3.3 Production of biodiesel using heterogeneous catalyst (Potato)......................................42
3.3.1 Extraction of KOH from Potato...............................................................................42
4 Results and Discussion........................................................................................................44
When calcination was done on heater...........................................................................................44
4.1 Results of biodiesel produced from homogeneous catalyst (KOH)................................44
4.2 Results of biodiesel produced from heterogeneous catalyst (Spinach)...........................45
4.3 Results of biodiesel produced from heterogeneous catalyst (Potato).............................48
5 Further Results....................................................................................................................51
6
5.1 Maximizing the yield......................................................................................................51
5.2 Calcination of potato and spinach by using electric furnace..........................................51
5.3 Electricity consumption..................................................................................................51
6 Conclusions and Future Work...........................................................................................52
6.1 Optimization of biodiesel................................................................................................52
6.1.1 Response surface methodology (RSM)...................................................................52
6.2 Tribological behavior......................................................................................................53
6.3 Exhaust emission.............................................................................................................53
6.4 Engine testing..................................................................................................................53
6.5 Acoustic behavior...........................................................................................................53
References:................................................................................................................................54
7
List of Figures:
Figure 1: Consumption of sources in 2020................................................................................10

Figure 2: Harmful effect of fossils fuels.....................................................................................11
Figure 3: CO2 closed loop cycle [3].............................................................................................12
Figure 4:Biofuel vs Petroleum fuel emission comparison [18]................................................17
Figure 5:The feedstocks for biodiesel synthesis [20]................................................................18
Figure 6: The oil proportion of feedstocks for biofuels [30]....................................................19
Figure 7:Thermal cracking process [35]....................................................................................21
Figure 8:Reaction of transesterification process [42]...............................................................22
Figure 9:Schematic diagram of transesterification process [36].............................................23
Figure 10:Flow diagram of biodiesel production [38]..............................................................24
Figure 11:Experimental Apparatus of Transesterification process [39]................................25
Figure 12: Agriculture products.................................................................................................28
Figure 13: Effect on Biodiesel production at different methanol: oil ratio [67]....................31
Figure 14: Biodiesel production by varying time.....................................................................32
Figure 15: Biodiesel yield by varying temperature [71]...........................................................33
Figure 16: Biodiesel yield as a function of catalyst amount utilized [12]...............................34
Figure 17: Effect of methanol to oil ratio on biodiesel yield [14]............................................35
Figure 18: Biodiesel yield at varying reaction time [13]..........................................................36
Figure 19: Biodiesel yield by varying temperature [12]...........................................................37
Figure 20: Transesterification process.......................................................................................38
Figure 21 : Flow diagram of transesterification process..........................................................40
Figure 22: Biodiesel from homogeneous catalyst......................................................................41
Figure 23: Calcination of spinach..............................................................................................41
Figure 24: Calcination of potatoes.............................................................................................43
Figure 25: FTIR Test graph.......................................................................................................45
Figure 26: FTIR Test graph.......................................................................................................47
Figure 27:FTIR Test graph........................................................................................................49
Figure 28: Working of RSM [12]...............................................................................................52
8
List of Tables:
Table 1: Fatty acid composition of feedstocks for biodiesel.........................................................19
Table 2: Catalyst derived from agricultural waste.........................................................................29
Table 3:Reaction parameters and yield..........................................................................................30
Table 4: Viscosity of biodiesel......................................................................................................32
Table 5: Operating parameters for biodiesel using homogeneous catalyst...................................40
Table 6: Operating parameters for biodiesel using heterogeneous catalyst..................................42
Table 7: Operating parameters for biodiesel using heterogeneous catalyst.................................43
9
Chapter 1
1. Introduction
Through the transportation and energy conversion sectors, fossilized energy has the
greatest impact on global economic contribution and development. About half of the
world's oil is produced in the Middle East, with the remainder coming from Asia's
central area and the American continent [1].
1.1 Quickly reduction of fossil fuels

The need for energy will rise over time as the population, industrial growth, agriculture,
and transportation sectors all grow. As a result, we must shift our focus to other
alternative fuel sources in order to satisfy the world's energy needs [2]. Biodiesel is an
excellent alternative renewable energy source that is environmentally benign and less
hazardous to overcome the lack of traditional fossil fuels. Sulphur and aromatic
chemicals, which cause hazardous emissions, are not present in biodiesel, making it
environmentally friendly. According to the World Health Organization, coal and oil
provide more than half of the world's energy needs [3].
Figure 1: Consumption of sources in 2020
10
1.2 Effects of traditional fossil fuels
Diesel engines now burn fossil fuels; however, it is predicted that the quantity of fossil
fuels will be reduced in the future. By 2030, global oil need is estimated to propel by
50%. This is due to peak fuel output, which results in a significant loss in fuel reserves.
This, in turn, raises the desire for success and, as a result, the price of fossil fuels [4].
Figure 2: Harmful effect of fossils fuels
1.3 Biodiesel the best alternative source

Biodiesel is a recyclable and sustainable resource that has the potential to
accommodate the current and future demand [1]. It is a viable alternative to fossil
fuels, which cause ozone depletion. It produces less pollutants when consumed
and can be used in diesel engines without requiring any adaptations [2].
Biodiesel's impact to environment is dramatically lower. Biodiesel usage as a
promising energy source, it has the feature of being sustainable, because the CO 2
emitted is not harmful to the environment.
11
Figure 3: CO2 closed loop cycle [3].
This figure presents the technique by which reusable plant sources are
transformed into biofuel, resulting in zero CO2 emission. It can be kept anywhere,
much the same as petro diesel fuel, because it has good storage attributes. When it
comes to addressing, shipping, and preservation, biodiesel has less chemical
challenges and threats than traditional diesel fuel [3]. Biodiesel may be formed
from oil and fats, which offers a way for biofuels [4]. Feedstock deduct 75% cost
of biodiesel production. Biodiesel is subdivided into three categories based on
where it comes from and what it consumes as a source: first generation, second
generation, and third generation. CH3ONa, NaOH and KOH are some of the most
frequent identical alkaline catalysts being used biofuel production [5]. To get true
speed, the homogeneous catalyzed technique with best-quality feedstocks with a
(FFA) quantity less than 3.2% by weight. Furthermore, the water in the feedstock
makes more complication since hydrolysis as it releases FFAs, which
subsequently react with catalysts to form soap [6]. Heterogeneous catalytic has a
benefits over homogeneous catalytic as it reduced energy consumption, and less
water use [7]. There are several strategies for boosting biodiesel production
recorded. RSM (Response Surface Methodology) was among the most broadly
12
applied techniques [8]. RSM is a mathematical approach for developing empirical
models. Yield is defined as the reaction to independent variables, which are the
transesterification process' operational parameters. RSM creates an appropriate
experimental design model to ensure the best possible operating conditions [9].
Many emerging countries' economies, such as Pakistan's, have become
uncompetitive owing to a lack of useable energy. Pakistan is one of those
economies that has the potential to create enormous amounts of renewable energy
due to its large agricultural area and population of over 220 million people. So
biodiesel is now uneconomical, necessitating need more study and technical
development.
1.4 Aim and Objectives
Aim of the Project

The aim is to find the better way of extracting the heterogeneous catalyst and to produce
the biodiesel through novel heterogeneous catalyst.
Objectives
• To identify the novel heterogeneous catalyst for the extraction of potassium hydroxide
(KOH) for biodiesel production.
• To compare the results of calcination done on electric heater and on electric furnace.
• To compare the yield of biodiesel using different heterogeneous catalysts.
• To examine the thermo-physical characteristics of produced biodiesel.
13
Chapter 2
2 Literature Review
2.1 Background of biofuel
Biofuels are not a new concept. In reality, the present procedure for producing
biofuels from biomass is the same as that has been used in the past. In addition,
the fuel sources used in their preparation were highly similar. Bean, hemp and
maize oil, as well as animal fat, have been utilized in the past. Wheat, rapeseed,
residual oil, forest wastes, and trees are being used to replace some of the fossil
fuels. Molasses is a kind of sugar cane [10].
2.1.1 Rudolph Diesel discovery

Since the dawn of the car industry, liquid biofuels have been utilized for
transportation. The IC engine was developed to run on ethanol by August Otto. In
his initial demonstration of his IC engine at the World's Expo in 1898, Rudolph
Diesel used peanut oil until the 1920s.
2.1.2 Henry Ford thoughts on biodiesel

Diesel was not the only one who believed that biofuels may be the automotive
industry's future. Similarly, Henry Ford was so certain that natural energy was the
key to his automobiles' success that he built them to run on ethanol (starting with
the 1907-08 Model T). He also established an alcohol unit to distribute the fuel
through their distribution substation [11].
2.1.3 Germany and allices utilization in biofuel
In World War II Germany faced oil shortages. The cars were then fueled by a
mixture of gasoline and alcohol fermented from potatoes known as
Reichskraftsprit. In the United Kingdom, the Distillers Company Ltd. combined
grain alcohol with gasoline and sold it as Discol through Esso's partner Cleveland.
Despite their usage during WWII, biofuels have stayed in the shadows, where
they were driven into by fossil fuels (petroleum) [12]. The robust petroleum
industry infrastructure made the globe very reliant on foreign oil until the 1970s.
The two crises took place in 1972-73. The second one, in 1977-78, was five years
later [13].
2.1.4 The international biofuels forum

China, Brazil, South Africa, India, US, and the European Commission make up
the UN International Biofuels Forum with Sweden, France and Germany leading
the world in biofuel production and consumption [14].
14
The whole expansion of biofuels business has been sparked by a crisis brought on
by excessive usage of fossil fuels, which has resulted in supply constraints, high
inflationary costs, and severe environmental consequences.
Energy production in Africa are widely dispersed, and the majority of South
Africans are net power importers since petroleum products are costly to acquire,
putting a financial strain on their economies and compromising their energy
security and sovereignty. However, despite its massive resource base, Africa has
vast biomass resources that are now underutilized or unutilized, and hence has the
potential to become a substantial source of biofuels, with such utilization
potentially contributing significantly to poverty reduction in rural African areas.
2.1.5 Development in South African region

Southern Africa is thought to contain the world's biggest untapped biofuels
potential. Continuous usage of nonrenewable fossil fuels has major environmental
consequences, while oil reserves are fast depleting as a result of rising worldwide
consumption, resulting in restricted supply and price variations. Diesel soot is
known to cause cancer, and burning diesel has been recognized as a large
contribution to worldwide man-made CO2 output [15].
2.1.6 Sustainable development commission (SDC) report

According SDC report biofuels reduces (GHG). The usage of biofuels must be
weighed against potential environmental and societal consequences, among other
things. Biofuels are details of the research for both advanced and emerging
economies for a multitude of reasons. Increased agricultural production in the
surrounding area, as well as new markets and money for farmers; and, as a result,
an increase in agricultural productivity [16]. Biofuel substitutes should reduce
dependency on oil while simultaneously helping to fulfil the GHG emissions
target to the greatest extent possible.
2.1.7 How South Africa overcome their problems?

The industry in South Africa accounts for over 15-17% of the country's GHS
emissions, making highest in Africa. According to Chapman (2007), this sector is
responsible for 26% of worldwide CO2 emissions, with about two-thirds coming
from the world's wealthiest 10%. Diesel fuel is accountable for almost 16-18% of
total emissions, or 11,750,000 tons of CO 2 eq. The usage of diesel fuel for power
generating releases an additional 1,622,000 tons. Ecologically friendly source of
energy is necessary to minimize CO2 emissions from automobile transportation
[17]. According to Thurmond studies, bio-proportion fuels of the vehicle fuel
industry is expected to expand rapidly during the next decade (2010). According
to IEA (2007) statistics, the use of these biofuels has increased exponentially in
15
the European Union (EU) during the previous several years (Figure 2). Biofuels
must gain energy.
Figure 2 Biodiesel consumption [17].
2.1.8 Expedito Parente making biofuel

Expedito Parente, a Brazilian scientist, produced the first authentic biodiesel fuel
in 1977, using a technique which is transesterification. He secures a patent for
biodiesel fuels using his technology. Rudolf Diesel developed the first
compression ignition engine, which employed huge injectors to minimize
clogging while utilizing fuels [18]. The petroleum sector then proceeded to
produce low-cost medium-weight diesel fuels, thereby shutting down the biofuel
business. The background of biofuel start in 1900 during the world fair of Paris,
when one of the five engines on display used peanut oil.
16
Figure 4:Biofuel vs Petroleum fuel emission comparison [18].
2.2 Feedstocks used for biodiesel making

Over 355 oil-producing plants have now been identified as possible biodiesel
triglyceride sources. Selecting the correct source is the key. Appropriate feedstock
should ideally meet two requirements: industrial-scale production with the lowest
possible cost [19].
2.2.1 Availability and classification of biodiesel

The cost and availability of raw materials for biodiesel synthesis are influenced
by the region's weather conditions, soil characteristics, geographical position, and
farming techniques [21]. Figure 2 depicts the three source groups for biodiesel
production. When assessing any new biodiesel feedstock, the oil yield and total
development of agricultural land are important factors to consider [22].
17
Figure 5:The feedstocks for biodiesel synthesis [20]
For biodiesel 1st generation feedstocks are commonly accessible. Sunflower oil
[20], coconut [21], Palm [22], olive, mustard, soybean [23] and rapeseed [24] are
among the plant oils. The use of vegetable oils has impacted supplies throughout
time, as this practice has a worldwide food market repercussion, disrupting
availability and pricing. As a result, edible oils are too expensive to employ for
fuel generation due to their high demand for food [25]. As a result, if the usage of
first-generation feedstocks maintains, the world may soon confront the "food vs.
fuel" dilemma. Because of their capacity to synthesis biodiesel, the cost of both
biodiesel and oils may rise [26]. Because it necessitates a larger amount of land
for feedstock cultivation, the method has significant environmental consequences.
This results in deforestation, particularly in tropical areas. Continued use of this
method for biodiesel production might harm flora and animals, with consequences
including weather changes. Alternative feedstocks for biodiesel synthesis were
investigated in order to reduce reliance on first-generation feedstocks [27]. In
comparison to generate biodiesel is seen to be useful in avoiding food shortages
and making biodiesel a premium procedure. The extraction of oil for biodiesel is a
time-consuming procedure that adds to the total cost of production [28]. Because
18
of the lack of rivalry with food, the second-generation feedstocks outlined below
are abundant in nature [29].
Figure 6: The oil proportion of feedstocks for biofuels [30]

Non-edible crops' oil might be applied as an additional source of biofuel by
tapping into non-usable oils, overcoming the food vs. fuel fight. Non-usable oil
plants may be produced primarily on wastelands across the world, reducing the
need for future deforestation and addressing food security concerns. The
proportion of oil that can be extracted and the agricultural output from cultivated
land are two primary elements that make a feedstock a consideration for
manufacturing biofuel. Non-edible oils might be effective biodiesel sources since
they are easily transferable in liquid form, renewable, efficiently combustion,
have minimal Sulphur and scent content, and are sustainable [30]
Table 1: Fatty acid composition of feedstocks for biodiesel
19
The long-term sustainability of these non-edible oils for biodiesel generation is
another incentive to promote them:
(1) These oils are accessible, and public support for producing biodiesel
encourages them.
(2) They sidestep the fuel vs. food debate [31].
2.3 Processes for the making of biodiesel
2.3.1 Direct blending

Fatty oils or vegetable oil can be used as a fuel in internal combustion engines as
it has a high heating value and can generate enough output. However, because its
unfavorable characteristics, it cannot be used without modification in the DI
engine. Alternative fuel sources are mixed directly with traditional fossil fuels to
reduce these dangers. This form of blending is the most feasible technique to use
fuels like biofuels as it improves fuel quality and reduces fossil fuel consumption.
The quantities of bio oil and diesel will fluctuate, such as 10:1.5, 10:2.5, 10:3.5,
and so on [37]. Despite the fact that the vegetable oils had biodiesel-like
properties, they had to be chemically treated before being used in the engine.
Though it has been experimented with almost a century, it has only recently been
properly examined. While some engines may run on pure vegetable oils,
turbocharged spark ignition engines.
2.3.2 Thermal cracking (Pyrolysis)

It is a method of converting a hydrocarbon's complicated structure into its
simplest form, either with or without the use of a catalyst. In this technique,
density and friction of the oil will be lesser. When adopting vegetable oil as a
renewable fuel, these two factors have an influence on engine atomization. The
fuel may now be utilized directly in a diesel engine without any changes as a
consequence of this technique. In the thermal cracking process for biodiesel
synthesis, alumina, zeolite, and red mud are often employed as catalysts [34].
Thermal cracking carried out between 250 to 355 ° C. A reactor, a safety valve, a
drain pipe, a temperature meter, and other components make up the thermal
cracking biodiesel plant. The biodiesel-making from oils or animal fats are
injected into the reactor, which is subsequently heated. The fat is now burnt and
delivered to the condenser through pipes. The condenser helps to cool the vapor
in the liquid, and the liquid is kept in the beaker, which is called renewable diesel
20
[39]. The depicts of the biodiesel synthesis process utilizing the thermal cracking
method is shown below.
Figure 7:Thermal cracking process [35].
2.3.3 Micro emulsion process

It's a liquid mixture of oil, water, and an emulsifier that's thermodynamically
stable. The interfacial tension between two liquids that would eliminate oil's
viscosity and other atomization characteristics [40]. Alcohol is typically used to
increase the flammable quality of the oil, which lessens smoke. Alkyl nitrate will
be used as an octane booster. The micro emulsion approach was also used to
obtain a good spry property when injected into the engine through nozzle. If
micro emulsified fuel has been used in engine, it will lead to uneven ignition,
carbon deposition, and nozzle breakage [41]. The use of alcohol such as CH 3OH,
C2H5OH, and C4H10O in micro-emulsions as a solution to the problem of
excessive viscosity in vegetable oils has been examined. By exploding the low
boiling elements in the micelles, they can increase spray properties.
21
2.3.4 Transesterification process
When triglycerides and alcohol interact they form fatty acid methyl ester and
glycerol.
Figure 8:Reaction of transesterification process [42].

The procedure is divided into many stages. The alcohol mixed with the catalyst.
After that, the fatty acid reacts with the alcohol/catalyst, resulting in the
transesterification reaction that demonstrates the catalyst's preparation with
alcohol. The OH- takes the hydrogen from the methanol, resulting in water, leaves
the CH3O- available for action. It's best if the methanol is dry. When the OH- ion
acts with the H+ ion, water is formed. Water raises the chance of soap production
as a result of an unfavorable side reaction with free fatty acids. Lipases can also
be used; alcohol is still required, but it just serves as a catalyst [42]. Lipases are
slower, more expensive, and provide poorer yields than chemical catalysts. After
the catalyst is generated, the triglycerides will react with mols of methanol, thus
more methanol must be added to ensure complete reaction. The overall quantity
of biodiesel and glycerin produced, as well as the amount of chemicals necessary
to complete the reaction The reaction completes because the amount of methanol
injected is roughly double that required. Using fat and 15-20 pounds of alcohol,
the process creates a considerable amount of biodiesel and glycerin. The reaction
occurs at a temperature range of 45 to 60 degrees Celsius. The rate of reaction
slows as the temperature of the reaction rises, taking around 1-2.5 hours at 65°C
against 2.5-4.5 hours at 45°C. The reaction will be completed fast if the ratio is
doubled. Both glycerol and biodiesel must be de-alcoholized before being reused.
To clean any undesired side products, mostly glycerol, that may remain in the
22
biodiesel, add water to the biofuel and glycerol. After the wash water is removed
from the biodiesel using a solvent extraction technique (which includes some
glycerol), the trace water is evaporated [43].
Figure 9:Schematic diagram of transesterification process [36]

As previously mentioned, the process's beginning reactants should be as dry as
possible. It may be used to separate Na and K from OH⁻, allowing the ions Na+
and K+ to combine with fatty acids to form soap. The formation of a free fatty acid
may be aided by water which can then combine with the Na+ ion to generate soap.
The sodium that was utilized as a catalyst has now become bonded to the fatty
acid and is no longer useful. It also makes separation and recuperation more
difficult. Animal fats are an unappealing feedstock [36].
2.4 Base catalyst transesterification process

Catalysts such as KOH, NaOH, and sodium methoxide are utilized in this process.
The best catalyst, however, is sodium methoxide, which is also the most
23
expensive [45]. To achieve the best biodiesel production, keep the reaction
temperature between 500 and 600 degrees Fahrenheit. The temperature should be
lower than methanol's. Methanol would otherwise be wasted owing to
evaporation. The stirring procedure (1300 rpm) is used throughout the operation
to accelerate the pace of reaction through dynamic mixing. The biodiesel and
glycerol produced by the aforesaid reaction should be separated, as a result the
solution should be split for 12 to 24 hours in a separate tank [46].
2.5 Acid catalyst transesterification process

Some feedstock contains over than 1.1% FFA which protect biofuels. The
transesterification process will produce very small quantity fuel. The feedstock oil
is implicated in this situation to describe a kind of fatty acid that the ester is
formed when a ketone is transformed into a ketone [37]. It got longer time
therefore it's not the best option [38]. The alcohol reacts with the oil in the
presence of an acid catalyst, resulted in the formation of alcohol. The biodiesel
and water must be separated as soon as possible since the water will trigger the
growth of mould [39].
24
Figure 10:Flow diagram of biodiesel production [38].
2.5.1 Significance of transesterification process

All the researches and analysis concludes that the transesterification process is the
optimal method for producing biofuel, and following are the primary reasons for
this decision.
• There is no soap making occur and it accelerates both esterification and
transesterification processes rate.
• Catalyst reaction time are higher, the costs are much lower, and the
catalysts are more readily available.
• Catalysts are non-corrosive, recyclable, and have a higher selectivity than
other materials.
2.6 Experimental procedure

In the experimental testing oil sample was weighed and placed in a three necked
flask in a fume closet for transesterification.
25
Figure 11:Experimental Apparatus of Transesterification process [39].
2.7 Selection of alcohols

Alcohol is one of most significant parameter for biodiesel production. Through an
alcoholysis reaction, any oil or fat can be transformed into fatty acid mono alkyl
esters (BD) (transesterification). A base, acid and enzyme catalysts are used to
react the oil or fat with mono-alcohols.
The purpose of this reaction is to convert oil or fat into a fuel with necessary
parameters such viscosity, boiling temperature, and flash point. Factors such as
technological, environmental, and strategic advantages, BD is the most commonly
acknowledged alternative fuel for engines [50]. Alcohols are primary and
secondary monohydric aliphatic alcohols having 1–8 carbon atoms [51]. A
number of alcohols have been examined for biodiesel generation; the most often
used acyl acceptors are methanol and, to a lesser degree, ethanol. Short-chain
alcohols such as propanol, butanol, isopropanol, tert-butanol, branched alcohols,
and octanol are also utilized in biodiesel manufacturing, but they are costly [52].
Methanol and ethanol are the most often utilized alcohols in biodiesel production.
Methanol is preferred because to its physical and chemical capabilities. It also
reacts immediately with triglycerides and dissolves quickly in NaOH [53].
26
Methanol is well-known as Wood Alcohol. Wood alcohol is highly burnable and
harmful. It's one of a slew of hazardous compounds contained in cigarette smoke.
Methyl alcohol is another name for methanol [40].
2.7.1 Methanol
Methanol is the most frequent alcohol utilized in the production in the
transesterification process. On the other hand, the amount of water in alcohol is
critical for its application in biofuels. This is because water causes triglycerides to
hydrolyze into free fatty acids during the transesterification process, resulting in
soap formation and low output.
Unfortunately, all short-chain alcohols are hygroscopic, which means they collect
water from the air readily [55]. Long-chain alcohols, on the other hand, are more
susceptible to contamination from water [56]. Biodiesel is manufactured from a
variety of alcohols [57].
2.7.2 Why methanol could be preferred
In particular, methanol is used in the making of biofuel because it has low market
price and highly reactive [41]. Mainly two considerations contributing to the
carefully choosing of methanol despite its high poison level [42]. Methanol not
make an azeotrope; therefore, it can reuse. Biodiesel fuels made from methanol
and ethanol exhibit slight distinctions of their qualities as fuels. Biodiesel produce
from methanol have high pour and cloud points and less viscosities [43].
2.8 Catalysts
To improve the reaction rate and yield, a catalyst is usually used. To activate the
transesterification process, chemical or biological catalysts are used. These are
effective in speedup the process, despite the fact that the reaction needs a lot of
energy and a long purification step to get the refined product [44]. Immobilized
lipases are the most popular biological catalysts [45].Acid catalyzed reactions are
further divided in two categories. [46]
• Homogeneous acid catalysts
• Homogenous base catalysts
2.9 Efficiency of acid catalyzed reaction

Acid catalyzed transesterification is not recommended to produce bio diesel due
to its slower rate of reaction. An examination depicts the utilization of acid
catalyzed reaction to deliver biodiesel by utilizing soybean oil combined with
methanol using 0.9%wt of HCl. The result obtained was almost 90-93%
transformation of triglycerides to biodiesel after 69 hours [47]. Similarly, some
researchers studied the different parameters affecting the biodiesel production
27
[48]. Researchers examined the special effects by varying oil to alcohol
proportion, volume of catalyst and time of reaction for conversion of esters by
using acid catalyzed reaction. They concluded that increased in oil to alcohol
ratio, increased quantity of HCl and increased the rate of reaction favors the
production of biodiesel [49].
An experiment was performed to produce biodiesel by taking acid catalyzed
reaction at pilot plant scale. Acid concentrations of 1.5-3.5 mole% were used.
97% of conversion of methyl eaters were obtained when 240 minutes were given
for the reaction [50]. This experiment also shows that acid catalyzed reaction uses
very higher amount of alcohol, and reaction time.
2.9.1 Difficulties in acid catalyzed reaction

A study shows that acid catalyzed reactions are not favorable to produce biodiesel
at industrial scale though acid catalyzed reaction is very slow. They need
considerable time to be carry out. These reactions have a big advantage that these
types of reactions do not require any type of pre-treatment step. This method is
free of presence of free fatty acids [51]. We mostly use the sulfuric acid or
hydrochloric acid for transesterification because these catalysts are easily
available and also cheaper than other catalysts. Due to the higher reaction times, it
is uneconomical to use acid catalyzed reactions for larger capacity productions of
biodiesel [52].
2.9.2 Agricultural wastes used as catalysts

Due to environmental concerns, the global practice of converting garbage into
useful resources for multiple applications is gaining popularity. Diverse
commercial heterogeneous catalysts for turning various feedstocks into fuels have
recently been described in the literature. [53] Despite the fact that these
heterogeneous catalysts have been proved to be quite effective, they are still
recognized as experimental. Due to the labor-intensive procedures needed in
generating biodiesel, it is unsustainable. In the process of synthesis moreover,
these catalysts are non-renewable and commercially supplied. As a result of the
use of catalysts, disposal challenges and environmental concerns arise [19]. The
agricultural waste-based catalysts, such as banana and orange peels, cocoa pods,
Husk ash, Musa balbisiana peel ash, leaf ash, banana trunk ash, and coconut husk
etc. They are non-toxic, cheaper, non-corrosive, and freely accessible. [54]
28
Table 2: Catalyst derived from agricultural waste
Waste Preparation Catalyst Oil Reaction Yield References

Used Parameters
(A/O, Catalyst
wt.%, Time,
Temperature)
It was completely Soybean 7, 0.8, 250, 26 99 [55]
Banana Potassium
burnt in the open air
peels oxide
to make ash.
Grapefruit Calcination at 700 Potassium Palm 9, 5, 170, 63 98 [56]
peels ◦
C, for three hours oxide
Wild Calcination at 800 greater % of Used 7, 3, 190, 63 98 [57]

banana
◦
C, for five hours K cooking
peels oil
Pineapple Calcination at 700 Reasonable % Soybean 30, 6, 27, 62 98 [58]
leaves ◦
C, for three hours of Potassium,
calcium,
magnesium
mustard Heated at 600 ◦C for
K2O Soybean 14, 8, 26, 63 99 [22]
plant three hours
Banana Calcination at 800 Reasonable % kapok 10, 2, 72, 68 99 [10]
stalk ◦
C, for five hours of Potassium,
calcium,
magnesium.
Walnut Calcination at 900 Reasonable % Sunflower 14, 6, 12, 62 97 [59]
shell ◦
C. of Potassium,
calcium,
magnesium.
Potassium Used 7, 3, 200, 26 99 [60]
Teak Calcination at 800
oxide cooking
leaves ◦
C, for five hours
oil
Banana Oxides of Soybean 7, 0.7, -, 27 97 [61]
It was completely
trunk potassium,
calcium and
to make ash.
magnesium
Cocoa pod Calcination at 600 Reasonable % 14, 6, 160, 63 99 [16]
Malabar
husk- ◦
C, for five hours of Potassium,
plantain Kino
calcium,
peel blend seed
magnesium
It was completely Soybean 7, 5, 350, 27 97 [39]
Mango Potassium
peels oxide
to make ash.
Orange It was completely Potassium and Soybean 7, 8, 430, 26 97 [62]
peel burnt in the open air calcium
to make ash. content
Cocoa bean Calcination at 800 Reasonable %
Neem oil 2.9/1.9, 0.55, 56, 64 98 [63]
husk ◦
C, for five hours of Potassium.
29
2.10 . Reaction parameters (For homogeneous catalyst)
2.10.1 Catalyst
Biodiesel yield produced from sunflower, soybean, and Waste cooking oil by
using different catalyst and at different concentration. [64]
Table 3: Reaction parameters and yield
Parameters Biodiesel Production
Catalyst(%wt/wt) Temperature(°C) Time(min) Sunflower Soybean Waste

oil oil cooking
0.5% KOH 30 60 78 75 63
90 78 80 60.5
1% KOH 30 60 78 80 64
90 87 84 74
0.5% KOH 60 60 94 83 77
90 92 90 75
1% KOH 60 60 92 94 80
90 95 96 90
0.5% NaOH 30 60 76 74 57
90 72 76 67
1% NaOH 30 60 74 69 66
90 72 70 68
0.5% NaOH 60 60 81 85 67
90 93 92 88
1% NaOH 60 60 96 95 88
90 92 93 87
For all the types of oil sample analyzed, the maximum yield of biodiesel was
achieved at 0.9 wt%. [65]
Bigger concentration of catalyst gives maximum production of biodiesel in lesser
time, according to reaction kinetics. On the other side, it allows for greater soap
formation, which makes washing and filtering bio diesel more difficult, as well as
raising the cost of biodiesel synthesis due to the need to acquire more catalyst. As
30
a result, based on these considerations, the optimum amount of potassium
hydroxide deemed acceptable was 0.9 wt%. [66]
2.10.2 Methanol to oil ratio
As a follow-up to the tests conducted with different oil samples using KOH as
catalyst.
Figure 13: Effect on Biodiesel production at different methanol: oil ratio [67]
More yield is produced by increasing the alcohol [67]. The oil dispersion during
agitation is usually improved by a high methanol/oil ratio, making
transesterification easier. When the amount of methanol used in these studies was
increased, the viscosity of the biodiesel decreased and also exhibited a clear
variation from the original values. [68] As shown in table
31
Table 4: Viscosity of biodiesel
Sample Viscosity Value(s) at 400 C (mPa.s)

Before reaction After reaction
Sunflower 29.4 3.48
Soybean 29.3 3.50
Waste cooking oil 37 3.85
2.10.3 Time
Generation of biodiesel from the various oil samples at different reaction
time.
Figure 14: Biodiesel production by varying time
Glycerol began to separate in 15 minutes after the trials were completed in this
experiment. From 15 minutes onwards, biodiesel yield increases with reaction
time, peaked at 90 minutes, and then stayed essentially steady as reaction time
32
increased. [69] In (90-150) minutes interval the yield starts decreasing.
Hydrolysis of esters starts at higher reaction time this favors soap formation 60
minutes was chosen as the best reaction time due to the economics involved. [70]
2.10.4 Temperature
Investigation of biodiesel yield at (30-70)°C range.
Figure 15: Biodiesel yield by varying temperature [71]

At 60°C, substantial amount of biodiesel yield was obtained. The product yield
began to drop when the temperature was raised above 60 °C for all of the oil
samples utilized in the study; this is due to the fact that high temperature speedup
the saponification [71]. Moreover, despite the employment of a reflux condenser
to prevent methanol to waste, Bubbles formation occurs at 65°C, which hinders
the process [72].
33
2.11 Parameters (For heterogeneous catalyst)
2.11.1 Catalyst
Investigation of the effect on biodiesel yield at catalyst (KOH) concentrations
ranged from 5 to 20 g per 100 g of oil. [66]
Figure 16: Biodiesel yield as a function of catalyst amount utilized [12]

At 5g, the yield was low (75%) and that as concentration of catalyst was
increased, the yield improved. [73]. At a catalyst quantity of 20g, the yield was
greater (96%) and (95.5%) were obtained for the 5% catalyst and 10% catalyst.
As concentration of catalyst increase maximum yield of biodiesel achieved in a
less time from the standpoint of reaction kinetics. [74] However, as the
concentration of catalyst was exceeds 15g, viscosity of reactants increases, posing
a mixing challenge and necessitating higher power usage for sufficient stirring
(bench scale at 600 rpm). [75] Because of these factors, the optimum catalyst
quantity in this system was determined to be 15 g per 100 g of oil, which was
sufficient for catalyzing the transesterification reaction. [76] A catalyst loading of
more than 15% wt/wt resulted in a decrease in oil conversion, resulting in a
maximum methyl ester yield of 94%.
34
2.11.2 Methanol to oil ratio
Investigation of biodiesel yield at different concentration of methanol to oil ratio.
Figure 17: Effect of methanol to oil ratio on biodiesel yield [14]

The results show that at 5% catalyst and 10% catalyst and at (15:1) gives high
yield (96% and 97%). [54] After that, at a methanol to oil ratio of 20:1, no
substantial increase in methyl output was found. For ash formed catalyst, (15:1)
was likewise shown to be optimal [77]. However, it has been noted that using
more methanol to push the forward process is limited due to increase in the active
sites by methanol catalyst. [78] Furthermore, adding high concentration making
glycerol difficult to get; the co-product form of biodiesel is extremely soluble in
alcohol, reversing the process [14].
35
2.11.3 Reaction time
Investigation of biodiesel yield at different reaction time ranges from 2 to 24 hours.
Figure 18: Biodiesel yield at varying reaction time [13]

As can be observed in Figure, the biodiesel yield for the 5 percent KNO3/FA
climbed to above 80 percent in the first 2 hours and then stayed reasonably stable
at 78%. [79] The yields were around 82 and 87 percent at reaction durations of 5
and 8 hours, respectively, whereas the yield rose from 2 to 5 hours for the 10%
KNO3/FA catalyst, with a maximum yield of 87.5 percent at 5 hours. Following
then, there was a drop in yield, which remained practically constant below 70%
from 12 hours onwards. [53] These data reveal that with 10% KNO3/FA and a
reaction temperature of 160°C, the reaction equilibrium was attained after 5
hours. The study found that a reaction time of more than 8 hours had a
detrimental impact on oil conversion. [80] However, it was discovered in this
36
study that utilizing class F-AFA based catalysts with a lesser reaction time of 5
hours could improve transesterification processes [13].
2.11.4 Reaction temperature
Investigation of biodiesel yield at different temperatures.
Figure 19: Biodiesel yield by varying temperature [12]

The results shown in Figure, show that as the reaction temperature increased, the reaction
speed increased as well, gives high yields (94% and 89%) at 160°C for the 10 % catalyst
and 5 % catalyst. [81] However, at 200 °C, yields (95.2 wt% and 90%) were obtained. It
also demonstrates that when the amount of oil converted increases, the temperature rises.
When the temperature was raised, the methyl ester output of fly ash increased steadily and
somewhat. [82] This could be due to the presence of metal oxides in the fly ash material,
such as CaO and Fe2O3 (XRF analysis) [12]. According to research using Fe2O3 as a
catalyst on Al2O3, the metal oxide is capable of commencing transesterification, albeit
higher temperatures (210-280°C) were required to achieve ester yields of > 95 percent [11].
When feedstock is heated at 260°C, unsaturated fatty acids are degraded, resulting in the
37
creation of unwanted polymeric compounds. As a result of this research, at 160°C necessary
to generate high yields of biodiesel employing an AFA catalyst is deemed to be pretty
acceptable. [83]
Chapter 3
3 Materials and Methods
The materials which are used in this purpose for the production of biodiesel are as follow:
• Oil (Lychee seed oil and Canola oil)

• Methanol
• Catalyst (Potassium hydroxide)
• Spanish
• Potato
• Ethyl Alcohol
• Phenolphthalein
3.1 Production of biodiesel using homogenous catalyst (KOH)

The Transesterification process is perform by lychee seed oil using homogenous catalyst
and the operating conditions are as given below:
 Taking 100g oil, 30g methanol and 1g KOH

 The operating parameters are:
 Methanol to oil ratio = 7.2: 1
 Catalyst concentration = 1% w/w
 Time = 1h 40min
 Stirring speed = 1000 rpm
38
Figure 20: Transesterification process
3.1.1 Defects in reaction

 During the washing and separation process some precipitates are also formed in the
biodiesel
 After examine the product output the conclusion is made that the FFA value of lychee oil
is greater than 2 (>2).
3.1.2 Titration process

 To check out FFA value titration process is performed
 Make a solution of 10g oil with 1ml phenolphthalein and 50ml ethyl alcohol at
temperature of 60ºC and titrate it with 0.1N solution of KOH
56.1× N × V
 The formula used for acid value is A.V = = 6.17
W
A .V
 The FFA value is obtained by = = 3.085 (which is >2)
2
3.1.3 Esterification process

 To reduce the FFA value of oil esterification process is performed by raw materials
quantity as
 Amount of methanol = FFA × 3.3 = 10g
 Amount of sulphuric acid = 35% FFA = 1g
 Amount of oil = 100g
 By performing titration process again, the FFA value was = 2.325 (which is still >2)
But the required value of FFA was still high so once again esterification process was
performed that the value falls in required range
39
3.1.4 Second time esterification process performed
 Take 50g of lychee oil
 Take 0.75g of sulphuric acid which is 1.5% wt of oil
 Take 12.5g methanol which in ratio form is 6:1
 Heat the solution on hot plate for the temperature upto 60ºC for 1hr
 Wash the solution with distilled water having same 60ºC temperature.
3.1.5 Perform second titration process

 Make a solution of 10g oil with 1ml phenolphthalein and 50ml ethyl alcohol at
temperature of 60ºC and titrate it with 0.1N solution of KOH
56.1× N × V
 The formula used for acid value is A.V = = 1.0098
W
A .V
 The FFA value is obtained by = = 0.5049 (which is <2)
2
3.1.6 Perform transesterification process

Take 30g of lychee seed oil and heat on hot plate up to the temperature 60 ºC. Further
parameters are given below:
Table 5: Operating parameters for biodiesel using homogeneous catalyst
Operating parameters Quantity Units
Methanol to oil ratio 6:1 -
Temperature 65 ºC
Stirring speed 1000 Rpm
Time 2 hrs
Catalyst concentration 1% wt
40
Figure 21 : Flow diagram of transesterification process
Figure 22: Biodiesel from homogeneous catalyst
3.2 Production of biodiesel using heterogeneous catalyst (spinach)
3.2.1 Extraction of KOH from spinach

Following are the steps followed in preparation heterogeneous catalyst:
 Wash them with distilled water (3 times)
 Dried them in direct sunlight
41
 Then dried them under heat bulbs for 48 hours
 Perform calcination at 600ºC for 2 hours
 Make a solution with distilled water at 60 ºC temperature
 Filter the solution using filter paper
 Boiled the remaining filtrate
 Collect the potassium hydroxide form the beaker which is used as catalyst
Figure 23: Calcination of spinach

Take 30g of canola oil and heat on hot plate up to the temperature 60 ºC. Further
Table 6: Operating parameters for biodiesel using heterogeneous catalyst
Methanol to oil ratio 9:1 to 15:1 -
Temperature 65 ºC
Time 2 to 3 hrs
Catalyst concentration 2 to 5% wt
42
3.3 Production of biodiesel using heterogeneous catalyst (Potato)
3.3.1 Extraction of KOH from Potato
Following are the steps followed in preparation heterogeneous catalyst:
 Wash them with distilled water (3 times)
 Dried them in direct sunlight
 Then dried them under heat bulbs for 48 hours
 Perform calcination at 600ºC for 2 hours
 Make a solution with distilled water at 60 ºC temperature
 Filter the solution using filter paper
 Boiled the remaining filtrate
 Collect the potassium hydroxide form the beaker which is used as catalyst
Figure 24: Calcination of potatoes

Take 30g of canola oil and heat on hot plate up to the temperature 60 ºC. Further
Table 7: Operating parameters for biodiesel using heterogeneous catalyst
Methanol to oil ratio 15:1 -
43
Temperature 65 ºC
Time 2 to 3 Hrs
Catalyst concentration 2% Wt
Chapter 4
4 Results and Discussion
When calcination was done on heater.

4.1 Results of biodiesel produced from homogeneous catalyst (KOH)
Thermo-physical properties of the biodiesel are as follow:
 Density
The density is calculated by the following procedure:
Mass of flask = 27.98g
Mass of water = 31.5 – 27.98 g

= 3.52g
Mass of oil = 2.8 g
Time for water = 19.39s
Time for oil = 228s
Density of water = 0.998g/cm3
44
Massof oil
Formula = × dw
Mass of water
0.0028 kg
= × 997 kg /m3
0.00352 kg
= 862.5kg/m3
 Viscosity
The viscosity is calculated by the following procedure:
Time for water = 26s
Time for oil = 295s
Density of water = 0.998g/cm 3

Viscosity of water = 1.1692mm2 / s
t×d
Formula = ×ƞw
tw × dw
= 11.46mm2 / s
 Fourier-transform infrared spectroscopy (FTIR Test)
45
Figure 25: FTIR Test graph
Discussion
The yield obtained from doing the process of transesterification of biodiesel from
homogeneous catalyst is about 85%. This yield can be improved by changing the
operating parameters and examining what the effect cause on the yield as we can change
different parameters like
1. Methanol to oil ratio
2. Catalyst concentration
3. Reaction temperature
4. Reaction time
By changing these parameters, the yield of the biodiesel can be easily enhance.
4.2 Results of biodiesel produced from heterogeneous catalyst (Spinach)

 Density

46
Mass of water = 27.38 – 24.43 g

= 2.95g
Mass of oil = 2.78 g
Time for oil = 734s
Density of water = 0.998g/m3
Massof oil
Formula = × dw
Mass of water
2.78 g
= ×0.998 g/m3
2.95 g
= 0.9404g/m3
 Viscosity:
Time for oil = 734s

t×d
Formula = ×ƞw
tw × dw
= 0.464 poise
As we know that,
1 poise = 0.1 pas.s
so,
0.464 poise = 0.0464 pas.s
47
Dynamic viscosity = 0.0464 pas.s
Dynamic viscosity
Kinematic viscosity =
Density of oil
= 0.049734 mm2 / s
Figure 26: FTIR Test graph
Discussion:
heterogeneous catalyst is about 89.5%. This yield can be improved by changing the
48
4. Reaction time
By changing these parameters, the yield of the biodiesel can be easily enhance.
4.3 Results of biodiesel produced from heterogeneous catalyst (Potato)

 Density
Mass of water = 27.38 – 24.43 g

= 2.95g
Mass of oil = 3.17 g
Time for oil = 462s
Massof oil
Formula = × dw
Mass of water
3.17 g 3
= ×0.998 g/m
2.95 g
= 1.0724g/m3
 Viscosity:
Time for oil = 734s
49
t×d
Formula = ×ƞw
tw × dw
= 0.33360 poise
As we know that,
1 poise = 0.1 pas.s
so,
0.464 poise = 0.033360 pas.s
Dynamic viscosity = 0.033360 pas.s
Dynamic viscosity
Kinematic viscosity =
Density of oil
= 0.031107 mm2 / s
Figure 27:FTIR Test graph
Discussion
50
heterogeneous catalyst is about 93.3%. This yield can be improved by changing the
4. Reaction time
By changing these parameters the yield of the biodiesel can be easily enhance.
Table 8: Comparison of biodiesel with standard
Parameters ASTM Standard Biodiesel Biodiesel

Biodiesel Potato origin (Spinach origin
catalyst) catalyst)
Density (g/m3) 0.86-0.90 1.0724 0.94
Viscosity (mm2 /s) 1.9-6.0 0.03 0.05
Chapter 5
51
5 Further Results
5.1 Maximizing the yield
Without optimization we get 93.3% yield from potato origin catalyst and 89.5% yield from
spinach origin catalyst.
We can get above 95% yield by optimization using RSM technique.
5.2 Calcination of potato and spinach by using electric furnace
 First we will crushing the dried potato and spinach into small partials
 Place in the electric furnace for calcination at the same operating parameters that
used in electric heater
 Then we will compare the results
5.3 Electricity consumption
When electric heater used for calcination
Table 9: Electricity consumption
Appliance Specification Total Time Electricity Units

consumed
Electric Heater 1500W 4hours 6
Electric Bulb for 300W --- 1bulb 6hours 11
drying 1800W---- 6 bulb
Total electricity consumed = 17 units
52
Chapter 6
6 Conclusions and Future Work
6.1 Optimization of biodiesel
One of the most important tasks in the biodiesel manufacturing process is to

optimize process variables and conditions in order to get maximum output.
Traditional approach (one element at a time) has been thoroughly explored, but it
has certain drawbacks, such as more experimental runs, time, and a lack of
illumination of the variables. [84] RSM is becoming more popular in optimization
studies since it delivers more information about the effect of selected Parameters
with less experiments. The experimental settings for optimizing biodiesel yield
were designed using Design-Expert software 8.0.6. [36]
6.1.1 Response surface methodology (RSM)

RSM (Response Surface Methodology) is a statistical method that may be used to
design, optimize, and analyze trials in any process.
Figure 28: Working of RSM [12]
The central composite design (CCD) and the Box-Behnken design (BBD) are two
types of designs used in RSM. [85] CCD is an effective and extensively utilized
53
for process optimization that has been reported in the literature. In CCD, the
parameters are set at 5 columns (+a, +1, 0, -1, -a) whereas, in BBD, the
parameters are set at 3 columns (+1, 0, 1). The results of the tests were analyzed
and interpreted using Design-Expert 8.0.6 (StatEase, Minnesota, MN, and USA).
[86] Regression analysis, charting of the response surface, and analysis of
variance are the three basic analytical procedures necessary to generate optimal
conditions (ANOVA). Biodiesel was manufactured at a pilot scale utilizing the
optimized parameters for the engine performance test after the yield was
optimized. [87] An electrical homogenizer was used to create biodiesel blends.
This homogenizer was operated at 1500 rpm for 20 minutes to combine HSD with
various amounts of biodiesel. B10, B20, B30, B40, and B50 were created on a
volume basis, with the biodiesel content defined by numbers in the blend name.
[88]
6.2 Tribological behavior

To analyze the tribological behavior of the biodiesel.
6.3 Exhaust emission
To check and analyze the exhaust emissions from engine when biodiesel is used.
6.4 Engine testing
Checking out the different aspects of the produced biodiesel by doing engine testing.
6.5 Acoustic behavior
To check out the acoustic behavior of produced biodiesel.
54
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Identification of novel heterogeneous catalysts for the extraction of

potassium hydroxide (KOH) for biodiesel production

Department of Mechanical Engineering,

A thesis submitted in partial fulfilment of the requirements of the

Registration NumberNumber Student Namedent Name

Figure 1: Consumption of sources in 2020................................................................................10

1.1 Quickly reduction of fossil fuels

Figure 1: Consumption of sources in 2020

Figure 2: Harmful effect of fossils fuels

1.3 Biodiesel the best alternative source

1.4 Aim and Objectives

Aim of the Project

2.1.1 Rudolph Diesel discovery

2.1.2 Henry Ford thoughts on biodiesel

2.1.4 The international biofuels forum

2.1.5 Development in South African region

2.1.6 Sustainable development commission (SDC) report

2.1.7 How South Africa overcome their problems?

Figure 2 Biodiesel consumption [17].

2.1.8 Expedito Parente making biofuel

2.2 Feedstocks used for biodiesel making

2.2.1 Availability and classification of biodiesel

Figure 6: The oil proportion of feedstocks for biofuels [30]

2.3 Processes for the making of biodiesel

2.3.1 Direct blending

2.3.2 Thermal cracking (Pyrolysis)

Figure 7:Thermal cracking process [35].

2.3.3 Micro emulsion process

Figure 8:Reaction of transesterification process [42].

Figure 9:Schematic diagram of transesterification process [36]

2.4 Base catalyst transesterification process

2.5 Acid catalyst transesterification process

2.5.1 Significance of transesterification process

2.6 Experimental procedure

2.7 Selection of alcohols

2.9 Efficiency of acid catalyzed reaction

2.9.1 Difficulties in acid catalyzed reaction

2.9.2 Agricultural wastes used as catalysts

Waste Preparation Catalyst Oil Reaction Yield References

Wild Calcination at 800 greater % of Used 7, 3, 190, 63 98 [57]

Table 3: Reaction parameters and yield

Parameters Biodiesel Production

Catalyst(%wt/wt) Temperature(°C) Time(min) Sunflower Soybean Waste

Sample Viscosity Value(s) at 400 C (mPa.s)

Figure 14: Biodiesel production by varying time

Figure 15: Biodiesel yield by varying temperature [71]

Figure 16: Biodiesel yield as a function of catalyst amount utilized [12]

Figure 17: Effect of methanol to oil ratio on biodiesel yield [14]

Figure 18: Biodiesel yield at varying reaction time [13]

Figure 19: Biodiesel yield by varying temperature [12]

• Oil (Lychee seed oil and Canola oil)

3.1 Production of biodiesel using homogenous catalyst (KOH)

 Taking 100g oil, 30g methanol and 1g KOH

3.1.1 Defects in reaction

3.1.2 Titration process

3.1.3 Esterification process

3.1.5 Perform second titration process

3.1.6 Perform transesterification process