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HARAMAYA UNIVERSITY

HARAMAYA INSTITUTE OF TECHNOLOGY

DEPARTMENT OF CHEMICAL ENGINEERING

RESEARCH PROPOSAL

ON

FORMULATION OF ANTI-MICROBIAL BAR SOAP FROM ENDOD BY USING


ADDITIVES SODIUM LAURETH AND LEMON PERFUME

By Group 5 ID:NO
1. FiromsaJida 0231/11
2. Simret Eshetu 0677/11
3. Natnael Korme 0421/11
4. Haymanot Dagne 0705/11

Advisor: Mr. Abelneh T.


Co-Advisor: Getachew C.

February 2023
Haramaya, Ethiopia
Declaration
We, Group 5 members, the undersigned, declare that the final year project proposal titled
“Preparation anti microbial bar soap from endod by using additives sodium laureth and lemon
perfume” is our original work, and has not been presented anywhere in its current form, and that all
resources of materials used have been duly acknowledged with citation. And we have prepared this
proposal under the supervision of Mr. Abelneh and Mr. Getachew C. at Department of Chemical
Engineering of Haramaya Institute of Technology, Haramaya University

1. Semret Eshetu (0677/11)


2. Natnael korme (0421/11)
3. Firomsa Jida (0231/11)
4. Haymanot dagne (0705/11)

Submission Approved by:


Mr. Abelneh T. (Major Advisor)
Mr. Getachew C.(Co-Advisor)
Mr. Nimona A.(Chairperson)
Dr. Abdisa J.(Course Instructor )
Mr. Workisa B. (Department Head)

Submitted on:

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Acknowledgement
First and foremost, we would like to thanks God who helps us and being with throughout our endeavor.
Next, we would like to express our deepest gratitude to our advisor Mr. Abelneh.for his advice,
comment and support, suggestion for better compile of our project and our co-adviser Mr. Getachew
C. Last but not least, we would like to express our thanks and loves to our families for their support
and giving moral to accomplish this senior proposal.

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Table of contents
Declaration .............................................................................................................................................. i

Acknowledgement .................................................................................................................................ii

Nomenclature ........................................................................................................................................ vi

List of tables.........................................................................................................................................vii

List of figures ..................................................................................................................................... viii

Executive Summary .............................................................................................................................. ix

Chapter One ........................................................................................................................................... 1

Introduction ............................................................................................................................................ 1

1.1 Background .................................................................................................................................. 1

1.2 Statement of problem ................................................................................................................... 3

1.3 Research question ........................................................................................................................ 3

1.4 Hypothesis .................................................................................................................................... 4

1.4 Objectives .................................................................................................................................... 4

1.4.1 General objective .................................................................................................................. 4

1.4.2 Specific objectives ................................................................................................................ 4

1.5 Scope of the study ........................................................................................................................ 4

1.6 Significances of the study ............................................................................................................ 4

Chapter Two........................................................................................................................................... 6

Literature review .................................................................................................................................... 6

2.1 Overview ...................................................................................................................................... 6

2.2 World production trends of soap.................................................................................................. 6

2.3 Soap production in ethiopia ......................................................................................................... 7

2.4 Soap uses and application ............................................................................................................ 7

2.5 Soap manufacturing process ........................................................................................................ 8

2.6 Processing technology for production of soap ........................................................................... 10

2.6.1 Cold process soap making .................................................................................................. 10

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2.6.2 Melt and pour soap making method.................................................................................... 10

2.6.3 Hand milled soap making method ...................................................................................... 10

2.6.4 Hot process soap making .................................................................................................... 11

2.7 Physical and chemical properties basic raw materials used for the production of soap in tabular
form .................................................................................................................................................. 11

2.8 Endod fruit description .............................................................................................................. 11

2.8.1 Physical characteristics of phytolacca dodecandra ............................................................ 12

2.8.2 Chemical property of phytolacca dodecandra fruit ............................................................ 12

2.9 Processes descriptions on extraction of oil from endod fruit ..................................................... 13

2.9.1 Preparation for extraction ................................................................................................... 13

2.9.2 Extraction of fruit oil .......................................................................................................... 13

2.10 Factors influencing the rate of endod fruit oil extraction ........................................................ 14

2.10.1 The effects of temperature in oil extraction ...................................................................... 14

2.10.2 Effect of reaction times ..................................................................................................... 14

2.10.3 Effect of particle size ........................................................................................................ 14

Chapter Three....................................................................................................................................... 15

Materials and methodology.................................................................................................................. 15

3.1 Materials and chemicals ............................................................................................................. 15

3.1.1 Chemicals ............................................................................................................................ 15

3.1.2 Equipment ........................................................................................................................... 15

3.2 Research methods ...................................................................................................................... 16

3.2.1 Raw material preparation .................................................................................................... 16

3.2.2 Proximate analysis of endod ............................................................................................... 16

3.2.2 Extraction of endod oil procedure using hexane as a solvent ................................................. 17

3.2.3 Characterization of the extracted oil ....................................................................................... 17

Determination of ph value procedure .......................................................................................... 17

Determination of specific gravity ................................................................................................ 17

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Determination of saponification value ......................................................................................... 17

3.2.4 Formulation of highly effective ant fungal bar soap ............................................................... 18

Saponification process to produce soap ....................................................................................... 18

3.2.5 Operating conditions on the quantity and quality of the products .......................................... 19

Effects of concentration on products ........................................................................................... 19

Effects of temperature on products .............................................................................................. 20

Effects of reaction time on product .............................................................................................. 20

3.6 Quality measurement on soap produced .................................................................................... 20

3.7 Analysis methods and expected results...................................................................................... 21

3.8 Challenges and limitations ......................................................................................................... 21

Chapter Four ........................................................................................................................................ 22

Work plan and budget breakdown ....................................................................................................... 22

4.1 Work plan................................................................................................................................... 22

4.2 Budget breakdown ..................................................................................................................... 23

References ............................................................................................................................................ 24

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Nomenclature

AV Acid Value
CAGR Compound Annual Gross Rate
CFCPD Centers for Control and Prevention disease
ETB Engaged in Trade Business
MC Moisture content
SG Specific gravity
SP Saponification value
USDT United states dollar
WHO World Health Organization

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List of Tables

Table 2.1: the world’s largest exporters of soap………………………………………………………7


Table 2.2: Soap uses and their application…..………….……………………………………………..8
Table 2.3: Physical and chemical properties of raw materials……………………………………….11
Table 3.1: List of chemicals…...……………………………………………………………………..15
Table 3.2: List equipment and their function…...……………………………………………………15
Table 4.1: Activities and time schedule….………..…………………………………………………22
Table 4.1: udget breakdown……….………….……………...………………………………………23

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List of Figures
Figure2.1: Process flow diagram of soap production……………..…………………………………. 9
Figure 2.2: Phytolacca dodecndra fruit………………….……..……………………………………12
Figure 3.1: Overall process flow diagram of soap production…..…..……………………………….19

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Executive Summary
This project work will carry out with the objective of extraction of oil from Endod fruit and its
utilization to produce an anti-fungal bar soap for cleaning cloth, dishwasher, washing hand and for
having a shower, and specifically, used for attacked body parts by fungus. The formulation of this soap
will be carried out using an oil extracted from Endod fruit. This work will be started through the
preparation of the raw materials, specifically Endod fruit. Endod fruit will be collected from Hararghe
area and it will be passed the pretreatment steps such as fruit collection, cleaning, size reduction,
drying, weighing, determination of moisture content, and sieving. The pretreated fruit will be
undergoing for oil extraction using equipment called Soxhlet extractor. Normal hexane will be used as
a solvent during the extraction process. The extracted oil will be examined or characterized using the
parameters such as PH value, specific gravity, acid value, and temperature. Solvent extraction method
will employ in extracting the oil and the total percent oil yield will find which is its standard ranges
from 45 to 69.64%.The well refined oil will be used as a main ingredient for the formulation of bar
soap following the process called saponification. The parameters such as reaction time and temperature
on soap efficiency will be investigated. The pH tests reveal mildly basic properties. The color and
efficiency of the bar soap will be improved with the addition of bleaching agent which is hydrogen
peroxide, and foaming agents Sodium laurite sulfate.

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CHAPTER ONE
INTRODUCTION

1.1 Background

The word “soap” came from the Latin word “Sapo.” it is believed that the name derived from
Mount Sapo in Rome(Routh, Bhowmik et al. 1996). The first production of soap happened
around 2800BC in ancient Babylon(Warra 2013). The Babylonians combined wood ashes with
animal and plant fat, and got a substance that was effective for cleaning. "The cold process
method" is the most popular soap making process today. Some soap makers use the hot process,
which was much more significant in past centuries. Soap is the term for a salt of a fatty acid or
for a variety of cleansing and lubricating products produced from such a substance. Soap is the
combination of fatty acids and alkalis obtained by reacting various animal and vegetable fats
and oils with caustic soda or potash(Lu, Rodriguez-Garcia et al. 2018).

The soap making reaction is called saponification. Soap prepared from caustic soda is hard
while soap from caustic potash is soft. Both soaps are readily soluble in hot water. However,
they dissolve very slowly in cold water forming a turbid solution owing to slight
decomposition. The soap itself was never actually "discovered", but instead gradually evolved
from a crude mixture of alkaline and fatty acid(Shahinuzzaman, Yaakob et al. 2016).
Cleanliness is a very important thing due to the increasing number of diseases caused by
bacteria and germs. The soap and soaps industry is very essential in people's day to day life.
The soap and soap industry includes companies that are primarily engaged in manufacturing
soap, synthetic organic soaps, inorganic alkaline soaps, and crude and refined glycerin from
vegetable oils and animal fats. It is an international industry, and during the early years of 1990,
world demand for its products has increased 1 to 3 percent every year(Achaw and Danso-
Boateng 2021). It has been made for more than 2500 years and the first recorded manufacture
of soap was in 600BC by the Phoenicians. Actually, they used soap for soap medicinally but
in the nineteenth century, it began to spread in the Western world as cleaning soap. The
invasion of non-native species is one of the major drivers of environmental and socioeconomic
changes around the world. Over the past 30-50 years, non-native Prosodic species have
emerged as a major invasive plant of the arid and semi-arid lands of eastern Africa(Baes, de
Viana et al. 2002). Invasive plants are naturalized plants that produce a large number of
offspring, have the ability for long-distance dispersal, and thus have the potential to spread
over a considerable area (Richardson, Pyšek et al. 2000). Soap is a common cleansing agent

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well known to everyone. Many authors defined soap indifferent ways and regarded it as any
cleaning agent, manufactured in granules, bars, flakes, or liquid form obtained from reacting
salt of sodium or potassium of various fatty acids that are of natural origin (salt of non-volatile
fatty acids). Soap can also be said to be any water-soluble salt of fatty acids containing eight
or more carbon atoms. Several things affect the soap-making process and the quality of this
soap produced(Onyegbado, Iyagba et al. 2002).The characteristics of this soap depend on the
quality of oil, and the amounts of the caustic soda and water used to make it. The speed of the
reaction between the oil and the caustic soda is influenced by the free fatty acid content of the
oil, the heat of the components before mixing, and how vigorously the mixing is to be done.
Free fatty acid contents, vigorous mixing, and heat speed up the given soap-making process.
Soaps are produced for a variety of purposes ranging from washing, bathing, medication, etc.
The cleansing action of the soap is due to the negative ions on the hydrocarbon chain attached
to the carboxylic group of the fatty acids(Warra, Hassan et al. 2010).

The affinity of the hydrocarbon chain to oil and grease, while the carboxylic group to water is
the main reason soap is being used mostly with water for cleaning purposes. Household uses
for soaps include washing, bathing and other types of housekeeping, where soaps act as
surfactants, emulsifying oils to enable them to be carried away by water. Soap usually comes
in a solid, molded form, called a bar, based on its typical shape. The chemical composition is
different for the installation of soap, but the same mechanism, it adversely affected by hard
minerals in the water(Anglen 2005). Therefore, this study aims to provide a means to use the
most invasive. At the beginning of the second half of the twentieth century past sales exceeded
sales of soaps, soap world, where replaced in the field of laundry and household cleaning and
industrial, with the exception of templates (parallel) soaps are still used to clean the body,
which began shampoo replaced by now. The needs for producing quality soap from locally
source Phytolacca Dodecandra require the assessment of the extraction as will be
demonstrated in this study. This will provide vital information on the presence of liquid-liquid
extraction that can separate the clear juice (Saponi one) to the user. In Ethiopia, toxic plants,
berries of Phytolacca Dodecndra are being commonly used for washing clothes and to control
fresh water snails. Since the discovery of Endod in 1965, there have been extensive studies on
the chemistry, toxicity, and epidemiology of Lemma toxins, together with cultivation of the
Endod plant(Lemma, Wolde-Yohannes et al. 1991). There are many types of soaps, depending
upon the usage. There are hard and soft. Hardness of soap is often achieved through the addition

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of hardening agents, so many natural soaps tend to be softer. They are further categorized into
two. Those are; Cleansers and Soaps
Cleansers: Those are often made with mild abrasives and they are formulated to eliminate
heavy oil or solid particles and hard-to-remove stains. The cleansers come in many different
types depending on the type of abrasives they contain.
Soaps: Dish soaps are made to remove tough grease and release the solid dirt particles in the
foam that is produced by the soap.
1.2 Statement of Problem
In our country the raw material for soap production is basically imported from other countries
which is soap noodles with higher cost, even though the sanitation activity of the society in our
country is poor. Additionally, the price of soap is increasing from day to day due to the increase
in its high demand to the society. In our country, the scarcity of soap is a chronic problem and
also it is not easily accessible to societies. Many people in Ethiopia specifically in the rural
areas, are inhabited with low-income and cannot afford soap, instead many of them are
intending to use Endod for cleaning purpose. This in turn makes the societies vulnerable to
diseases like, diarrhea and cholera, etc. The soap helps in improving sanitation and hygiene to
address stunting, diarrhea, and trachoma. Around 60 to 80 percent of communicable diseases
are attributed to limited access to inadequate sanitation and hygiene services.
So, to alleviate those problems we have intended to prepare antimicrobial solid soap from
domestic raw materials. This study is majorly focus on endod since it is traditionally used by
almost all Ethiopians for hygiene and sanitation purpose and used as a medicine for a skin
attacked by fungal diseases. The hot process is takes place within a few minutes to a few hours
when compared with other process and it is more suitable for laboratory or industrial
preparation, yields a more chemically pure powder; by-products and excess starting materials
are separated. So that, the oil used to formulate ant fungi bar soap will be extracted from endod
fruits using Soxhlet which is used to extract the endod juice from endod fruits and use Hexane
as a solvent.(Pednekar and Mangaonkar 2023)
1.3 Research Question
• Is it financially feasible?
• How much volume of oil can we get from endod fruit?
• Is endod fruit available everywhere?
• Is it highly effective to kill fungus?

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1.4 Hypothesis
To inform peoples of about the benefit of endod fruit through practical way, Growing the plants
in a coordinated manner, Making the fruit available in the market, Creating a source of income
and employment for many people and producing antimicrobial bar from endod.
1.4 Objectives
1.4.1 General Objective
Formulation of anti microbial bar soap from Endod (Phytolacca Dodecandra) fruit by using
additives such as sodium laureth and lemon perfume.
1.4.2 Specific Objectives
➢ To Preparation of Raw materials
➢ To extract oil from Phytolacca Dodecndra fruit by using Soxhlet extraction method
and using Hexane as a solvent.
➢ To characterize the extracted oil based on their chemical and physical properties.
➢ To formulate highly effective ant fungal bar soap by using oil extracted from endod
fruit through hot process soap making method.
➢ To study the effects of operating conditions (temperature, concentration of lye,
reaction time) on the quantity and quality of the products.
1.5 Scope of the study
Our study will extend in collection of Phytolacca dodecandra fruit from East Hararghe up to
production of Anti-fungal bar soap. The fruit will be collected, clean and we measure the initial
moisture content. Drying and grinding to appropriate size. Extraction of oil from Phytolacca
dodecandra fruit the study also further analysis the laboratory experimental work to determine
the pH value, solubility, viscosity and odor of bar soap.
1.6 Significances of the study
The aim of this project is to produce bar soap which can be highly used on the infected body
parts of that caused by fungus and other microbial, and additionally to wash cloth both in hard
and soft water with natural based soap from the Endod fruit oil. By doing so the first beneficial
are farmers who are going to prepare a farm of this plant, because raw materials suppliers for
the industries that are engaged in the production of Endod fruit-based bar soap. The soaps are
also sold for the purpose of dish washing and cleaning floors industrial use in textiles, and
commercial buildings, hospitals& clinic, and hotels, similarly railway coaches, road vehicles,
aircrafts, milk bottling plants and food preservation equipment are washed with the help of

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soaps. Used to minimize the cost of importing / import substitution soap and to introduce the
technology of extracting oil from Phytolacca dodecandra (endod).

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CHAPTER TWO
LITERATURE REVIEW
2.1 Overview
This study try to review all the information that have to include in the proposal. Those are the
production trends of soap from the world to Ethiopia and it is tried to list the benefits of soap.
This study reviews different articles that are written in this project area. In addition, it is tried
to list chemical and physical properties endod plant and also characterstics oil extracted from
this plants fruit. Generally this study review different articles and literatures which are written
on different methods of production of soaps.
2.2World production trends of soap
Worldwide sales for soap exports by country totaled US$11 billion in 2019. The global soap
market size is projected to reach USD 55.29 billion by 2027, exhibiting a CAGR of 5.0% during
the forecast period. Rapid transmission of the COVID-19 infection is set to play a central role
in fueling the growth of this market, states Fortune Business Insights in its recent report, titled
"Soap Market Size, Share & Industry Analysis, By Product Type (Bath & Body Soaps, Kitchen
Soaps, and Laundry Soap), Form (Solid and Liquid), Application (Household and
Commercial), Distribution Channel (Hypermarkets/Supermarkets, Pharmacies, Online
Channels, and Others), and Regional Forecast, 2020-2027".
According to the World Health Organization (WHO), the corona virus spreads through
respiratory droplets and physical/body contact(Nikhra 2020). Therefore, to avoid spreading the
virus through these routes, the WHO along with many other bodies such as the Centers for
Disease Control and Prevention (CDC) has recommended regular washing of hands using soap
and water. Comprehensive washing of hands kills the virus and this practice is currently seen
as the most effective way of preventing transmission among people, especially given that a
vaccine for the infection is many months away. Thus, the demand for soaps in all shapes and
forms is slated to experience a meteoric rise as the COVID-19 pandemic intensifies and
worsens during the current year(Tokiwa 1978).

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Table 2.1: the world’s largest exporters of soap(Mahagamage and Marasinghe 2023).

Rank Country Export value (millions of USD)

1 United states 558

2
German 543

Indonesia 524
3

4 Malaysia 456

5 China 367

2.3 Soap production in Ethiopia

The industrial sector of Ethiopia is small and highly import-dependent. Ethiopia's requirement
of soap is largely met through import. The average import of soaps is 57% while the domestic
production covers 43%. Data obtained from the Ethiopian Revenues and Customs Authority
on the import of soap for nine years starting from 2003 up to 2011 shows that the imported
quantity during the nine years was highly erratic, which ranges from the lowest 165.7 tons in
the year 2007 to 2,313.6 tons in the year 2006. The demand for the year 2012 for soap was
estimated to be 922 tons. According to the Central Statistical Agency on the survey of Medium
and Large Scale and Electricity Industries in 2011, 43 companies are engaged in the
Manufacture of soap and soaps, cleaning and polishing, perfumes and toilet preparations,
Manufacture of chemical products. (Nura and Debebe 2019).
2.4 Soap uses and application
Beyond its cleaning ability, soap has been used in other applications. For example, certain
soaps can be mixed with gasoline to produce gelatinous napalm, a substance that combusts
more slowly than pure gasoline when ignited or exploded in warfare. Soaps are also used in
"canned heat," a commercialized mixture of soap and alcohol that can be ignited and used to
cook foods or provide warmth(Falbe 2012).

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Table 2.2: Soap uses and their applications (Joshi, Bakshi et al. 2022)
Soap uses and their applications
Bug repellent place some liquid soap in a bowl mixed with water under a light and it
will attract fleas and they will drown
Rid your house of some liquid soap in a bowl mixed with water under a light and it will
fleas attract fleas and they will drown
Household bug mix soap and water and place in a spray bottle and spray around your
repellent home to rid your house of spiders and bugs
Drawers use soap to loosen and quiet dresser drawers or other household drawers
by running the soap along the metal rails
Freshen place a bar of soap in a mesh holder to keep stored clothes or luggage
clothes/luggage smelling fresh
Car freshener place slivers of left-over soap in a mesh bag and tie around your
rearview mirror to keep a fresh smell in your car
Removing mix soap and water and sponge on old wallpaper and it will help in
Wallpaper removing the glue
Remove a light- remove a broken light-bulb by placing a soap bar on top and then
bulb turning it
Zippers Loosen stuck or rusty zippers by sliding some bar soap up & down the
zipper
Detect gas leaks Mix a solution of water and soap and rub along pipes, if it bubbles, you
found your leak.
Lubricate Dip a screw or nail into a bar of soap before drilling or hammering and
screws/nails it will move through wood more easily/also for saw blades too.
Fabric Marker Use those little left-over’s to make fabric for hemming and it washes
right away when complete.

2.5 Soap manufacturing process


The length of the hydrocarbon chain ("n") varies with the type of fat or oil but is usually quite
long. The anionic charge on the carboxyl ate head is usually balanced by either charged
potassium (K+) or sodium (Na+) cat ions. In making soap, triglyceride in fat or oils are heated
in the presence of a strong alkali base such as’ sodium hydroxide producing three molecules of

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soap for every molecule of glycerol, the process is called saponification. The equations below
represent typical saponification reactions;(Baptista, Martins et al. 2019).

Soap is produced industrially in four basic steps: saponification, glycerin removal, soap
purification, finishing.
Saponification: a mixture of tallow (animal fat) and oil is mixed &heated with sodium
hydroxide then the soap produced is the salt of a long chain carboxylic acid.
Glycerin removal: glycerin is more valuable than soap, so most of it is removed. Some is left
in the soap to help make it soft and smooth. Soap is not very soluble in salt water whereas
glycerin is soluble; salt is added to the wet soap causing it to separate out.
Soap purification: any remaining sodium hydroxide is neutralized with a weak acid such as,
citric acid and two thirds of the remaining water is removed.
Finishing: additives such as preservatives, color and perfume are added and mixed with the
soap, and then it is shaped into bars for the market. Soaps are similar in structure and function
to soap and for most uses they are more efficient than soap. In addition to the actual 'soap'
molecule, soaps usually incorporate a variety of other ingredients that act as water softeners,
free flowing agents etc.

Saponification Glycerin removal

Finishing Soap purification

Figure2.1 Process flow diagram of soap production.

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2.6 Processing technology for production of soap

Soap is a water-soluble salt of fatty acids that contain more than eight carbon atoms. The
cleaning properties of soaps depend on their chemical properties as an anionic surface-active
agent or surfactant. A soap molecule has a long hydrocarbon chain with a carboxylic acid group
on one end, which has an ionic bond with a metal ion, usually sodium or potassium. The
hydrocarbon end is non polar, which is soluble in non-polar substances and the anionic end is
soluble in water. This ability is seen from the molecular structure of soaps, when these materials
are burnt in air, the resulting extraction of KOH from wood ash. Ashes contain oxides of
potassium and sodium that dissolve in water to give hydroxides. The glycerol which is
separated from the crude soap will be sold to lotion and cream manufacturers(Van Gerpen
2005).
There are several different soap making processes that will allow easy production of soap
products (Yahaya, Ajao et al. 2012).
• Cold process soap making
• Melt and Pour soap making method
• Hand milled soap making method
• Hot process soap making
2.6.1 Cold process soap making
This process requires a scale, a large stainless-steel pot, measuring cups, kitchen thermometers,
rubber gloves, mold, cardboard, plastic bags, olive oil, coconut oil, shortening, lye, distilled
water, and fragrances. The cold process gets its name from the general low temperatures that
are used to mill this type of soap (Letcavage 2009).
2.6.2 Melt and pour soap making method
Out of all of the soap making methods, this is perhaps the easiest for novice soap makers. It
involves simply melting a soap base in a double boiler, adding in fragrance and dyes, and then
placing the soap mixture into a mold(Browning 2002).
2.6.3 Hand milled soap making method
This method is also called soap re-batching, in which soap is made from soap scraps that can
still be reworked into a new bar of soap. To do this, soap scraps, a mold, a grater, fragrance,
dyes, and other additives are needed. The best type of soap base for this type of soap making
is a cold process soap. To start with, you will want to grate your soap into fine particles. Then
place all of your shavings into a glass bowl that can be placed in a double boiler. As the double
boiler heats up, you will need to stir your grated soap pieces. Add in your vegetable oils and

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fragrances at this point, making sure that everything is incorporated. Break up soap clumps that
form. Continue to cook until the soap reaches the string stage. At this point, the soap will
thicken rapidly. Remove the pot from the heat source quickly add in fragrances, coloring herbs,
and optional items in that order. Spoon into molds and allow it to cure (Browning 1999).
2.6.4 Hot process soap making
This process is named for its boiling pot method of soap milling. For this type of homemade
soap making, you will need oil (palm oil, coconut oil, sesame oil, shea butter, and castor oil),
potassium/sodium hydroxide, water, borax, soap molds, stainless steel pot, stirring stick or
spoon, plastic wrap(Karimah and Kristiana 2020).
2.7 Physical and chemical properties basic raw materials used for the production
of soap in tabular form

Table 2.3: physical and chemical properties of raw materials(Manji, Sarah et al. 2013).

Raw materials Chemical property Physical property


Hydrogen peroxide (H2O2) Colorless liquid, less Highly unstable, act as both
volatile and more viscous oxidizing and reducing
than water agent

Potassium hydroxide Reactive acid, highly Clear solution, white and


(KOH) corrosive and combustible granular solid, odorless

Sodium chloride (NaCl) Corrosive to base metals White in color, conduct of


electricity. Soft enough to be
Doesn’t undergo
cut with knife
combustion and chemicals
have hygroscopic quality
2.8 Endod Fruit Description
The essential oil from Phytolacca dodecandra, a traditional herb of Ethiopia, will be studied,

including the chemical composition and antimicrobial activity. The essential oils were obtained

by steam distillation. The essential oils from P. dodecandra fruit were yellowish and the

viscosity of oil is range from 0.0488 ± 0.0002pas at temperature range from 25-50(van Galen

2014).

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Figure 2.2: Phytolacca Dodecndra Fruit
2.8.1 Physical Characteristics of Phytolacca Dodecandra

Endod is a perennial plant. It is a climbing plant with hanging branches growing up to 10 m.


usually, in a year twice it used to provide fruits from December – February and then June –
July. Often, it is found in highlands of Ethiopia from 1600m-3000 m above the sea level.
General Uses Parts of the Endod plant have been used as a soap and as traditional medicine for
centuries in Ethiopia. Endod is known as traditional soap in rural Ethiopia and rids clothes of
parasites such as lice. It is also used in traditional medicine against dandruff and other skin
diseases. People of all ages are familiar with the plant and its soaps and medicinal uses. Endod
is considering being associated with poor people. Common medicinal uses include treatment
of skin itching (ringworm), abortion, gonorrhea, leeches, intestinal worms, anthrax and
rabies.(Wolde-Yohannes 1984).
2.8.2 Chemical property of Phytolacca Dodecandra Fruit
The endod plant provides material of special interest to organic chemists involved in saponin
chemistry, partly because of the high percentage by weight of crude saponins in dried berries,
and partly because of the chemical complexity of the materials. Most chemical work on ended
until now has concentrated on the saponins of dried berries (Chi and Kim 1985).
The leaves, fruit and root contain numerous saponin (triterpenoid glycosides). These compound
cause hemolysis red blood cells the aglycones of the glycosides are mainly composed of
oleanolic acid (66%), bayogenin (15%), hederagenin (9%), and 2-hyderoxyoleanoic acid
(6.5%). On a dry weight basis, the fruit pulp contains 25% saponins, and the non-saponin
fraction contains a lipid fraction (palmitic acid, oleic acid, stearic acid and a non-saponifiable
bright orange, wax material), 12 sugars, starches, pectin’s and gums and a water insoluble
fraction. The saponins have become important as they have strong molluscicide activity against

12
a range of water snail. In Ethiopia different cultivars yielded between 1050kg/ha to 2750kg/ha
of dried fruit, with a saponins content of 20-25% ((Admasu, Deressa et al. 2014).
2.9 Processes Descriptions on extraction of oil from endod fruit
2.9.1 Preparation for Extraction
The Phytolacca dodecandra fruit will be collected from East Hararghe area, the pre-treatment
involves the preliminary preparations of the Phytolacca dodecandra fruits to make suitable for
extraction. The fruit will be wash with tap water and lean to remove dirty introduced during
preparation. After cleaning the fruit will grind and mill with mortal and pistol in order to
achieve size reduction and so as to increase reactivity and to homogenize for extraction
process(Yugi, Okeyo-Owour et al. 2016).
2.9.2 Extraction of Fruit Oil
Extraction is the withdrawing of an active agent or a waste substance from a solid or liquid
mixture with liquid solvent. The solvent is not or only partial miscible with the solid or the
liquid. By intensive contact the active agent transfers from the solid or liquid mixture in to the
solvent (extract). After mixing the two phases are separated which happens either by rotary
separator. For recovery of the solvent (hexane) and to get the active agent in pure form a further
separation process is necessary. Hexane is poured into the round bottom flask. Endod fruit is
placed in the thimble and inserted in the center of the Soxhlet extractor. The extractor is heated
when the solvent is boiling; the vapor rises through the vertical tube into the condenser at the
top. The liquid condensate drips into the filter paper thimble in the center which contains the
solid sample to be extracted. The extract sips through the pores of the thimble and fills the
siphon tube where it flows back down into the round bottom flask. This is allowing for 4 hours
the output from Soxhlet is mixture of oil and solvent, hexane this mixture cool for few minutes
and inter to the rotary evaporator to recover solvent that is hexane the temperature in the rotary
evaporator is the boiling point temperature of solvent(hexane). After the required oil was
obtained from the recovery process the viscosity, free fatty acid specific gravity and density of
oil was identified. The desired yield on this experiment (Soxhlet extraction) is free fatty acid
oil(Anastassiades, Lehotay et al. 2003).
Process selection
Selection of hot process over cold process
There are two types of soap. Those are soft soap and hard soap. Soft soap can be made using
either a cold process or a hot process, but hard soap can only be made using a hot process. Soap
is completely saponified quicker than in Cold Process soap. Essential and fragrance oils, super

13
fatting oils, and other additives are added at the end of the cook and are not affected by the
saponification reaction. Hot Process soaps are easier to slice and do not crumble.
The cold process may require several days or even months, depending upon the strength and
purity of the ingredients, whereas the hot process takes place within a few minutes to a few
hours. The hot process, more suitable for laboratory or industrial preparation, yields a more
chemically pure powder; by-products and excess starting materials are separated (Partovi
2007).
2.10 Factors influencing the rate of Endod fruit oil extraction
The factors which affect the laboratory extraction of endod fruit thus leading to variations in
oil yield and composition, includes; moisture,contents, samples, particle size, temperature,
reaction time, solvent type and solvent to sample ratio. The parameters are discussed in this
paper as follows:
2.10.1 The effects of temperature in oil extraction
Temperature is increased for fruit oil after pre-treatments such as cleaning, grinding and milling
by drying, sieving and milling again the over -size of endod fruit prior to extraction and is
termed thermal treatment of fruit oil. Better extraction is achieved by heating, which reduces
the oil viscosity and releases oil from intact cells, and also reduces moisture in the cells.
Temperature plays an active role in the fruit treatment for mechanical extraction and ensures
an effective solvent process by heating the solvent which hastens the extraction process. At the
right temperature and moisture content, the individual oil droplets unite to form a continuous
phase and flow out maximizing oil yield(Merga, Daba et al. 2021).
2.10.2 Effect of reaction times
Oil yield obtained (expressed in percent) is extraction time dependent. In general, the oil yield
increases with increase in extraction time. But after a time the amount of oil would be lower
and constant oil yield would be obtained(Shorstkii, Khudyakov et al. 2020).
2.10.3 Effect of particle size
Particle size plays a great role on the yield of endod fruit oil. Medium particle size gives high
yield while samples with large particle size and very smaller particle size deliver low yield.
That means less oil is extracted from the larger particles compared to the medium size of the
particles(Agu, Orakwue et al. 2022)

14
CHAPTER THREE
MATERIALS AND METHODOLOGY
3.1 Materials and Chemicals
3.1.1 Chemicals
Table 3.1: list of chemicals
Chemicals Functions
Sodium hydroxide 20% (NaOH) Used for saponification process
Sodium chloride (NaCl) Used to increase the brightness of the product and
change the product to semi solid
Hydrogen peroxide (H2O2) Used us bleaching agent
Water Used for dilute the ingredients and act as the reaction
media
Hexane 10.5% (C6H16) Used as solvent
Sodium laureates 1% Used as foaming agent

3.1.2 Equipment
Table 3.2: list equipment and their function
Equipment’s function
Test tubes Use to measure the liquid ingredients
Soxhlet Used to extract the endod juice from
endod fruits.
Beakers To mix the ingredients
Rotary evaporator Used to separate the solvent from the
produced oil
Stand To carry the stirrer motor
PH meter To identify the pH of the product weather
it is acidic or basic
Measuring cylinder To prepare solution of potassium
hydroxide and to read the volume
Mixer Used for mixing the ingredients
Thermometer For measuring the temperature of reaction
Heater or Bunsen burner To heat the solution or for saponification
reaction

15
Analytical balance Measure the required amount of
ingredients

3.2 Research methods


3.2.1 Raw Material Preparation

✓ Phytolacca dodecandra fruit collection: the samples of Phytolacca dodecandra fruit


will be obtained from east Hararghe area.
✓ Cleaning: the fruit will be separated from the chaffs and other impurities. This
Preparation is very important since any impurity in the fruit will eventually reflect on
the oil extracted.
✓ Size Reduction: milling and grinding the endod fruit using mortal and pistol to provide
a greater surface area to facilitate the extraction process.
✓ Drying: after grinding and milling the Phytolacca dodecandra fruit thoroughly; they
will be dry in sun light for 8:00 hour to reduce the moisture content of the fruit.
✓ Weighing: These will be done before and after the crushed fruit dried. The weight will
take and recorded using electronic weighing balance. The methodology that going to
use for this project experimentation the experiment extraction of oil from endod fruit
will be carried out in laboratory of Haramaya University department of chemical
engineering.
3.2.2 Proximate analysis of endod

✓ Determination of moisture content of the seeds: 2250g of the wet sample will be
weighed and dried in sun light for 8:00 hour and the Weight will be measured. Then
the moisture content will be obtained. The Percentage moisture in the dried fruit will
be calculated using the following:
MC% = (M1-M2) / (M1) * 100…………………………………………..……. (3.1)
Moisture content (%) = (Initial mass of sample – dried sample mass) / (Initial sample
mass) * 100 Moisture content (%) = (2250 - 1621) / (2250) * 100 = 27.9%
✓ Size reduction and sieve analysis of the fruit powder
The sample will vibrate shaker with set of sieves sizes arranged in decreasing order
4mm, 3mm, 2mm, 1mm and 0.5mm. This is because to Investigate the effect of particles
size on yield oil. But it is not advisable to use very small size sieve, because it affects
the produced oil quality, the oil became residue and black in color. To produce anti-
microbial bar soap, we follow two experiments.

16
✓ Ash content:The crucible will be weighed and recorded. The recorded value will be
weighed to 4 decimal places.Weigh approximately 2 g into crucible.Record weight to
4 decimal places.Ash sample at 600oC for 2 h. (Bring temperature rapidly to 600)Cool
in desiccator and weigh within 1 h after reaching room temperature.Weighed ashed
sample and recorded weighted to 4 decimal places. % Ash will be calculated and
recorded with one decimal.
% ASH = ((ashed wt.) - (crucible wt.)) x 100/((crucible and sample wt.) - (crucible wt.))
The first experiment is extraction of Endod oil from Phytolacca dodecandra fruit and
The second is saponification of Endod oil to produce anti-fungi bar soap.
3.2.3 Extraction of Endod Oil Procedure Using Hexane as a Solvent

240ml of normal hexane will be poured into round bottom flask, the proportionality of Endod
fruit to hexane is 1:3. 80g of the sample will be in the thimble and insert in the center of the
extractor. the Soxhlet wiil be at 69oC. While the solvent boiling, the vapor rises through the
vertical tube into the condenser at the top. The liquid condensate drips into the filter paper
thimble in the center, which contains the solid sample to be extracted. The extract seeps through
the pores of the thimble and fills the siphon tube, where it flows back down into the round
bottom flask. This will be allowed to continue for 4 hours. The extract will then removed from
the tube. Further extraction will be carried out repeatedly until the required amount of oil is
obtained. At the end of the extraction, the resulting mixture containing the oil will be heated to
recover solvent from the oil.
3.2.3 Characterization of the extracted oil

Determination of PH value Procedure


23g of the sample will be poured into a clean dry 25ml beaker. The pH electrode will be with
buffer solution and immerse the electrode into the sample and read pH and record the pH
value of the oil it should be 6.19.
Determination of Specific Gravity
Specific gravity will be determined by measuring the density of oil by using density balance
equipment, after density of oil obtained, it is possible to deteemine the density of oil by using
the following formula, calculate the specific gravity of the oil.
S G = Density of oil /Density of water………………………………………. (3.2)
Determination of Saponification Value
2g of the oil will be placed in a conical flask which 25ml of hexanoic sodium hydroxide (0.1M)
will be added to it and allow the mixture will be boiled gently for about 60 minutes with shaking

17
at regular intervals of 5mins. Few drops of phenolphthalein indicator will be added to the warm
solution and then will be titrated with 0.5M HCL. The end point will be reached when the pink
color of the indicator just disappeared. The same procedure will be followed for the rest. The
saponification value (SV) is given by:
𝑉𝑜−𝑉𝑖)
SV = 56.11 *( 𝑁………….……………………………………………… (3.3)
𝑀

Where: Vo = volume of
HCl solution used for the blank test, vi = volume of HCl solution for the determination, N =
actual normality of HCl used, and m = mass of sample
Determination of Acid Values
6.1g of the oil will be placed in to 250ml dried conical flask followed by 25 ml of absolute
hexane and 3 drops of phenolphthalein indicator will be added in to a dried 250 ml conical
flask. the mixture will be heated in a shaking water bath for 5 minutes. Titrate, the mixture
against 0.1N NaOH until pink color appears. Vigorous shaking will be done when
approaching the end point to ensure thorough mixing. The volume of 0.1 N NaOH consumed
by an acid will be recorded. The acid value can be calculated as.
AV=56.11*V*N/m………………………………………...……………… ……. (3.4)
V∗N
Acid value =56.11* ……….................………………………… ……………. (3.4)
m

3.2.4 Formulation of highly effective ant fungal bar soap


Saponification process to produce soap
25ml of endod oil will be measured by measuring cylinder, then pour the oil in to glass beaker.
Take another measuring cylinder and measure 30ml 20% NaOH solution in it, and then pour it
in to the beaker containing endod oil. the mixture will be stirred vigorously using a glass rod,
then touch the beaker from outside it will be observed that the beaker is warm due to the
exothermic reaction between endod oil and sodium hydroxide, (you should be careful because
the solution is very alkaline. If during the ebullition there are some drops outside the beakers,
they should be immediately clean with a wet cloth). The beaker will be placed on a Bunsen
burner and it will be heated until the mixture become a whitish paste. The mixtures is made up
of soap (in suspension form) and glycerol, then the beaker will be removed from the flame and
allow it to cool and red litmus paper will be dipped in the suspension formed, and when dipped
in the suspension red litmus changes in to blue color, this shows that the solution is basic in
nature, dip blue litmus in the suspension, the color of blue litmus paper remains the same, this
show that soap suspension is not acidic in nature. 15g of common salt (NaCl) will be added in
to the suspension, and stir it with a glass rod, it is observed that the soap is precipitated out as

18
a solid. A filter paper will be taken and fix it in a filter funnel and hold a glass rod over the
funnel. Take the beaker containing soap and pour it over the glass rod and filter the mixture
and soap is left on the filter paper. Take a filter paper and remove soap from the funnel using
a spatula and place it on the other filter paper.dry the soap by pressing it with another filter
paper and cut it in to desired shape with a knife.

Bleach the oil by Add NaCl to


H2O2 suspension and
addition foaming
agents

Mixing of oil and


NaOH

Separation by filter Glycerin


paper
Stirring the mixture

Wet soap
Heating mixture on
Bunsen burner

Cutting of
Drying by filter
dried soap
Cooling the mixture
and measure the
PH

Figure 3.1: overall flow diagram of soap production

3.2.5 Operating conditions on the quantity and quality of the products

Effects of concentration on products


When soap produced at concentration of 30g of NaOH, since the concentration lowers than the
normal lye concentration, the solution produced will be greasy soap. When soap produced at
concentration of 40g, here the concentration higher than the normal lye solution is will be very
viscous almost change to soap. It forms scum like structure. When it produced at concentration
of 50g, soap is at normal lye concentration it will give a good soap.

19
Effects of temperature on products

The higher the temperatures, the faster the trace times. Ideally, the temperatures will be below
110 degrees F for best results. If the lye solution is too cold, it can solidify the oils upon contact.
If the lye is extremely hot, it can cause the saponification process to speed up dramatically. An
increase in temperature can potentially cause a reduction in the viscosity of the fluid. As
temperature increases, more foaming agents must be used.
Effects of reaction time on product
To determine the most effective time for the reaction
Set different time interval in saponification process, time stirring and retention from 40 -120
minute
✓ The saponification value will be recorded
✓ The result will be compared on different time interval
✓ Finally the most effective time interval will be sellected on which we obtain good result.

3.6 Quality measurement on soap produced

Foam ability Tests:Add about 60gm of the soap to a 500ml measuring cylinder containing
100ml of distilled water. Shake the mixture vigorously, so soap produced from endod fruit oil
generate foams. After shaken for about 2mins, the cylinder was allowed to stand for about
10mins. Measure and record the height of the foam in the solution.
Hardness:A quality bar of soap will have a dense, hard feel, and will not immediately begin
to degenerate when wet. It should last a long time. We cure all our soaps before selling, to
achieve a desirable hardness. It is possible to determine the hardness by the following
procedures:
50cm3 boiled water sample will be measured and added into a conical flask. 1cm3 of soap will
be added to the solution, insert the stopper and shake vigorously for 5 seconds. step 2 will be
repeated until a lather forms that lasts for 30 seconds. The total volume of soap will be recorded
solution added. Steps 1-3 will be repeated with 50cm3 samples of all other types of water.
Skin-Safe Ingredients contents: Essential oils and fragrance oils of varying degrees of
quality can be purchased on the open market. In this study natural lemon fragrances
will be added in the processed soap which is preferable for the skin.

20
3.7 Analysis methods and expected results

In the application of this study it is expected to prepare a soap which is very effective in treating
skin attacked by fungus and used in other sanitation service. The soap we are going to produce
can fulfill the demands of a community regarding the problems of lack of antifungal soap and
develop the culture of using indigenous raw materials in the production of soap. And also, a
soap which can meet the required specifications meaning a pH-balanced that recommended for
human body and omits any negative effects. From the indicator of quality of soap one is foam
ability, therefore from our products we expect that the optimum foam ability factor will be 2.57
cm on the 90min, 35 and 40g, time, temperature and NaOH respective.

3.8 Challenges and limitations

✓ Shortage of internet access and computer


There is a lack of internet and computer in institute we ask our class mates and they
help us by giving their computer to use and their internet router.
✓ Lack of time management: All group members have a lack of time to meet, discuss and
work together then we divide tasks of project for each member and then we meet every
important meeting.

21
CHAPTER FOUR
WORK PLAN AND BUDGET BREAKDOWN
4.1 Work Plan
Table 4.1: activities and time schedule
s/n Activities Dec Dec Jan Jan Feb Feb Mar Apr May Jun

1 Title selection

2 Title
submission&
approval
3 Literature
review
4 Develop
method
5 Proposal
submission &
presentation
6 Experimental
setup
7 Conduct
experiment
8 Data inputs

9 Data analysis

10 Report
writing
11 Presentation

22
4.2 Budget Breakdown
Table 4.1 budget breakdown
1 Chemicals Purchase

Chemical Quantity Unit cost (ETB) Total cost


1.1 Sodium hydroxide (NaOH) 1000g 300 300
1.2 Sodium chloride 500g 50 50

1.3 Water 1000ml --- ---


1.4 Hydrogen per oxide 50ml 150 150
1.5 Hexane 2000g 1000 1000
1.6 Sodium laurate 100g 300 300
1.7 Color 50ml 150 150
1.8 Lemon perfume 50ml 300 300
Subtotal 2250

2 Other costs
2.1 Stationary materials 200
2.2 Lab equipment (blender) ---
2.3 Transportation cost 300
2.4 Printing and binding cost 600
Subtotal 1100
Grand total 3350

23
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