WOLLO UNIVERSITY

KOMBOLCHA INSTITUTE OF TECHNOLOGY

SCHOOL OF TEXTILE, LEATHER AND FASHION

TECHNOLOGY

DEPARTEMENT OF TEXTILE ENGINEERING

THESIS TITLE:
EXTRACTION AND APPLICATION OF NATURAL DYE FROM
SYZYGIUM GUINEENSE (DOKIMA) FRUIT FOR DYEING OF COTTON
FABRIC

GROUP MEMBERS

NAME ID NO

1. Belete Desalew………………………………………… WOUR/4944/10

2. Fentabil Getie ………………………............................. WOUR/4955/10

3. Mulu Awoke……………………….............................. WOUR/4355/10

Advisor: Mr. Abebe Marie

Submission date:

Kombolcha, Ethiopia
 DECLARATION

We hereby certify that we are the sole authors of this thesis and that no part of this thesis has
been published or submitted for publication. Our thesis does not infringe upon anyone`s
copyright nor violate any proprietary rights and that any ideas techniques, quotations, or any
other materials from the work of other people included in our thesis, published or otherwise, are
fully acknowledged in accordance with the standard referencing practice and that this thesis has
not been submitted for a higher degree to any other University or Institution.
We hereby declare that the work which is being presented in this project in the title of
"Extraction, application and characterization of Syzygium guineense (dokima) fruit powder for
dyeing of cotton fabric.

Name of candidate Signature Date

Belete Desalew --------------------- -------------
Fentabil Getie --------------------- -------------
Mulu Awoke --------------------- -------------

This thesis was first submitted for approval by our advisor

Name of advisor Signature Date
Mr. Abebe M ---------------------- ------------

Approval by examination committee

This thesis adhere to the provisions of guidelines, policies and legislations of the Kombolcha
Institute of Technology, The thesis is complete and is approved according to the Institute‟s
regulation.
Committee Names Signature Date
1 _________________
2 _________________
3 _________________
4 _________________

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 ACKNOWLEDGMENT

First of all, we would like to thank our almighty God for being source of our capability and
strength to accomplish this project and in fact, throughout our life. Then we would like to
express our most profound thanks to our advisors; Mr. Abebe for their understanding, guidance
and constructive comments and for their encouragement to do this project. Finally, we would like
to express our deep gratitude to Mr.Abebe Marie who is our university advisor for his guidance
on how to write our report and how to do a project. We gratitude also goes to Wollo university
for providing the opportunity to do this study.

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 ABSTRACT

Natural dyes are the colorants collected from the naturally occurring materials such as plants,
animals or from some insects. They are biodegradable and can be decomposed by the
environment, leading to less harmful effect and less pollutant produced to the environment. The
contemporary environmental concerns have stimulated the public interest in natural dyeing that
produces less toxic contamination. Syzygium guineense (dokima) fruit were studied in this
project, the dyability and color fastness of these fruit under different conditions were studied.
The dyeing property study was done by dyeing the cotton fabric with the extract obtained from
the fruits under various conditions and parameter such as the mordents used. The performance
of the color fastness and the dye extracted were evaluated in the present study. Experimental
results revealed that different shades were created by the fruits. The result also showed that
cotton fibers had a better dye absorption and better color fastness. Mordant can help obtain a
better dye absorption and the color fastness on fabric under certain specific dyeing conditions.

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Table of Contents
DECLARATION .......................................................................................................................................... I
ACKNOWLEDGMENT ............................................................................................................................... II
ABSTRACT .............................................................................................................................................. III
List of figure ........................................................................................................................................... VI
List of table ............................................................................................................................................ VI
List of acronyms/abbreviation ............................................................................................................... VII
CHAPTER ONE ......................................................................................................................................... 1
INTRODUCTION ....................................................................................................................................... 1
1.1 Background of the study ................................................................................................................ 1
1.2 Statement of the Problem .............................................................................................................. 3
1.3 Objectives ...................................................................................................................................... 4
1.3.1 General objective ................................................................................................................... 4
1.3.2 Specific objective .................................................................................................................... 4
1.4 Scope of the Study ......................................................................................................................... 4
1.5 Significance of the Study ................................................................................................................ 4
1.6 Benefits and Beneficiaries .............................................................................................................. 5
1.6.1 Benefits .................................................................................................................................. 5
1.6.2 Beneficiaries ........................................................................................................................... 5
1.7 Limitation of the study ................................................................................................................... 6
CHAPTER TWO ........................................................................................................................................ 7
LITERATURE REVIEW................................................................................................................................ 7
2.1 Introduction ................................................................................................................................... 7
2.2 Cotton ........................................................................................................................................... 8
2.3 Natural Dye.................................................................................................................................... 9
2.3.1 Source of Natural Dye ............................................................................................................ 9
2.3.2 Advantages and Disadvantages of Natural Dyes .................................................................. 10
2.3.3 Methods of extraction of the natural dye ............................................................................ 12
2.4 Cotton dyeing .............................................................................................................................. 15
2.4.1 Preparation of cotton fabric and dyeing with natural dyes .................................................. 15
2.5 Mordant ...................................................................................................................................... 17
2.5.1 Classification of Mordant ..................................................................................................... 17
2.5.2 Influence of Mordants on Dyeing and Colorfastness ............................................................ 19

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 2.5.3 Mordanting Methods ........................................................................................................... 19
2.6 Syzygium guineense (dokima) fruit............................................................................................... 20
2.6.1 Characteristics of syzygium guineense fruit.......................................................................... 22
2.7 Synthetic Dyeing .......................................................................................................................... 25
2.7.1 Synthetic Dyeing and their Influence.................................................................................... 25
2.8 Literature gap .............................................................................................................................. 26
CHATER THREE ...................................................................................................................................... 27
METHODOLOGY .................................................................................................................................... 27
3.1 Materials ..................................................................................................................................... 27
3.2 Chemicals .................................................................................................................................... 27
3.3 Equipment’s................................................................................................................................. 27
3.4 Methods ...................................................................................................................................... 28
3.4.1 Sample preparation .............................................................................................................. 28
3.4.1 Aqueous extraction of syzygium guineense.......................................................................... 29
3.4.2 Dyeing of cotton with syzygium guineense .......................................................................... 30
3.4.3 Mordanting procedures........................................................................................................ 31
3.5 Evaluation of syzygium guineense dyed cotton samples ............................................................... 32
3.5.1 Color strength....................................................................................................................... 32
3.5.2 Washing fastness.................................................................................................................. 33
3.5.3 Rubbing fastness .................................................................................................................. 34
Figure 3.8 rubbing fastness test ............................................................................................................. 34
CHAPTER FOUR ..................................................................................................................................... 35
RESULTS AND DISCUSSION .................................................................................................................... 35
4.1 Extraction of Colorant .................................................................................................................. 35
4.2 Washing and rubbing fastness result analysis ............................................................................... 35
4.3 Color strength result analysis ....................................................................................................... 37
CHAPTER FIVE........................................................................................................................................ 39
CONCLUSIONS AND RECOMMENDATIONS ............................................................................................. 39
Conclusion............................................................................................................................................. 39
Recommendations ................................................................................................................................ 40
Reference .............................................................................................................................................. 41

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 List of figure
Figure 2.1: Cotton ready for harvest ...........................................................................................8
Figure 2.2: The molecular structure of cellulose ..........................................................................9
Figure 2.3 flower and fruit of syzygium guineense .................................................................... 21
Figure 2.4 the chemical structures of compounds isolated/detected from Syzygium guineense .. 24
Figure 2.5 Molecular structure of anthocyanin........................................................................... 24
Figure 3.1chart flow method of dye powder preparation ............................................................ 28
Figure 3.2 figure flow method of dye powder preparation ......................................................... 29
Figure 3.3 dye extraction procedure .......................................................................................... 30
Figure 3.4 fabric sample dyeing procedure ................................................................................ 31
Figure 3.5 spectrophotometer data color 850(Color strength tester machine) ............................. 33
Figure 3.6 washing fastness test by Launder meter ISO test method 4 ....................................... 33
Figure 3.7 rubbing fastness test ................................................................................................. 34
Figure 4.1 graphical compare of color strength of the dyed sample ............................................ 38
Figure 4.2 tested sample fabric .................................................................................................. 38

List of table

Table 1 Different natural dye extraction with optimum conditions ............................................. 14

Table 2 Nutritive value of dokima fruit per 100g of edible portion ............................................ 23
Table 3 optimization of dye extraction from syzygium guineense fruit peel ............................... 30
Table 4 dyeing optimization for dyeing of cotton with this extracted dye................................... 31
Table 5 washing fastness result analysis .................................................................................... 36
Table 6 rubbing fastness result analysis ..................................................................................... 36
Table 7 dyed fabric color strength result analysis ...................................................................... 37

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 List of acronyms/abbreviation

ISO International standard organization

K Light absorbency coefficient

S Light scattering coefficient

R Light reflection

O.W.F On weight of fabric

Gpl Gram per litter

MLR Material to liquor ratio

PH Potential of hydrogen

Mg Milligram

Kcal Kilo calorie

Cm Centimeter

O
C Degree Celsius

% percent

Λ lambda

CIE Commission international d,eclarge

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 CHAPTER ONE

INTRODUCTION

1.1 Background of the study

Anciently, the purpose of coloring textile was initiated using colors of natural source, until
synthetic colors/dyes were invented and commercialized.

Dyes may be defined as substances that, when applied to a substrate provides color by a process
that alters, at least temporarily, any crystal structure of the colored substances. Such substances
with considerable coloring capacity are widely employed in the textile. The dyes can adhere to
compatible surfaces by solution, by forming covalent bond or complexes with salts or metals, by
physical adsorption or by mechanical retention. Dyes are classified according to their application
and chemical structure, and are composed of a group of atoms known as chromophores,
responsible for the dye color. Chromophore-containing centers are based on diverse functional
groups, such as azo, anthraquinonoid, methane, nitro, aril methane, carbonyl and others. [1]

Dyes derived from natural materials such as plant leaves, roots, bark, insect secretions, and
minerals were the only dyes available to mankind for the coloring of textiles until the discovery
of the first synthetic dye in 1856. Rapid research strides in synthetic chemistry supported by the
industrialization of textile production not only led to the development of synthetic alternatives to
popular natural dyes but also to a number of synthetic dyes in various hues and colors that
gradually pushed the natural dyes into oblivion However, environmental issues in the production
and application of synthetic dyes once again revived consumer interest in natural dyes during the
last decades of the twentieth century. Textiles colored with natural dyes are preferred by
environmentally conscious consumers and today there is a niche market for such textiles. [2]

Most textile dyers and manufacturers therefore shifted towards the use of synthetic colorants,
because they were cost advantageous, easy to obtain in different grades, types and classes. As a
result, this considerably lowered the cost of natural dyes, because the quality of dyeing needed
improvement. [3]

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Natural dyes were the main source of colorants for textiles until the end of 19th century.
However, after the discovery of synthetic dyes, natural dyes were completely replaced by
synthetic dyes. The ease of application, availability of wide range of colors, better reproducibility
and improved quality of dyeing at lower cost are the main advantages of synthetic dyes over
natural dyes. However, many of the synthetic dyes particularly azo dyes are found to be
carcinogenic and harmful to health and environment. [4]

Most of the natural dyes have no substantively for the fiber and mordents are used. But mordant
are usually derived from metallic salts; the commonly used metal salts include alum, chrome,
stannous chloride (tin), copper sulphate and ferrous sulphate. These chemicals act as mordant by
fixing themselves on the fiber and also combines with the dyestuff. Therefore, mordant form a
link between the fiber and the dye, which allows certain dyes with no or little affinity for the
fiber to be fixed. [5]

Syzygium guineense (dokima) is an under exploited indigenous fruit tree of India and some
African countries like Ethiopia. It is a hardy crop and can tolerate drought as well as heavy
rainfall conditions. The tree is evergreen but sheds its leaves under drought conditions. It
produces purple delicious fruits with prominent seeds. Because of its medicinal values and
suitability for planting as wind break, its demand is increasing day by day and that will require
selected plants of superior quality and high yield potential [6]. The syzygium guineense tree
starts flowering from March-April followed by fruiting (berry), which appears in May-June.
Fruit color change from green to deep-red or bluish-black at full ripening stage [7].

Syzygium guineense (dokima) is always appreciated for the color, flavor and taste of its fruit. It
is very large tropical tree that belongs to Myrtaceae family and known by synonyms jambolan or
black plum. Worldwide, it is known by some other names like Java Plum, dokima, Black Plum,
Indian blackberry, Portuguese Plum, Jambolan Plum etc. Syzygium guineense fruits have a
single seed and a soft dark purple colored almost black skin and a lighter purple flesh. When
eaten, the fruits coat the mouth and the tongue a deep purple color that stays for a few hours. The
fruit is sweet and leaves a slight astringent action in the mouth. The fruit of syzygium guineense
is a great benefit when it comes to lowering of blood glucose level and reduces glycosuria. It also
contains Vitamins C & A, riboflavin, nicotinic acid, choline, folic acid, maleic acid, sodium,
potassium, calcium, phosphorus, manganese, zinc and iron [8].

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1.2 Statement of the Problem
Today, most processes executed in the textile and clothing industry discharge atmospheric
emissions that are disturbing the eco-balance. Most of textile dyers/ manufacturers shifted
towards use of synthetic colorant due to pure synthetic dyes of different types/classes and its cost
advantages. But almost all synthetic colorants are being synthesized from petrochemical sources
through hazardous chemical processes and The synthetic dye stuffs are suspected to cause
allergies, and are carcinogenic and detrimental to human health, these lead textile factories to
look backward for eco-friendly dyeing. One of the many options of eco-friendly dyeing is
application of natural dyes for coloring textiles. So to solve the above problem we were extracted
dye from syzygium guineense (dokima) fruit peel and use for coloring textiles.

Natural dyes are believed that they have better biodegradability, have wide variety, less-toxic,
non-carcinogenic, easily available and Renewable, eco-friendly and generally higher
compatibility with the environment; provide a wide range of beautiful shades with acceptable
levels of colorfastness. Many of natural dye pose anti-microbial property. Therefore, textiles
dyed with such materials are also likely to show anti-microbial property as reported by many
researchers. The present study focuses on the extraction of dye from syzygium guineense fruit
peel for to dyeing of cotton fabric by optimizing the extraction and dyeing condition. Making
color or dye by using syzygium guineense (dokima) fruit is not common in dyeing with natural
dyes and this research aims to investigate the above phenomenon. Such a trial might also lead to
anti-microbial property which would avoid or reduce the development of microorganism on the
fabric.

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1.3 Objectives
1.3.1 General objective
To extract and study the characterization of natural dye from syzygium guineense (dokima) fruit
for dyeing of cotton fabric

1.3.2 Specific objective

• To extract dye from syzygium guineense fruit

• To optimize the extraction of dye from syzygium guineense fruit

• To dyeing of cotton fabric by using syzygium guineense fruit peel of natural dye

• To checking the fastness property of dyed fabric

• To test the performance of natural dye and their application

1.4 Scope of the Study

The scope of this research includes collection of the raw materials, extraction of the natural dye,
dyeing of cotton with the extracted natural dye, determining the dye ability of selected plant dye
sources namely, syzygium guineense (dokima) fruit, carrying out test to the dyed fabric and
finally analyzes result and discussion.

1.5 Significance of the Study

This study is significant enough not only to convert the material into some useful product or dye
but also; it can identify the dye ability of this dye on cotton fabric.

Quantitative and qualitative finding of this research will enhance knowledge and understanding
on the potential utilization of plant extract for dye manufacturing. The study seeks to explore and
capture natural plants from which dyes can be extracted and applied to cotton. In addition, the
study would create the awareness of using plant dyes and finally serve as a reference material to
other research works.

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This study should be significant in a way that it will: -

• Minimize the significant environmental pollution aspect and impact of synthetic dye.

• Minimize the impact of health hazardous from human beings and animal.

1.6 Benefits and Beneficiaries

1.6.1 Benefits
• The shades produced by natural dyes/colorant are usually soft, lustrous and soothing to
the human eye.

• Natural dyestuff can produce a wide range of colors by mix and match system.

• Natural dyestuffs produce rare color ideas and are automatically harmonizing.

• Unlike non-renewable basic raw materials for synthetic dyes, the natural dyes are usually
renewable, being agro-renewable/vegetable based.

• It is biodegradable, non-toxic and non-allergic.

• It can reduce environmental pollution.

• Increase awareness about the realization that the intermediates and chemical used in
synthetic dye being toxic and hazardous to human health as well as to the environment.

1.6.2 Beneficiaries
The direct beneficiaries of this research will be:

Customers: customers become satisfying having health product for their skin and for
environment also.

The Societies: for the reason that natural dyes are environmentally friendly, the introduction of
special natural dyes will decrease suffering of environmental pollution by synthetic dyes.

Researchers: the researcher will get a great benefit from this research such as knowing how to
make research.

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Textile industries: extracting of natural dye from dokima plant has a great advantage for textile
industries i.e. the company reduces the cost for purchasing dye and to reduce the environmental
pollution of aquatic life in the dyeing company.

1.7 Limitation of the study

In our project there are different limitations in order to done the study? Those are: -

The duration of time to perform the research was short period due to inter personal conflict of
Ethiopian people.

Lack of extraction equipment and chemical in our textile department laboratory. Such as there is
no ethanol and evaporator when we want to extract the dye by using solvent extraction method.

Lack of fastness tester machine in our laboratory.

Electric power shortage in our campus due to this the work is not perfectly done and many time
consumption.

Lack of industrial soap for washing of the dyed fabric in our textile department laboratory.

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 CHAPTER TWO

LITERATURE REVIEW

2.1 Introduction
Dyes are a highly colored substance used to impart color to an unlimited variety of materials like
textiles, paper, wood, varnishes, leather, ink, fur, foodstuff, cosmetics, medicine, toothpaste, etc.
a dye molecule has two principal chemical groups i.e. chromophores and auxochromes. The
chromophore, usually an aromatic ring, is associated with the coloring property. It has
unsaturated bonds such as –C=C, =C=O, –C–S, =C–NH, –CH=N–, –N=N– and –N=O, whose
number decides the intensity of the color. The auxochrome helps the dye molecule to combine
with the substrate, thus imparting color to the latter. [9]

Natural dyes are colorants derived from plants, invertebrates, or minerals. The majority of
natural dyes are vegetable dyes from plant sources –roots, berries, bark, leaves, fruit and wood
and other organic sources such as fungi and lichens. Dye yielding plants, unlike synthetic dyes
may contain more than one chemical constituent, each exhibiting different color and properties
operating singly or in combination with the different groups, depending on their chemical
structure and composition. The colorants from plant origin used in dyeing different fibers are
mainly flavonoids, anthraquinone and indigoids. [10]

Reports on the phytochemical screening tests of the fruit extracts of Syzygium guineense showed
presence of secondary metabolites such as flavonoids, tannins, saponin, alkaloids and cardiac
glycosides. These metabolites are believed to be responsible for traditional medicinal uses of the
plant or its potential as source of bioactive compounds to be used in drug discovery. Studies
carried out on Syzygium guineense (of Ethiopian origin) also indicated that extracts from its
different parts showed antimicrobial, antihypertensive and antimalarial activities. [17]

Different parts of the Syzygium guineense were also reported for its antioxidant, anti-
inflammatory, neuropsycho-pharm-mycological, anti-microbial, and anti-bacterial, antifungal,
nitric oxide scavenging, and free radical scavenging, anti-diarrheal, antifertility, and radio-

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protective activities. Syzygium guineense of good size and quality, having a sweet or sub acid
flavor and a minimum of astringency, are enjoyable raw and may be made into tarts sauces and
jam. [18]

Syzygium guineense are an important sourceof wine, resembling Port.Jamunvinegar, extensively

made throughout India, is an attractive, clear purple, with a pleasant aroma and mild flavor.
Traditionally the syzygium guineense fruits, leaves, seeds, and bark are all used in Ayurvedic
medicine. [19]

A glycoside in the seed, syzygium guineense is considered to have anti-diabetic properties. The
seeds have also shown anti-inflammatory effects in rats and antioxidant properties in diabetes
[20]. Syzygium guineense fruit reduces the sugar in the blood and is very good in the control of
diabetes. Its seeds contain Glycoside, Jamboline and Elegiac acid, which are reported to have the
ability to check the conversion of starch into sugar in case of excess production of glucose [21].

2.2 Cotton
Cotton is a soft, fluffy staple fiber that grows in a boll, or protective case, around the seeds of the
cotton plants of the genus Gossypium in the mallow family Malvaceae. The fiber is almost
pure cellulose, and can contain minor percentages of waxes, fats, pectin‟s, and water. Under
natural conditions, the cotton bolls will increase the dispersal of the seeds.

Cotton was independently domesticated in the old and new Worlds. The fiber is most
often spun into yarn or thread and used to make a soft, breathable, and durable textile. And it is
the most widely used natural fiber cloth in clothing today. [23]

Figure 2.1: Cotton ready for harvest

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Cotton, as a member of the vegetable fibers family, is composed fundamentally of cellulose,
which is chemically classified as a carbohydrate. The structure formula of cellulose is
(C6H10O5) n, which has a technical name 1, 4-β-D-glucan. [24]

Figure 2.2: The molecular structure of cellulose

2.3 Natural Dye

The word „natural dye‟ covers all the dyes derived from the natural sources like plants, animal
and minerals. Natural dyes are mostly non-substantive and must be applied on textiles by the
help of mordents, usually a metallic salt, having an affinity for both the coloring matter and the
fiber. Transition metal ions usually have strong coordinating power and/or capable of forming
week to medium attraction/interaction forces and thus can act as bridging material to create
substantivity of natural dyes/colorants when a textile material being impregnated with such
metallic salt (i.e. mordanted) is subjected to dyeing with different natural dyes, usually having
some mordant able groups facilitating fixation of such dye/colorant. These metallic mordant after
combining with dye in the fiber, it forms an insoluble precipitate or lake and thus both the dye
and mordant get fixed to become wash fast to a reasonable level. [25]

If we compared natural dye with synthetic dye, then natural dyes are found eco-friendly and they
have no carcinogenic or allergic effect for human being especially for dyers. They can get these
natural dyes at low prices that are used mostly in our industry for dyeing of cotton fabric. [29]

2.3.1 Source of Natural Dye

Natural dye can be obtained from different sources. Natural dyes fall into four categories on the
basis of their origin: plant, animal, mineral and insect. [29].
1) Plant dye: Natural dyes obtained from plants -Berry, flower, bark, leaf, seed etc. (e.g.
catechu, Indigo era, myrobalan, pomegranate).The different parts of plants for example roots,
nuts and flowers are sources of coloring pigments and dyes and used for extracting natural color

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and they have antimicrobial, antifungal, insect repellent, deodorant, disinfectant and other
medicinal values. Henna (orange-red) -from leave of henna plants, Crochu (brown) -from resin,
sticky substance from plant of acacia tree, Fustic (yellow)-from the wood of the fustic tree,
Indigo (C16H10N2O2(blue)-from leaves and stems of the indigo plant, Logwood (black)-from
the core (heart) of the log wood tree, Turmeric (violet) - from the roots the turmeric plant and
Saffron (yellow) -from stigmas of the common crocus are the common ones [31]. Local plants
are one source of natural colorant which is grouped under plant sources. They are easily
available in the country and can be considered as zero cost dyes as they are planted for other
purposes. These vegetable sources are not only replaceable but also biodegradable. They also
have pharmaceutical and health benefit. [29]

2) Animal dye: Natural dyes obtained from animal – Mollusk, murex snail, cuttlefish and
shellfish. Red mouthed rock shell was one of the main sources of Tyrian purple and study blames
its collapse on rising sea temperature. Phoenician purples and Biblical Blues are the most royal
and sacred of all ancient dyeing was produced from Levantine sea snails of the family Muricide.
These mollusks may have been in use for the production of the royal purple pigment. [32]

3) Mineral dye: Natural dyes obtained from mineral – Clay, ochre and malachite. As minerals
are used for fixing or improving the fastness of vegetable dye, the name natural dye is more
appropriate which cover all the dyes derived from natural resources including vegetable dyes as
well as minerals. And some minerals are also used to give a coloring matter. For examples, cow
urine, cow dung, egg albumin. [29]

4) Insect dye: -Natural dyes obtained from insects – Cochineal and lac. Secretion of insects and
dried insect bodies are the major source of natural dyes. For example, shell-fish provides the
coloring matter. [9]

2.3.2 Advantages and Disadvantages of Natural Dyes

In the recent years, there has been a trend to revive the art of natural dyeing. This is mainly
because in some aspects natural colorants are advantageous against synthetic dyes. Some of these

Advantages along with some limitations are listed below: [34]

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 A. Advantages of natural dyes
• Natural dyes are non-allergic, non-toxic, less polluting, less health hazardous, on
carcinogenic and non-poisonous.
• Natural dyes have better biodegradability and generally have higher compatibility with the
environment.
• These dyes can also reap in social benefits. They can give inputs to the economy of the
developing nations.
• These provide sustainable livelihoods for the agriculturists.
• They are environment friendly, easily available and can be recycled after use.
• The shades produced by natural dyes/colorants are usually soft, lustrous and Smoothing to
the human eye.
• Natural dyestuffs produce rare color ideas and are automatically harmonizing.
• Unlike non-renewable basic raw materials for synthetic dyes, the natural dyes are usually
renewable, being agro renewable/vegetable based and at the same time biodegradable.
• Application of natural dyes has potential to earn carbon credit by reducing consumption of
fossil fuel (petroleum) based synthetic dyes.
• Some of its constituents are anti-allergens, hence prove safe for skin contact and are mostly
non-hazardous to human health.
• Some of the natural dyes are enhanced with age, while synthetic dyes fade with time.
• Natural dyes bleed but do not stain other fabrics, turmeric being an exception.
• Natural dyes are usually moth proof and can replace synthetic dyes in kids‟ garments and
food-stuffs for safety.
B. Disadvantages of natural dyes
Although natural dyes have several advantages but there are some limitations as well. These are
as follows:
• Inadequate fastness properties in comparison with synthetic dyes.
• Great difficulty in blending natural dyes.
• Non-standardized methods.
• Difficult to standardize a recipe for the use of natural dyes, as the natural dyeing process,
• Color development depends not only on color component but also on materials.
• Natural dyes are the low to medium fastness properties especially poor light fastness.

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• Have poor reproducibility, particularly the plant sources since they are affected by
environment conditions like varying planting time, place and species.
• Non-availability due to difficulty in collection, bulk isolation of dye-stuff, standardization
of dyeing procedure, color yield and complexity of the dyeing process.

2.3.3 Methods of extraction of the natural dye

As natural dye-bearing materials contain only a small percentage of coloring matter or dye along
with a number of other plant and animal constituents such as water-insoluble fibers,
carbohydrates, protein, chlorophyll, and tannins, among others, extraction is an essential step not
only for preparing purified natural dyes but is also required to be carried out by users of crude
dye-bearing materials. As natural coloring materials are not a single chemical entity and the plant
matrix also contains a variety of non-dye plant constituents, extraction of natural dyes is a
complex process. The nature and solubility characteristics of the coloring materials need to be
ascertained before employing an extraction process. [35].

i. Acid and Alkali Extraction Process

As many dyes are in the form of glycosides, these can be extracted under dilute acidic or alkaline
conditions. The addition of the acid or alkali facilitates the hydrolysis of glycosides resulting in
better extraction and higher yield of coloring materials. An acid hydrolysis process is used for
the extraction of dye from fruit. Acidified water is also used for extracting some flavone dyes to
prevent oxidative degradation. Alkaline extraction is suitable for dyes having Phenolic groups as
they are soluble in alkali, which improves the dye yield. Dyes can be later precipitated by the use
of acids. [35] The disadvantage of this process is that some coloring materials may be destroyed
under alkaline conditions considering the fact that some of the natural dyes are pH sensitive.

ii. Ultrasonic and Microwave Extraction

These are actually microwave- and ultrasound-assisted extraction processes where extraction
efficiency is increased by the use of ultrasound or microwaves thus reducing the quantity of
required solvent, time, and temperature of extraction.

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iii. Fermentation

This method of extraction uses the enzymes produced by the microorganisms present in the
atmosphere or those present in the natural resources for assisting the extraction process.

Fermentation method is similar to aqueous extraction with the exception that this method does
not require high temperatures. The microorganisms disintegrate the coloring matter binding
substances in natural way. Long extraction time, need for immediate extraction of pigments after
harvesting, foul smell due to microbial action, and so on, are some of the disadvantages of this
method [36].

iv. Enzymatic Extraction

As plant tissues contain cellulose, starches, and pectin‟s as binding materials, commercially
available enzymes including cellulose, amylase, and pectinase have been used by some
researchers to loosen the surrounding material leading to the extraction of dye molecules under
milder conditions. This process may be beneficial in the extraction of dye from hard plant
materials such as bark, roots, and the like. [36]

v. Solvent Extraction
Natural coloring matters depending upon their nature can also be extracted by using organic
solvents such as acetone, petroleum ether, chloroform, ethanol, methanol, or a mixture of
solvents such as mixture of ethanol and methanol, mixture of water with alcohol, and so on. The
water/alcohol extraction method is able to extract both water-soluble and water insoluble
substances from the plant resources. The extraction yield is thus higher as compared to the
aqueous method as a larger number of chemicals and coloring materials can be extracted. Acid or
alkali can also be added to alcoholic solvents to facilitate hydrolysis of glycosides.

vi. Supercritical Fluid Extraction

Supercritical fluid extraction is an emerging area in natural product extraction and purification. A
gas functions as a supercritical fluid above its critical values of temperature and pressure. Such a
fluid has physical properties somewhere between those of a liquid and a gas. The disadvantage of
the method is the high cost of the equipment and poor extraction of polar substances. [38]

Page | 13
Vii. Aqueous Extraction

The aqueous extraction method is conventional, simple, and suitable for the extraction of plant
components that can be distilled with steam without changing the molecular structure. To
escalate the extraction efficiency the coloured materials are cut into small pieces then crushed
into powder form and stored overnight in a steel container or even longer to loosen the cell
structure. These compounds are incompatible with water or slightly soluble and have a certain
vapour pressure at the boiling point of 100 °C. [39]
The substance can be carried out with the steam when the water boils. After condensation, it is
isolated by an oil-water separator to separate the water to obtain the required plant components.
The boiling and separation process may be repeated depending on the extraction outcomes. A
trickling filter can easily separate the dye and thin plant residues. However, the colour yield of
temperature-sensitive dyes may be affected by boiling, so low temperature is recommended.
Dyes obtained by this process can be used for textile applications.
Like all methods, this method also has some disadvantages like, long processing time, high water
usage, and temperature. [40]
Table 1: Different natural dye extraction with optimum conditions

N Natural Source Material Form Tmp (oC) Time MLR pH Yield

o (min) (w/w) %
1 Pomegranate Pre-cut dried rind 90°C 45 min 1:20 11 40%
Rind crushed to powder
form
2 Mariegold Dried petal crushed 80°C 45 min 1:20 11 40%
(Genda) to powder form
3 Babool (Babla) Sun- dried bark 70°C 120 min 1:20 11 40%
rushed to powder
form
4 Catechu powder form 90°C 60 min 1:20 40%
(Khayer)

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2.4 Cotton dyeing
There are many dyes used on cotton fabrics. Depending on their chemical structure, the principle
of dyeing varies. Most natural dyes require a metal mordant or tannic acid in dyeing cotton
fibers. [42]
It has been reported that pretreating cotton with a cationic surfactant enhances the uptake of acid
dyes. Usually cotton fabrics undergo a series of preparation steps before dying, such as bleaching
and scouring to enhance the dyeing process. The associated factors include the temperature, time,
amount and type of surfactant, all of which influence dye uptake on cotton. [43]
Most of the studies reported on dyeing of cotton with natural dyes are mainly on use of different
mordants, pre, post and simultaneous Mordanting techniques, standardization of dyeing
condition, influence of pH on color, mordant mixing along with use of sonication for optimum
extraction technique.
Optimization process was done by considering different pH conditions, type of mordant and
concentration of dye. [44]

2.4.1 Preparation of cotton fabric and dyeing with natural dyes

Cotton is purely cellulosic fiber and found throughout the world with many varieties and
qualities. In general, cotton fiber-based textiles is desized (for woven fabric only), scoured
And bleached as preparatory process before dying. In many places of world, the age-old process
followed in preparing a cotton cloth and its dyeing with natural dyes followed by artisan/cottage
level dyers is given below. [45]
A. Dunging - The cloth is soaked for one night in a solution of water and fresh dung.
B. Washing- Next morning, cloth is thoroughly washed, rinsed and water sprinkling is continued
over the cloth at short interval until evening, then it is finally washed and dried mechanism of
fixation of natural dyes through mordents.
C. Steaming– Then the cloth is steamed for one night in an ordinary Khumb or washer man‟s
steaming pot.
D. Steeping in alkaline lye- The cloth is soaked in a mixture of water, oil.
E. Rinsing- Cloth is then again rinsed thoroughly and spread out to dry.

Page | 15
F. The last two processes are repeated for several days, the details varied in different localities,
but generally from 3 to 7 days. In specific case, the cloth is kept in the solution for sometimes,
and then taken out, rinsed and dried twice daily.
G. Washing- The cloth is then finally washed in clean water, but not so thoroughly as to remove
the whole of the oil, and finally dried in air under the sun.
H. Galling-The cloth is then soaked in a solution of harda (haritaki) or myrobolan
(Terminalachebula) extracts. Behda or bahedas (terminalabelerica) is also used instead of harda.
The period during which the cloth is kept in the harda extract varied in different places but it is
continued until the fabric assume a yellowish tint.
I. Drying- The cloth is spread or wrung out for drying
J. Mordanting- The cloth is then pre-mordent by dipping it in a solution of potash alum and
water. In some places, gum or a paste of tamarind seed (tamarind kernel powder) is added to
make it sticky. In some parts of Kutch, fuller‟s earth is also used by some dyers. The cloth is thus
ready for subsequent dyeing.
K. Dyeing- For dyeing the cloth is generally boiled with an aqueous extracted solution of the
natural dye until all the coloring matter is absorbed by the cloth.
L. Further dunging- In some places, the cloth is further soaked in dung for one night and
batched before final wash and dry.
M. Drying- The dyed fabric is next washed and spread out to dry gradually in air under the sun.
Water is sprinkled at certain interval over the cloth, so as to brighten the color; this process is
continued for 2-4 days.
N. Finishing- If required, the cloth is finally starched by dipping it in a paste of rice or wheat
flour, or in a solution of babool gum and then dried. However, now a day, many small-scale
dyers/export-oriented units follow much shorter economical and standard recipe based optimized
processes for natural dyeing of cotton yarns/fabrics. Before natural dyeing usual method of
desizing (acid bath), scouring (soap & soda) and H2O2 bleaching are followed. Well prepared
cotton textiles are then mordant (single or double mordanting using hard and aluminum sulphate
individually or in combination) before subjecting to dyeing with aqueous extract of selective
natural dyes at standardized condition of process variables of dyeing.
the dyeing conditions of natural dye may be as follows: dyeing time, 30 -120 minutes (depending
on shades); dyeing temperature, 70- 100°C; material to liquor ratio, 1:20 -1:30; concentration of

Page | 16
natural dye, 10-50% (owf) or more; common salt concentration, 5-20g/L and pH, 10-12. In each
case after the dyeing is over, the dyed samples are repeatedly washed with hot and cold water
and then finally, the dyed samples are subjected to soaping with 2g/L soap solution at 60 OC for
15 min, followed by repeated water wash and line dried. For improving its wash fastness,
treatment with ecofriendly cationic dye fixing agent is advisable. [44]

2.5 Mordant
The term mordant comes from the Latin modere “to bite”. In the past it was thought that a
mordant helped the dye bite on to the fiber so that it would hold fast during washing. A mordant
or dye fixative is a substance used to set or bind dyes on fabrics by forming coordination
complex with dye, which then attaches to fabrics. [46]
Limitation on color yield and poor fastness properties prompted a search for idea mordents, the
chemicals which increase natural dye uptake by textile fibers. Different types of mordents yield
different colors even for the same natural dye. Therefore, final color, their brilliance and color
fastness properties are not only dependent on the dye itself but are also determined by varying
concentration and skillful manipulation of the mordents. Thus, a mordant is more important than
the dye itself. Moreover, the ideal mordant for bulk use should produce appreciable color yield in
practicable dyeing conditions at low cost, without seriously affecting physical properties of fiber
or fastness properties of the dyes. Also, it should not cause any noxious effect during processing
and the dyed textile material should not have any carcinogenic effect during use. [46]

2.5.1 Classification of Mordant

A. Metallic mordents
They are generally metal salts of aluminum, chromium, and iron, copper and tin. The metallic
mordents are of two types. [47]
1. Brightening mordents
i. Alum: Among all types of alum, potash alum is cheap, easily available and safe to use
mordant. It usually produces pale versions of the prevailing dye color in the plant.
ii. Chrome (potassium dichromate): It is also referred to as red chromate. It is relatively more
expensive. However, Cr3+ or Cr6+ is considered to be harmful for human skin as objectionable
heavy metal beyond a certain limit of its presence. Its use has been limited as per the norms of
the eco-standards. The dichromate solution is light sensitive and therefore it changes color under

Page | 17
light exposure.
iii. Tin (stannous chloride): It gives brighter colors than any other mordant. However, they are
oxidized on exposure to air and may impart a stiff hand to the fabric. Stannous Chloride also
causes higher loss of fabric tenacity (tensile strength) if applied beyond a certain concentrations.

2. Dulling mordents
i. Copper (cupric sulphate): Known as blue vitriol, it is readily soluble in water and easy to
apply. It gives some special effects in shades, which otherwise cannot be obtained. However,
copper beyond a certain limit is also under the eco-standard norms as objectionable heavy
metals.
ii. Iron (ferrous sulphate): It is also known as green vitriol and is readily soluble in water. It is
used for darkening /browning and blackening of the colors/ shades. It is easily available and one
of the oldest mordents known. It is extensively used to get grey to black shades. [48]
B. Tannins
The term „tanning agent‟ is given initially to those water-soluble cellulosic materials that
predicates gelatin from solution. But all gelatin precipitation did not identify as tanning agent.
Tannins are polyphenol compounds having capacity of gelling under certain conditions. [49]
(a) It may be hydro ysablepyrogallol tannins exemplified by „tannic acid‟, by Chinese or Turkish
Gallo tannins (galls) and by Sicilian and Stags horn sumac,
(b) Hydroysableellagi tannins that give ellagic acid or similar acids on hydrolysis, exemplified
by Valona, chestnut, and
(c) Condensed or catechol tannins that contain little or no carbohydrates and are converted to
acids to insoluble amorphous polymers. Among the tannins, myrobalan (harda) and galls/sumach
are most important.
C. Oils type mordents
The main function of an oil mordant is to form a complex with alum when it is used as the main
mordant. This is because oil is insoluble in water and doesn‟t have affinity for cotton hence
won‟t easily be washed out from the treated fabric. Oil mordents contain fatty acids such as
palmitic, stearic, oleic, ricinoleic and glycerides. [50]

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2.5.2 Influence of Mordants on Dyeing and Colorfastness
Numerous researchers investigating the application of natural dyes and mordants have examined
dye exhaustion, colour quality, and colourfastness properties with varied results, depending on
the complex interaction among fibre type, mordant agent, dye type, and application parameters
(e.g., substrate preparation, component concentration, time, temperature, etc.).
The mordant type can influence dye-fibre association and thus colourfastness to wet and
mechanical treatments (e.g., crocking) as well as lightfastness. [51]

2.5.3 Mordanting Methods

Mordanting can be achieved by pre-mordanting (before dyeing), simultaneously mordanting and
dyeing or post mordanting system (after dyeing). [52]
1. Pre-mordanting
Pre-mordanting is a technique which involves primarily mordanting the fabric before dyeing i.e.
the mordant is applied to the fabric prior to dyeing. It‟s the most common method of mordanting
practiced on cotton, cellulosic and some animal fibers such as cochineal because these often in
un mordanted form don‟t have affinity for many natural dyes. The advantage of this method is
that the standing baths can be reused many times after replenishing with the mordents. This
makes the process economical as well as reducing the pollution load hence sufficient for large-
scale application
The procedures for mordanting are;
i). Dissolve the mordant and added to a dye bath containing ample amount of water.
ii). Add the substrate and bring the whole mixture to boil for a period of about ¾ of an hour.
iii). Cool the solution
iv). gently remove the substrate to ensure even take-up of the mordant.
v). Rinse the substrate to remove unfixed dyes, dry under room temperature and analyze. The
fabric can afterwards be dyed.
The disadvantage associated with this method is that there is a lot of fabric handling.
2. Simultaneous mordanting
As the name states, both the dyeing and mordanting process is carried out in the same dye bath
and at the same time. For cotton and other cellulosic, the mordant is usually added to the dye
bath at the start of dyeing so that both mordanting and dyeing processes take place concurrently

Page | 19
The procedures for this method are;
i). First dissolve mordant in a separate bath.
ii). Transfer mordant solution to the dye bath and add the wetted fabric.
iii). Bring whole mixture to boil while stirring at intervals using a stirring rod.
iv). Simmering until maximum dye uptake.
v). Cool solution, remove fabric, rinse with mild detergent, dry and analyze.
Although this method is associated with less fabric handling, it gives colors that are not as
permanent as pre-mordant fabrics because mordanting is dissolved at a separate stage and later
on introduced into the dye solution.
3. Post mordanting
In this method, the fabric after dyeing is treated with the mordant in a separate bath. The final
color is developed during the last phase. Iron salts are very often applied in this manner for
producing grey and black colors
The procedures are as follows;
i). Dissolve mordant in ample amount of water.
ii). during simmering (after dyeing), add solution to dye bath in the final five to ten minutes.
iii). Cool solution, remove substrate.
iv). Rinse with cold water to remove unfixed dyes, dry and analysis.
The action of a mordant on a substrate depends on various factors such as its concentration, kind
of mordant used, type of substrate and the method of mordanting and dyeing. Usually, the type
of mordant affects the fastness property of the dye and also changes the shade after dyeing. If the
action of the mordant on the cotton substrate is hard (acidic mordant with an acidic dye), the best
technique to employ is either pre or post mordanting because they limit the potential damage to
the substrate.

2.6 Syzygium guineense (dokima) fruit

Syzygium guineense is named locally as “dokima‟‟. Commonly known as Jamun or Indian
blackberry in English it goes by the scientific name Syzygium guineense. Syzygium guineense
the tall tree with a heavy trunk is native to the Indian sub-continent but is also widely found in
various Asian and African countries. The tree bears fruits which are oblong in shape – that are

Page | 20
green when raw but turn pink or purple as they ripen. The outer layer of the fruit appears to be
blackish or dark purplish in color and has a distinct sweet taste with sour and astringent
undertones. [53]

Figure 2.3 flower and fruit of syzygium guineense

The syzygium fruit is small and ovoid in shape, with purple red to black color peel and white
pulp. They belong to the most important group of water-soluble pigments in nature and occur as
glycosides or alkyl glycosides of their respective anthocyanin. The peel of the syzygium
guineense fruit has been revealed to contain a high number of anthocyanins, and therefore is a
potential source of natural colorants for the food industry. The artificial synthesis of
anthocyanin‟s still represents a challenge and is expensive. However, these compounds can be
extracted from vegetal species, especially fruits, where there is high concentration of
anthocyanin.
Natural dye that will be extracted from syzygium guineense fruit has little been reported.
Therefore, the objective of this study will to investigate the extraction of natural dye from
Syzygium guineense fruit using the various methods for cotton fabric. [54]

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2.6.1 Characteristics of syzygium guineense fruit
Syzygium guineense is a nutritious fruit with a variety of uses. The nutritive properties of the
species have been extensively studied, particularly with reference to the pulp and seed. The fruit
is a good source of anthocyanin, iron, pectin, phenols and protein. Fully ripe fruits are eaten fresh
and can be processed into a variety of products like jelly, jam, squash, wine, vinegar and pickles.
Fruit has sub-acid spicy flavour and squash is a very refreshing drink for quenching the thirst in
summer season. Unripe fruit is used for making vinegar. The juice of ripe fruit is used for
preparing sauces as well as beverages. Other constituents of the fruit include resin, albumen,
Gallic acid, essential oil and tannic acids. Explorations carried out, particularly in the eastern
Uttar Pradesh, indicated considerable variability in respect of fruit shape (round, oval, oblong,
perform), fruit base (flat, necked), fruit apex (flat, pointed), skin color (deep purple, purple -pink,
bluish-black, black), flesh color (purple, purple-pink, white), fruit weight (5.77 - 19.73 g), fruit
length (2.06 - 3.81 cm), fruit diameter (1.94 - 2.98 cm), seed weight (0.141 - 1.94 g), seed length
(1.6 - 2.4 cm), seed diameter (0.8 – 1.3 cm), pulp content (54.29 – 85.71 %) , acidity (0.524 -
0.832 %) , moisture (84.5 - 86.4%), total sugars (5.32 - 11.10 %) which need to be characterized
for utilization in crop improvement.
The fruit shape varied from round to oblong and apex of fruits from flat to point. They also
observed great variability in physico-chemical characteristic of fruits, offering possibility of
selecting varieties suitable for fresh market and processing. Small seed size and high pulp
content with better chemical parameters are considered ideal. The fruit is a good source of
carbohydrates, protein, vitamins, anthocyanin, pectin, minerals and tannins. [55]

Page | 22
Table 2 Nutritive value of dokima fruit per 100g of edible portion

Page | 23
Anthocyanidins and anthocyanin are the most highly colored of the flavonoids. They are
responsible for the scarlet, reds, violets and blues in many flowers, fruits and vegetables. When
Anthocyanidins bond to sugar molecules they become anthocyanin.
The peel of the syzygium guineense fruit has been revealed to contain a high number of
anthocyanins, and therefore is a potential source of natural colorants for the food industry. [56]
Anthocyanin is soluble in water and easily extracted into weakly acidic solution. However, the
color is pH dependent.

Figure 2.4 the chemical structures of compounds isolated/detected from Syzygium

guineense

Figure 2.5 Molecular structure of anthocyanin

Page | 24
2.7 Synthetic Dyeing
Synthetic dyes are classified based upon their chemical composition and the method of their
application in the dyeing process. Almost all the synthetic colorants being synthesized from
petrochemical sources through hazardous chemical processes pose threat towards its produce a
wide variety of colors, sometimes causes skin allergy and other harmfulness to human body,
produces toxicity chemical hazards during its synthesis, releases undesirable hazardous toxic
chemicals etc. Like other environmentally damaging dyes, these dyes are made from synthetic
petrochemicals. The process requires very high concentrations of salt (20%-80%) of the weight
of the goods dyed) alkali and water. Even if the unfixed dye is reclaimed, the effluent from this
process can still contain high concentrations of salts, surfactants and defoamers, and is strongly
alkaline as reactive dyes currently make up 50% of world dye consumption, more knowledge on
how to improve upon this method is needed [57].

2.7.1 Synthetic Dyeing and their Influence

Direct dyes: given this name because they color the fibers directly and eliminates the need for a
mordant (the chemical fixing agent lots of dyes need). Azo dyes are a type of direct dye made
from a nitrogen compound; azo dyes are known to give off a range of carcinogenic particles and
have been banned in many places. Effluent contains 5 – 20% of original dyestuff, plus salt and
dye fixing agents [58].
Vat dyes: these dyes need a powerful reducing agent, such as alkali, to make them soluble.
Expensive and complicated to use, effluent contains 5 – 20% of residual dyestuffs, plus reducing
agents, oxidizing agents, detergents and salts.
Sulphur dyes: 90% of all sulphur dyes contain sodium sulphide, which endangers life and alters
DNA, corrodes sewage systems, damages treatment works and leads to high pH and unpleasant
odors. Effluent contains 30 – 40% of the dyestuff plus alkalis and salt.
Reactive dyes: these dyes bond directly with the fibers, rather than merely remaining as an
independent chemical entity within the fiber. Applied with relatively cool water (saving energy)
and of all the classes of synthetic dyes, a subset of reactive dyes (called “low impact fiber
reactive”) seems to be the best environmental choice [58].

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2.8 Literature gap
Ethiopia is reported to have over 6500-7000 plant species of which about 15 % are endemic.
However, the dye-yielding plants in Ethiopia have neither been identified, nor documented
scientifically. In view of the imminent and large biodiversity of the country it is expected that
several plants may have important color constituents for textile coloration. The present study has
Been designed to secure this gap and it is focused on identification of few potential dye plants
through dyeing and testing the color strength, CIE L* a* b* values and fastness properties of
dyed sample using standard methods. Structural identification of the exact nature of the chemical
compounds of dyes, which are responsible for color are beyond the scope of the current study.

Page | 26
 CHATER THREE

METHODOLOGY

3.1 Materials
Substrate: -

Scoured cotton fabric: A commercially prepared and scoured ready- to-dye, plain weave 100 %
cotton fabric of some ends/ inch and picks/ inch was used.

Dye Source: -

Syzygium guineense fruit: this was collected for dyeing of cotton fabric. This fruit were
collected from Bahir Dar capital city of Amhara region.

3.2 Chemicals
Sodium chloride: used to facilitate dye bath exhaustion.

Industrial soap: used for wash fastness test.

Use Sequestering agent (EDTA), water.

Chrome (potassium dichromate): used as a mordant on any fiber and does not change the shades.

3.3 Equipment’s
To carry out the experiment the following equipment‟s used; water bath, grinding machine,
sieve, thermometer, beaker, laundry, stirrer, and measuring cylinders, stove, digital balance,
oven, scissor, filter paper, grey scale (for color fastness rating).

Launder meter, crock meter, and spectrophotometer to check washing fastness, rubbing fastness
and color strength of dyed samples used.

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3.4 Methods
3.4.1 Sample preparation
Syzygium guineense fruit were collected manually from Bahir Dar Ethiopia. The unwanted part
of the fruit will be removed manually. The Syzygium guineense fruit was dried under shade
hidden from direct sunlight (at room temperature) and it was grind by grinder machine and then
the powder can be sieve to separate small particle size of material from large particle of dye
material. The powder is passing through a sieve to obtain uniform particle size of the materials.
The sieved powder is used for dye extraction at different experimental conditions.

Separation of peel from

Finding Syzygium Fruit collection
seed
guineense tree

Grinding and Powder

Sieve the powder Drying the peel
formation

Figure 3.1chart flow method of dye powder preparation

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 Figure 3.2 figure flow method of dye powder preparation

3.4.1 Aqueous extraction of syzygium guineense

Among this extraction method aqueous extraction method is easily apply to extract dye from
syzygium guineense fruit it has advantage over other extraction method, no pollution to the
environment, apply in short period of time (easily apply) and no destroy any color component of
the dye as well as easily capable to perform extraction of the dye from syzygium guineense fruit.

In this method, color containing compound if dry broken down into small pieces or in powdered
form by grinding and soaked with water in vessel for some time to loosen the cell structure.
Coloring component present in syzygium guineense fruit is anthocyanin. If color containing
compound is in wet form, then it is split down to fine pieces or grinded to fine paste. Then these
broken-down pieces are boiled in water to get the coloring component dissolved in water.

During this hot water process the coloring component anthocyanin present in syzygium
guineense liquefied properly in water. This solution is filtered to separate coloring solution and
non-coloring residue by using filter paper. The optimization extraction of natural dye from
syzygium guineense fruit peels were done below. We use 0.3g sequestering agent to reduce
water hardness and use 15g amount of powder syzygium guineense fruit peel were dissolved in
water.

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 Table 3 optimization of dye extraction from syzygium guineense fruit peel

Time (min) Temperature (oc) MLR

Sample 1 90 80 1:20

Sample 2 60 70 1:20

Sample 3 90 70 1:20

Sample 4 120 70 1:20

Sample 5 90 60 1:20

Sample 6 90 70 1:15

Figure 3.3 dye extraction procedure

3.4.2 Dyeing of cotton with syzygium guineense

The extracted solutions of dye will apply to cotton fabric with and without mordant under
identical and different conditions. The concentration of the dye material we use 5g of fabric, use
30% owf of dye solution and 14g/l sodium chloride are used for exhausting agent. The dyeing
process can take in direct dyeing process. We use pre mordanting process and without
mordanting use.

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 Table 4 dyeing optimization for dyeing of cotton with this extracted dye

Sample Time(min) Temperature (oc) MLR PH

five samples from 60 60 1:20 10

each extracted dye
solution

Sample 6 (without 60 60 1:20 10

mordant)

Then the dyeing procedure are:-

After prepared dye solution in beaker the fabric sample immersed in it.

After five minute 1/5th total amount of Nacl added.

After 25 minute 4/5th total amount of Nacl added for exhaustion. After completion of dyeing
time the fabric was wash for 10-minute, temperature 50oc, MLR 1:20 and 2g/l industrial soap
and then drying at room temperature. The dyed samples then dried to be ready for next quality or
performance test.

Figure 3.4 fabric sample dyeing procedure

3.4.3 Mordanting procedures

We use pre-mordanting method: In this method, cotton fabrics were penetrated with the solution
of chemical mordant. It‟s the most common method of mordanting practiced on cotton.

Page | 31
The advantage of this method is that the standing baths can be reused many times after
replenishing with the mordents. This makes the process economical as well as reducing the
pollution load hence sufficient for large- scale application.

We use Chrome (potassium dichromate) type of mordant: It is also referred to as yellow

chromate. It is relatively more expensive it take from chemical department laboratory. The
concentration of mordant material we use 10% owf potassium dichromate, temperature 60oc, at
45 minute and MLR 1:20. The dichromate solution is light sensitive and therefore it changes
color under light exposure.

The procedures for this mordanting are;

i). Dissolve the mordant and added to a dye bath containing 99.5ml of water.
ii). Add the substrate and bring the whole mixture to boil for a period of about ¾ of an hour.
iii). Cool the solution
iv). gently remove the substrate to ensure even take-up of the mordant.
v). Rinse the substrate to remove unfixed dyes, dry under room temperature and analyze. The
fabric can afterwards be dyed.

3.5 Evaluation of syzygium guineense dyed cotton samples

The dyed cotton sample was evaluated in terms of color strength (k/s) measurement, washing
fastness, rubbing fastness.

3.5.1 Color strength

The color depth and richness of the dye was assessed used the reflectance method on a
spectrophotometer data color 850 by reflectance method. The color intensities (K/S) of the cat
ionize samples at different conditions will determine. The reflectance (R) value of dyed fabric at
the maximum wavelength of absorbency (λ max) will find and The Kubelka Munk function
(K/S) defines the depth of color in a diffused spectrum given by K/S = (1-R) 2/2R. Where K is
the light absorption coefficient, S is the light scattering coefficient while, R is the light reflection.

Higher K/S values mean a higher depth of color. The color values of both modified and
unmodified thickeners was compared to each other.

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 Figure 3.5 spectrophotometer data color 850(Color strength tester machine)

3.5.2 Washing fastness

These test can evaluate the dye tend to fade over time and also because of repeated washing. So
it is important to test the fastness of cotton dyed in order to assess the quality of the dye being
used.

Washing fastness of textile refers to the ability of textile to maintain the original color under
washing condition. The washing fastness property was evaluated using method by Launder meter
ISO test method 4 and was compared to grey scale. The resistance to the loss of color of cotton
dyed to wash was preferred to as its wash fastness. The dye molecules have not penetrated inside
the inter polymer chain space of fiber or not attached to the fiber with strong attractive force,
poor washing fastness result.

Figure 3.6 washing fastness test by Launder meter ISO test method 4

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3.5.3 Rubbing fastness
The Dyed samples were subject to both dry and wet rubbing fastness tests on crock meter
machine, & color fading extent were check using gray scale. To assess rubbing fastness the
sample was rub against half bleached fabric at 15 time and check the color is fade on the
bleached fabric to compare with the standard grading scale. Rubbing fastness were test according
to ISO 105 F09 2009 standard. Two specimens was take-one for dry state and one for wet state
for one sample. A rubbing cloth prepares and one rubbing cloth is wet out with water for wet
rubbing.

Procedures of rubbing fastness tests:-

The specimen was mounted on the base board of the crock meter.

Putting the long direction of the specimen parallel to truck of rubbing.

The white rubbing cloth was mounted flat over the end of the peg on the crock-meter and holds it
taught by means of the spring clip provide.

The finger was rest on the specimen ensuring that the spring clip is not in contact with the test
specimen.

The specimen then rub back and forth over a straight truck for some complete cycles at a rate of
second for each cycle.

Finally, the white rubbing test cloth was removed and the degree of stained on the undyed fabric
was evaluated with grey scales.

Figure 3.7 rubbing fastness test

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 CHAPTER FOUR

RESULTS AND DISCUSSION

4.1 Extraction of Colorant

The sieved powder can be measure and dissolved in water and then boiled for 60, 90 and 120
minutes in a hot water bath for quick extraction for 1:20 and 1:15 MLR at a temperature of 60,
70 and 80oc. At the end of each extraction time the total color was extracted. The solution was
then filtered by filter paper and used to carry out the dye.

The amount of color availability determined by drying and measuring residual of color trash to
the original crush color powder. Dye on cotton fabric in appropriate dyeing condition by varying
the amount of dye concentration and the type of mordant.

Optimize dyeing concentration, temperature and dyeing time.

Amount of color available (%) = mass crush powder before - mass residual powder after *100

Mass of crush powder before extraction

Amount of color available (%) = (90g – 87.7g)/90g * 100 = 2.6%

4.2 Washing and rubbing fastness result analysis

The fastness rating goes from 5 to 1:

5: No visual change (Best rating) – Excellent, 4/5: very good to excellent,

4: Very good, 3/4: Good to very good

3: Good 2/3: Fairly good to good

2: Moderate 1/2: Fairly moderate to moderate,

1: Large visual change (Worst rating) –Poor

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 Table 5 washing fastness result analysis

Sample number Washing fastness rate

Sample 1 4

Sample 2 2/3

Sample 3 ¾

Sample 4 ¾

Sample 5 3

Launder meter was adjusted to 60°C and laundering was carried out for 30 minutes with 5g/l
detergent to evaluate the wash fastness of the dyed samples by using greyscale to give the grade
of sample. Washing fastness property of our dyed fabric sample evaluated with in this
temperature is good washing fastness almost take the largest grade one as the temperature
increase because the washing fastness grade were grade 4 at 80oc of extracted dye that indicates
the dye have very good wash fastness.

Table 6 rubbing fastness result analysis

Sample number Rubbing fastness rate

Wet dry

Sample 1 ¾ 4/5

Sample 2 ¾ 4

Sample 3 ¾ 4/5

Sample 4 ¾ 4/5

Sample 5 3 4/5

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When the dyed fabric was mounted on the base board of the crock meter it rubbed with half
bleached fabric. The dyed fabric then rub back and forth over a straight truck for 15 times cycles
and checked the color is fades on the bleached fabric to compare with the standard grading scale.
Due to this except sample 5 all samples were rate 3/4 those, was good to very good grade with in
wet rubbed, but sample 5 was dyed at low temperature it give good wet rubbed.

In dry rubbed all samples were rate 4/5 it yields very good to excellent, except sample 2.

Generally our dyed samples were good in dry rubbing fastness test that means the availability of
taken mordant was good fixation between the dye and the fabric.

4.3 Color strength result analysis

Scoured and 100% cotton fabric was used for this experiment. To do this experimental work we
were optimizing at different temperature and time used.

Table 7 dyed fabric color strength result analysis

Dyed fabric sample Wave Reflectance k/s

length(nm)

Sample 1 390 24.56% 1.16

Sample 2 390 28.33% 0.91

Sample 3 380 27.49% 0.96

Sample 4 390 26.54 1.02

Sample 5 380 27.26% 0.97

In order to find the suitability of the dye extracts for dyeing, cotton fabric was dyed with pre-
mordanting. The K/S values of dyed samples were measured using color eye spectrophotometer
data color 850. The wavelength at which, the highest K/S was recorded. The relative increase in
K/S after pre-mordanting was expressed in terms of the ratio of K/S values of dyed cotton fabric.

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These values were calculated by using Kubelka-Munk equation. This Equation can be
mathematically expressed as K/S = (1-R) 2/2R. K/S value is the ratio of the coefficient of
absorption (K) to that of scattering (S). The maximum dye absorption has been observed deep
shade rather than the other (K/S is 1.16 at wave length 390nm) dye with 10% owf potassium
dichromate for the period of 60 minutes at temperature 65oc and pH 10. From the above table as
the dye concentration increase the color strength was increase in this dye bath.

Figure 4.1 graphical compare of color strength of the dyed sample

Sample 1 sample 2 sample 3 sample 4 sample 5

Figure 4.2 tested sample fabric

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 CHAPTER FIVE

CONCLUSIONS AND RECOMMENDATIONS

Conclusion

Generally extraction of dye from syzygium guineense fruit. This natural dye does not have any
effect on human body. The results obtained from in the form of dyeing which was extracted from
syzygium guineense fruit yellowish color our analysis was to choose proper dyeing recipe for
cotton.

From our research we came to know that the natural dyes along with mordant are giving better
result on 100% cotton fabric for given natural dyes. After optimized extraction, the extract was
filtered, diluted and immediately used for dyeing using pre mordanting. The optimized dyeing
conditions for pre mordanting were;-Temperature 600oc,70oc,80oc, and time 60, 90, 120 minutes,
as on weight of fabric (owf),dye concentration 30% (owf) and concentration of salt as 1.4g with
MLR 1:20.

The main target of this study focus dye ability of natural dye from syzygium guineense fruit. It is
successfully established that natural dyes can dye textiles fabric. Syzygium guineense fruit dye is
highly suitable for dyeing cotton fabric by using chrome as a mordent. Cotton fabric dyed with
syzygium guineense fruit with the help of chrome has excellent wash fastness and rubbing
fastness. These dyes are safe and eco-friendly.

Aqueous extract of natural dye syzygium guineense fruit was dyed on the cotton fabric gives
different shade. The syzygium guineense fruit containing flavonoid as the main colorant species
to produce different shade with mordant salts.

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 Recommendations

The recommendations from this research are; where possible, the textile department was very
lower the availability of testing instrument and other material like fastness testing, lack of
chemical availability like mordents, so textile laboratory should fulfill those equipment and
chemicals. In view of the results of the study of this thesis, the following recommendations are
suggested:

 syzygium guineense plant source for Ethiopia that growths in seasonal time, so we should
scale up those productions at every seasonal condition. I.e the fruit time starts May up to
June.
 There should be given enough awareness about extraction of natural dye and dyeing
method.

Mordants used for this work are chrome. So, one can try with other mordants to get different
color shades.

Investigating functional groups of the dye‟s extract will help to determine more about dyeing
effect.

Determining the property of syzygium guineense fruit will be to know the extraction and dying
condition.

Wash fastness and rubbing fastness used for this work .So, one can try light fastness.

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