Introduction

The increasing industrialization and motorization of the world has led to a steep rise for the
demand of petroleum-based fuels. Petroleum-based fuels are obtained from limited reserves.
These finite reserves are highly concentrated in certain regions of the world. Therefore, those
countries not having these resources are facing energy and foreign exchange crisis, mainly
due to the import of crude petroleum. Hence, it is necessary to look for alternative fuels
which can be produced from resources available locally within the country, such as alcohol
and vegetable oils. Because of the global warming and depletion of fossil fuels, in recent
years, intensive investigations are carried on for providing the greater use of sustainable
biofuels instead of fossil fuels. Biomass, which various biofuels are produced from, has an
important role among other alternative energy sources including wind energy, solar energy,
geothermal energy, etc

This project reviews the production, characterization and current statuses of vegetable oil and
biodiesel as well as the experimental research work on the production

Biodiesel is one of the important biofuels and a clean energy source as an alternative to
petroleum-based diesel fuels. Biodiesel has some advantages and disadvantages.
Transportability, high combustion efficiency, low sulphur and aromatic content, high cetane
number and biodegradability are advantages of the biodiesel. Disadvantages of biodiesel are
high viscosity, lower energy content, high cloud and pour point, high nitrogen oxide
emission, lower engine speed and power, injector cooking, high price and engine erosion.

The flash point of biodiesel is higher than diesel fuel. This feature is important for fuel
storage and transportation in the way of safety. Cetane number of biodiesel (~50) is higher
than diesel fuel. Biodiesel does not include aromatic and sulphur content and contains oxygen
at the rate of 10-11% by mass. Cetane number is an important factor to determine the quality
of diesel fuel, especially ignition quality of diesel fuel. In other words, it determines the
ignition tendency of fuel when being injected into engine. Ignition quality of biodiesel is
determined by the structure of methyl ester. Viscosity is also an important factor for
biodiesel. Viscosity affects mostly fuel injection equipment and the increase of fuel viscosity
changes the viscosity at low temperatures. High viscosity has a negative effect on fuel spray
atomization.
Biodiesel has more polar structure than diesel fuel because of the oxygen, which is an
electronegative element present in its structure, and therefore biodiesel has higher viscosity
comparing with diesel fuel. In addition, elemental oxygen content is responsible for lower
heating value of biodiesel when compared with diesel fuel. Biodiesel can be used in its pure
form or when mixed with diesel fuel in certain proportions. Most common biodiesel blends
are B2 (2 % biodiesel, 98 % diesel), B5 (5 % biodiesel, 95% diesel), B20 (20 % biodiesel, 80
% diesel).

Vegetable Oils

Vegetable oils are candidates as alternative fuels for diesel engines with their high heat content . But,
direct use of vegetable oils is not possible because of the high kinematics viscosity of them which are
varies in the range of 30–40 at 38 °C and are about 10 times higher than of diesel fuel (Grade No. 2D)
leads to many problems .Therefore, modification of vegetable oil is necessary and the valuable
product of this modification is named ‘‘biodiesel’’. The edible vegetable oils such as soybean,
sunflower, palm , cottonseed, canola and olive oils have been widely used in enzymatic trans
esterification. In developed countries, edible oils constitute more than 95% of biodiesel production
feedstock because the produced biodiesel from these oils have properties very similar to petroleum-
based diesel. Also, the country and its climate, the oil percentage and the yield per hectare are
effective parameters in selecting the potential renewable feedstock of fuel

Shea butter.
Shea butter is obtained from the shea tree, Butyrospermum parkii (G. Don) Kotschy . Atta

(1978) reported that Butyrospermum parkii has three main varieties namely,

Mangifolium, poissoni and niloticum. it furthers reported that only one variety, poissoni,

occurs in Ghana. The shea tree grows spontaneously in the wooded savannah areas of

West Africa namely Ghana, Mali and Burkina Faso.The tree is stout, can grow up to 20

metres high and its trunk can reach one metre in diameter, bearing leathery oval leaves

(http://www.sheabutter.com, 2001). It produces its first fruit when it is about 25 years old

and reaches its full production at the age of 40 or 50 years. Shea butter is obtained from the
 nuts of the tree and it is also called or African butter. It is high in triglycerides and has

5% fatty acids, 8% unsaponifiables,

and 7% waxy esters. The edible fruit contains one to three seeds surrounded by a thin
brittle hull. The kernels are about 50% shea butter. One tree produces 15 to 20 kg of fresh

fruit, which corresponds to 3 to 4 kg kernels and 4 kg of kernels makes 1 kg of shea butter.

Shea Butter Quality for Consumption and Industrial Use

The fundamental composition determined by identity characteristics such as iodine

value, saponification value and refractive index does not change with the method of

extraction of the fat, i.e. Whether by screw press, solvent extraction or by the traditional

method provided the same species of plant material is used. The quality characteristics

however, may change due to the method of processing. Among the quality

characteristics, the most important for consideration from the point of view of human

consumption and industrial use are;

i. Colour

ii. Free fatty acid

iii. Peroxide value

iv. Impurities

The traditionally manufactured fat exhibit some amount of plasticity since it has fairly high

levels of moisture (1%) with which it forms an emulsion. Table 2 presented below
shows a comparison of quality characteristics of a traditionally manufactured shea butter

and laboratory screw press samples

A Comparison of the Quality Characteristics of Traditionally

Produced and Laboratory Screw Pressed Sample of Shea Butter

Quality characteristics Traditional Laboratory

25 different samples 10 samples
Impurities 1.20 – 3.49 0.0 – 0.02
(IUPAC, 1964)

Peroxide value 2.15– 7.0 0.6 – 1.0

Acid (oleic)

Colours (subjective) dirty greyish pure white and attractive

when fat solidifies colour when fat solidifies

Source: Adomako (1982)

From the point of view of edibility the laboratory screw press sample present an ideal

quality of virgin oil. The free fatty acid content is low, indicating minimum lipolitic

activity; the peroxide value is low also indicating a lower oxidation state of the fat.

The level of impurities is an indication of the level of contamination of the fat with

fine particles of the solids phase that is the cake. In the laboratory sample, the lower
 value is due to a good filtration process after extraction. It was observed that in the

traditional system, there is no filtration and the separation of the oil phase from the non

fatty phase is by skimming or decantation. Though the colour difference between the two

samples was assessed subjectively, the poor colour of the traditionally processed sample

is an indication of poor quality. The dark greyish colour may be

associated with both impurities and wash water. This state renders the fat unattractive for

purposes of human consumption.

Characteristics of Shea Butter

Shea fat is obtained from the kernels of the shea tree, Butyrospermum parkii and

Vitellaria paradoxa in Ghana. The tree being a member of the Sapotaceae family grows

well in West and Central Africa (Salunkhe and Desai, 1986; Atta, 1978). The fat,

estimated to form 40-55% of the kernel has the characteristics and fatty acid composition

as indicated in Tables 3 and 4 below (Tano-Debrah and Ohta, 1994; Salunkhe and Desai,

1986).

Product Characteristics of Shea Butter

Characteristic Mean Value

Iodine Value 58.5

Saponification Value 180.4

Unsaponifiable matter 7.5

Melting range (°C) 34-36

Source: Tano-Debrah and Ohta (1994)

 Fatty Acid Composition of Shea Butter

Fatty acid Mean Value

Palmitic 3.6

Stearic 44.4

Oleic 42.4

Linoleic 5.9

Source: Salunkhe and Desai (1986)

According to the Ghana Standards Board, standards for vegetable oils and fats should

conform to the stipulated standards (Ghana Standards Board, 1970). Crude shea butter shall

be the oil obtained by expression or by solvent extraction or by traditional methods from

whole, sound and clean kernel of Butyrospermum parkii nuts. It shall be free from

admixture with other oil or fat and shall conform to the specifications as stated in Tables

Standard Specifications for Crude Shea Butter in Ghana

Index Mean value

o
Refractive index at 40 Ċ 1.4619-1.4670

Iodine value 54.0-63.0

Saponification value 289-299

Unsaponifiable matter 2-3%

Free fatty acid Not more 5%.

Source: Ghana Standards Board (1970

Physical and Chemical Properties of Shea butter

 The physical and chemical properties of crude shea butter extracted and analysed at the

Cocoa Research Institute of Ghana by Adomako (1982) had observed properties as

indicated in Table 8.

Physical and Chemical Properties of Crude Shea Butter

Characteristic Content

Ash content 3.2

Melting point 38.0-39.5°C

Slip point 36.7-37.4

Iodine number 64.2

Acid number 13.4

Free fatty acid (as oleic) 6.8%

Saponification number 179.6-190.0

Unsaponifiable matter 7.3-9.0

Fat Content 52.1%

Solidification point 26.5-30.0°C

Degree of unsaturation 0.59

Source: Adomako (1982)

Biodiesel from Shea butter

Biodiesel from shea nut oil could be carried out either through continuous or batch process.
A supply of inexpensive and sustainable biodiesel could aide in the development of the more
remote regions of Ghana. In order to design a biodiesel production facility sized to
accommodate local demand for biodiesel from shea butter, many variables must be factored
into the equation. 1. Process development,

2. Product demand,

3. Quality/availability of labor,

4. Quality of product required

5. Transportation of product
6. Processing method for oil extraction from nut production scale
7. Reaction mechanism

8. Complexity of equipment method for making shea butter from nuts

Some reasons to consider a batch process is;

1. Inexpensive, requiring less initial capital & infrastructure investment
2. Flexible, accommodates variations in feedstock type, composition, and quantity
Shea Butter was chosen as a raw material because
1.Less expensive
2. Reduce/eliminate Ghana's dependence on foreign oil
3.Create jobs within villages where shea trees are grown

AIMS AND OBJECTIVES

i. Processing Shea butter oil into biodiesel which can be used as a substitute for
conventional petro fuel.
NEEDS

1. Sustainability
2. Cheap/ inexpensive
3. Energy efficiency
4. Biodegradable and less toxic fumes (environmentally friendly)
5. Biodiesel can use in existing diesel engines without modifying the engine
6. Multi-purpose (cleaning, solvent etc.)
7. Smell, engine sound(noise), volatility
8. Foaming nature of diesel
9. It can be produced domestically and thus reduce a country’s dependence on foreign
fuel

Essential

1. Product composition should be able to enhance a higher burning rate

2. Biodegradable and less toxic fumes (environmentally friendly) toxic fumes-attaining a
green environment by reducing the rate of carbon monoxide emission. Produces
fewer particulate matter (PM10)
3. Biodiesel can use existing engines without changing- it should be compatible with the
existing engines without having to redesign new engines or modify existing engines

Desirable

1. Energy efficiency- its ability to burn the well or achieve the desired results without
wasted energy. Distance per vehicle per consumption volume
2. Smell, engine sound(noise), volatility
3. Foaming nature of diesel

Useful

4. Multi-purpose, solvent – it brings about an additional use or advantage since that is

not its main reason for production.
5. Sustainability- continues to exist for a long time without destroying the ecological
balance.
6. Affordable- inexpensive and readily accessible
 7. It can be produced domestically and thus reduce a country’s dependence on foreign
fuel

SPECIFICATIONS

Biodiesel is defined as the mono alkyl esters of long chain fatty acids derived from
vegetable oils or animal fats, for use in compression- ignition (diesel) engines. This
specification is for pure (100%) biodiesel prior to use or blending with diesel fuel.

1. Viscosity: viscosity of a fluid is the resistance of flow a fluid. Viscosity can be

expressed as dynamic viscosity and kinetic viscosity. Generally, the viscosity of a
fluid reduces as temperature rises. The viscosity of a fluid can be expressed as a
dynamic viscosity (it's measured in centipoises) and a kinematic viscosity (is
measured in centistokes)

2. Flashpoint –is the lowest temperature at which the fuel will ignite if exposed to a
flame. Limit is 130 degrees Celsius minimum. The higher the flashpoint, the higher it
ignites and the much safer it is than other petroleum products therefore, it is beneficial
to have a higher flashpoint for our product to enhance in higher and faster ignition.
(38 degrees Celsius flashpoint for petroleum products)>>>note… how safe is the
biodiesel product?
3.
Water & sediment: biodiesel and other fuels has certain amount of water present and
the amount needs to be carefully controlled. Water present in the fuel both free and
bonded can lead the formation of free fatty acids and corrosion of engines and other
fuel storage equipments. Water presence allows microbial growth and degradation
making it hydrophilic.
Appreciable amounts of sediments can block fuel filters and cause abrasive damage to
injectors and components. It can also cause oxidation.
4. Sulphated ash: it is defined as residue remaining after a biodiesel has been
carbonized (combusted) and the residue subsequently treated and heated with constant
weight. The standard is 0.02%mass. The higher the sulphated ash, leads to engine
deposits as well as filter plugging. It will therefore be beneficial to have a biofuel that
is lower than 0.02%mass to make it better. The deposited can lead to wear and tear
therefore there is the need to limit the sulphated ash in a biodiesel. (ASTM D874-07
standard test method for sulfated from lubricating oil and additives)

5. Sulphur: the effect of sulphur content on engine slender wear and deposits appears to
vary considerably in importance and depends largely on operating conditions. Fuel
sulphur can also affect emission control systems performance, and various limits on
sulphur have been imposed for environmental reasons.

6. Copper strip corrosion. This test serves as a measure of possible difficulties with
copper and brass or bronze parts of the fuel system. The presence of acids or sulphur
containing compounds can tarnish the copper strop, thus indicating the possibility for
corrosion.

Cetane: the number of combustion quality of diesel fuel during compression ignition.
Thus it is approximate equivalent of octane rating for gasoline. The number is
important is an important factor in determining the quality of the diesel.( Wikipedia)

7. Cloud point: biodiesel generally has a higher cloud point than petroleum based fuels.
To ensure trouble free operation in cold climate, the cloud point of biodiesels and its
impacts on cold flow properties should be monitored.

8. Carbon residue: the amount of carbon that is made by a chemical process such as
heating up oil. It is mainly considered to be a by-product of fuel. High amount of
carbon residue can be damaging to the environment.
 9. Acid number: the acid numbers used to quantify the amount of acid present. The acid
number should be lower than 0.5mg to prevent corrosion of automotive parts
(Wikipedia). The acid number can also be explained as potassium hydroxide in mg
consumed in neutralizing one gram of free fatty acid.

10. Free glycerin: it is a measure of the amount of glycerin remaining in the fuel. High
levels of free glycerin can cause injector deposits, as well as clogged fuel systems, and
result in the buildup of free glycerin in the bottle of storage and fuel systems.

11. Total glycerin: it is the sum of free glycerin and the glycerin portion of any unreached
or partially reacted oils or facts. Low levels of total glycerin ensure the high
conversion of the oil or fats into its mono-alkyl ester has taken place. High levels of
mono-,di-,triglycerides can cause injector deposits and may adversely affect cold
weather operation and filter plugging

The table below shows the specifications of a biodiesel regulatory body, which is
a source of reference, against which our specifications for this project are made.

Table 1.

Property ASTM Limits Unit

Method
Flash Point D93 130min Degree
Celsius
Water & Sediment D2707 0.050max % Vol
Kinematic D445 1.9-6.0 mm 2/Sec
Viscosity,40C
Sulfated Ash D874 0.020max %Mass
Sulfur D5453 0.05max %Mass
Copper Strip D130 No.3max
 Corrosion
Cetane D613 47min
Cloud Point D2500 Report Degree
Celsius
Carbon Residue D4530 0.050max %Mass
100% Sample
Acid Number D664 0.80max Mg
KOH/g
m
Free Glycerin D6584 0.020max %Mass
Total Glycerin D6584 0.240max %Mass
Phosphorous D4951 0.001max %Mass
Content
Distillation Temp, D1160 360max Degree
Atmospheric Celsius
Equivalent
Temp,90%
Recovered

To meet special operating conditions, modifications of individual limiting requirements may be agreed
upon between purchaser, seller and manufacturer.
** The carbon residue shall be run on the 100% sample.
# A considerable amount of experience exists in the US with a 20% blend of biodiesel with 80%
diesel fuel (B20).
Although biodiesel (B100) can be used, blends of over 20% biodiesel with diesel fuel should be
evaluated on a case-by-case basis until further experience is available

There are various procedures in biodiesel production. Three of such will however mentioned.
They are:

1. Pyrolysis
2. Micro-emulsification
3. Trans-esterification
 Pyrolysis
Pyrolysis refers to a chemical change caused by application of thermal energy in the
absence of air or nitrogen. The liquid fractions of the thermally decomposed vegetable oil are
likely to approach diesel fuels. The pyrolyzate has lower viscosity, flash and pour points
than diesel fuel but equivalent calorific values. The acetane number of the pyrolyzate is
lower. The pyrolysed vegetable oils contain acceptable amounts of sulphur, water and
sediment with acceptable copper corrosion values but unacceptable ash, carbon residue and
pour point.

Micro-emulsification

The formation of micro-emulsions (co-solvency) is a potential solution for reducing the

viscosity of vegetable oil. Micro-emulsions are defined as transparent, thermodynamically
stable colloidal dispersions. A micro-emulsion can be made of vegetable oils with an
ester and dispersant (co-solvent), or of vegetable oils, an alcohol and a surfactant and
acetane improver, with or without diesel fuels. Water (from aqueous ethanol) may also be
present in order to use lower-proof ethanol, thus increasing water tolerance of the micro-
emulsions.

Transesterification

The process of converting the raw vegetable oil into biodiesel, which is fatty acid alkyl
ester, is termed as transesterification. The transesterification reaction can be influenced by
several factors including molar ratio of alcohol, catalyst, presence of water, free fatty acid in
oil samples, temperature, time, purity of reactant and agitation speed. In this context, an
understanding of the factors affecting the process is very important to make economically and
environmentally biodiesel production.
To accelerate reaction rate, transesterification process is carried out in the presence of
catalysts. So, biodiesel production is made by using chemical or enzymatic catalysts.
Compared to chemical, enzymatic reaction is more attractive because of ability of make a
high quality product, simplify the separation of products, mild reaction conditions, the reuse
of the catalyst and especially environmental impact, although high conversion and reaction
rate are obtained with chemical catalysts. Lipase is important enzyme catalyst that catalyzes
esterification and trans esterification reaction to produce methyl esters (biodiesel).

There are three basic routes to biodiesel production from bio-lipids (biological oils and fats)

i. Base catalyzed transesterification of the biolipid carried out under atmospheric

pressure and at temperature of 60-70 °C,
ii. Direct acid catalyzed transesterification of the biolipid

iii. C o n v e r s i o n of the biolipid to its fatty acids and then to biodiesel

The processing steps for the most commonly used method namely base catalyzed
transesterification of the biolipid would be as follows:
i. Exact quantity of potassium hydroxide required as determined by titration is
thoroughly mixed in methanol till it dissolves completely to result in potassium
methoxide.

Transesterification, also called alcoholysis, is the displacement of alcohol from an ester

by another alcohol in a process similar to hydrolysis. Methanol is most commonly used
for the purpose since it is the cheapest alcohol available. Ethanol and higher alcohols such as
isopropanol, butanol etc. can be used for esterification. Using higher molecular weight
alcohols improves the cold flow properties of biodiesel but reduces the efficiency of
transesterification process.
Methods commonly used for producing biodiesel are Batch and Continuous processes. In
general, smaller capacity plants, in particular with variable feedstock quality justifies the use
of batch systems
Systems generally require larger capacities to justify larger staffing needs and also require
uniform feedstock quality. The Trans esterification works well when the input oil is of high
quality. However, quite often low quality oils are used as raw materials for biodiesel
preparation. In cases where FFA content of the oil is above 1%, difficulties arise due to the
formation of soap, which promotes emulsification during the water washing stage. If the
FFA content is above 2%, the process becomes unworkable.

weighting Pyrolysi trans micro

Criterion factor s esterification emulsification
maturity 0.1 5 9 5
engineerin
g 0.15 7 9 8
Cost 0.35 4 10 5
quality 0.4 10 8 6
total score 1 6.95 8.95 7.85

Out of these three processes, the trans-esterification method is chosen for this project. This is
because using the weighting factor analysis, it was detected to be matured, had good
engineering, less costly and produced a quality end product.

MATERIALS NEEDED

 Shea butter
 Potassium hydroxide/ Sodium hydroxide
 Methanol
 Phenolphthalein indicator
 Sulfuric acid

GLASS WARES

 Conical flask
 Burette
 Pipette
 Separating funnel
 Beaker

SHEA BUTTER
The oil is the basic ingredient in the production of biodiesel. The oil is extracted from
threshing and pressing of shea nut. This oil is environmentally safe, renewable source of non-
conventional energy and a promising substitute for diesel, kerosene and other fuels. The oil
burns with little or no smoke. It is not toxic. It is not inflammable.

METHANOL

The methanol is used in the process to reduce the free fatty acids and aid the
transesterification process.

SODIUM HYDROXIDE

Sodium hydroxide acts as a catalyst in the transesterification process.

DISTILLED WATER

Distilled water is used in the washing of the crude biodiesel.

METHODOLOGY

Determination of free fatty acid

● 1 ml of the oil is pipetted into a conical flask.
 ● 10 ml of isopropyl alcohol is added to the content of the conical flask to dissolve the oil
with effective mixing.
● Three drops of phenolphthalein indicator is then added
● The mixture is titrated with 0.1 M KOH solution until the endpoint is reached upon,
which the solution will turn pink and the color should persist for 30 seconds.
● The volume of KOH used was then recorded and the value obtained was used to predict
the
Free fatty acid content of the oil.

Production of Biodiesel
● the oil to be used is heated at 105 degrees c for an hour to evaporate any available water
which causes soap formation.
● 0.3 g of KOH/ NaOH was weighed and dissolved in 12 ml methanol to form the
methoxide. The methoxide is covered to prevent evaporation as the reaction between
methanol and NaOH/KOH is exothermic.
● 48 ml of the oil was then measured and heated at 650C for 30 minutes.
● Themethoxide prepared was then added to the oil to begin the trans esterification of the
oil
(esters and triglycerol molecules) with effective stirring at 400 rpm (radical pair
mechanism)
● The reaction was carried out for an hour and the trans esterified oil was then separated
from the glycerol using a separatory funnel
● Washing was then carried out to remove any residual catalyst and excess methanol
present
● the washed biodiesel (Trans esterified product) was then heated at 1100C to remove any
water that remained after separation by evaporation.
● the volume of the washed biodiesel was then taken and the yield of the process was
computed.

Summary
In the alkali catalytic methanol Trans esterification method, the catalyst (KOH or
NaOH) is dissolved into methanol; the methoxide formed is then added to the reaction
vessel containing the oil at 65 degrees Celsius. At the end of the reaction, there are two
layers formed in the reaction Vessel. The topmost layer is the desired biodiesel and the
 lower layer, the glycerol which is the by product. Washing is done for a number of
reasons
1. To remove any excess NaOH/KOH,
2. To remove any excess glycerol within the separated biodiesel