WOLLO UNIVERSITY

KOMBOLCHAINSTITUTE OFTECHNOLOGY
FACULITY OF TEXTILE, LEATHER AND FASHION ENGINEERING
Self-extinguishable cellulosic fabric treated by using spinach leave juice to
substitute synthetic flame retardant chemicals.
A final year project submitted to department of textile engineering in partial
fulfillments of the requirements for the degree thesis in textile engineering
BY ID NO
1. DESALE ADINO……...........................0519/08
2. BIHON AMARE ……………….............0400/08
3. TEJE GETANEH …………………….....1546/08
4. DESALEGN BIRHANU………..............0521/08

Advisor name: Prof. Vishnu

KOMBOLCHA, ETHIOPIA
December.2013E.C

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 DECLARATION OF ORIGINALITY
We declare that this work of title “Self-extinguishable cellulosic fabric treated by using costa
plant leaf juice to substitute synthetic flame retardant chemical” is uniquely prepared by us and
submitted to department of textile, leather and fashion engineering wollo university Kombolcha
institute of technology for partial fulfillment for degree thesis in textile engineering is honestly
ours. We also confirm that this is a true copy of my thesis, including any final revisions, as
approved by our thesis committee and the Graduate Studies office.

NO Students Name ID NO Signature

1. Desale Adino……………………0519/08 ……………….
2. Desalegn Birhanu……………….0521/08 ………………..
3. Teje Getaneh……………………1546/08 ………………….
4. Bihon Amare…………………….0400/08 …………………

………………. ………………… ……………

Advisors name [Link] Signature

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 ACKNOWLEDGEMENT
First of all we would like to say thanks to our God for his infinite miracle gifts to us without
asking him and we would like also say thanks to his mother St. Virgin Mariam. Secondly, we
would like to thank the University of Kombolcha for giving us this opportunity to study our
Bachelor’s degree in textile engineering. Then, we would like to express our deepest gratitude to
our respectful Advisor Prof. Vishnu. For his valuable comments and suggestions to work on this
project and also his fatherhood and friendly advice starting from the beginning to the end. Next,
it’s our pleasure to thank to other teachers who showing us all the things that we asked at the
time of done this project.

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 ABSTRACT

Spinach juice extracted from spinach leave is excellent flame retardant of both control and
treated fabrics and has a medium price in the international market, being the best vegetal juice.
Besides the flame retardant characteristics, Spinach leave is equivalent nutrient food. The
recovery of essential spinach juice is the value added product because the quality of the juice is
delay fire accident. A large number of organic and inorganic flame retardant materials
containing phosphorus and non-phosphorus compounds are mostly popular in the textile
industry due to their excellent fire retardant property and wash durability. However, connected
to those above-mentioned popular processes, larger quantity of the toxic formaldehyde based
chemicals and acidic conditions are required and the treated fabric lost his tensile strength later
the treatment. In this project extract of spinach juice was used to finish cellulosic fabric. The
results showed that the spinach juice improves physical properties, washing durability and
basically flame retardant of treated cotton fabrics as compared to the controlled cotton fabrics.

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 TABLE OF CONTENTS

Contents
DECLARATION OF ORIGINALITY ................................................................................... II
ACKNOWLEDGEMENT .................................................................................................... III
LIST OF ABREVATIONS ............................................................................................................ X
Chapter-1......................................................................................................................................... 1
INTRODUCTION .......................................................................................................................... 1
1.1. Theoretical background ....................................................................................................... 1
1.2. Problem Statement of the Study .......................................................................................... 3
1.3. Objective .............................................................................................................................. 4
1.3.1. General Objective ............................................................................................................. 4
1.3.2. Specific objective .......................................................................................................... 4
1.4. Significance of the study...................................................................................................... 4
1.5. Scope of the study ................................................................................................................ 4
Chapter -2........................................................................................................................................ 6
LITERATURE REVIEW ............................................................................................................... 6
2.1. Mechanism of imparting flame retardancy .......................................................................... 7
2.1.1. Testing of the flame retardancy .................................................................................... 9
2.1.2. Spinach leaves (Spinacia Oleracea) .............................................................................. 9
2.1.3. Mordanting for cotton fabrics ..................................................................................... 11
2.1.4. Method of mordanting for cellulosic fabric ................................................................ 12
2.5. Literature gap of the study ............................................................................................. 13
Chapter 3 ....................................................................................................................................... 14
MATERIALS AND EXPERIMENTAL METHODS .................................................................. 14
3.1. Materials ............................................................................................................................ 14
3.1.1. Fabric Materials .......................................................................................................... 14
3.1.2 Mordanting Agents ...................................................................................................... 14
3.2. Equipment ...................................................................................................................... 14
3.3. Process flow chart of spinach juice extraction ................................................................... 15
Diagram 1: Extraction process of spinach juice ....................................................................... 15

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 3.4. Application (treatment/finishing) methods of cotton fabric are:- ...................................... 15
3.2.2. Direct application methods on cotton fabric (fabric and spinach juice only .............. 15
Diagram 2: Treatment methods of cotton fabric with spinach juice ......................................... 15
3.5. Application methods of cotton fabric (spinach juice and mordant or binder) ................... 16
Diagram 3: treatment methods of cotton fabric with (spinach juice and mordant or binder) ... 16
3.6. Method of raw material collation and extraction of spinach juice..................................... 16
3.6.1. Raw material collection .............................................................................................. 16
Figure 1 :Collections of fresh costa plant leaves ...................................................................... 17
3.6.2. Raw material preparation ............................................................................................ 17
Figure 2:Washing fresh costa leaves......................................................................................... 17
3.6.3. Eliminate the prepared leaves moisture ...................................................................... 17
Figure 3:dried the spinach leaves with sunlight ........................................................................ 17
Diagram 4 :Eliminate spinach leaves moisture with oven ........................................................ 18
3.6.4. Remove the stem parts of the leave ............................................................................ 18
Diagram 5 Eliminate spinach leave stem manually .................................................................. 18
Figure 4: Eliminate spinach leave stem manually .................................................................... 18
3.6.5. Size reduction.............................................................................................................. 19
Diagram 6: crushing of pure spinach leave with mechanical disc ............................................ 19
Figure 5:Crushing of pure spinach leaves with mechanical disc .............................................. 19
3.6.6. Squeeze the crushed spinach leave ............................................................................. 19
Diagram 7: squeezing crushed spinach leave manually ........................................................... 19
Figure 6: squeezing the crushed spinach leave manually ......................................................... 20
3.6.7. Formation of spinach juice/solution............................................................................ 20
Diagram 8: filtration of spinach juice filter paper .................................................................... 20
Figure 7 :Filtrations of spinach juice with filter paper ......................................................... 20
3.7. Experimental work of the study ......................................................................................... 21
Table 1: Parameter of the treatments ........................................................................................ 21
Table 2: Mordant and its concentration the treatment .............................................................. 21
3.7.1. Experimental design of the study................................................................................ 21
Table 3: Treat cotton fabrics at different concentration parameter....................................... 22
3.7.2. Experimental work options of the study are ............................................................... 22
Diagram 9: Pre-mordant cellulosic fabric ................................................................................. 23
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 Figure 8: Pre-mordant cellulosic fabric treated with spinach juice .......................................... 23
Diagram11: Pre-mordent cellulosic fabrics with aluminum potassium Sulphate. .................... 24
Diagram14: Treated cellulosic fabric with 2gr citric acid and100ml water. ............................ 25
Diagram15: Half bleached cotton fabric treated with spinach juice. ........................................ 26
Figure 11: Half bleached cotton fabric treated with 4 gm. of citric acid and 100 ml water. .... 27
Diagram17:Treated cellulosic fabric with 120ml spinach juice ............................................... 27
Figure 12:Treated cellulosic fabric with 120ml spinach juice .................................................. 27
Diagram 18 :Treated cellulosic fabric with 60ml spinach juice and 60ml water. .................... 28
Figure 13: Treated cellulosic fabric with 60ml spinach juice and 60ml water. ........................ 28
3.8. Evaluation method of treated and untreated cotton fabrics are.......................................... 28
3.8.1. Methods of flammability tests .................................................................................... 28
Chapter-4....................................................................................................................................... 31
RESULTS AND DISCUSSION ................................................................................................... 31
[Link] of the study ............................................................................................................. 31
[Link] of the flammability of treated and control cellulosic fabric ...................... 31
Table 4 Treat cotton fabric at different concentration parameter ............................................. 31
4.2. To study the washing durability of treated fabric .............................................................. 32
Table 5: Washing durability of treated fabric ........................................................................... 32
4.2. Discussion of the study ...................................................................................................... 32
Figure 14 Flammability test of the treated fabric...................................................................... 33
Figure 15 Flammability test of control cotton fabric ................................................................ 34
Chapter –5 ..................................................................................................................................... 35
CONCLUSION AND RECOMMENDATION ............................................................................ 35
5.1. Concussion ......................................................................................................................... 35
5.2. Recommendations .............................................................................................................. 35
REFERENCES ............................................................................................................................. 36

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 LIST OF TABLES
Table 1 Parameter of the treatments ............................................................................................. 21
Table 2 Mordant and its concentration the treatment ................................................................... 21
Table 3 Treat cotton fabrics at different concentration parameter ................................................ 22
Table 4 Treat cotton fabric at different concentration parameter ................................................. 31
Table 5 Washing durability of treated fabric ................................................................................ 32

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 LIST OF FIGURES
Figure 1 Collections of fresh costa plant leaves .......................................................................... 17
Figure 2 Washing fresh costa leaves ............................................................................................. 17
Figure 3 dried the spinach leaves with sunlight ............................................................................ 17
Figure 4 Eliminate spinach leave stem manually ......................................................................... 18
Figure 5 Crushing of pure spinach leaves with mechanical disc .................................................. 19
Figure 6 squeezing the crushed spinach leave manually .............................................................. 20
Figure 7 Filtrations of spinach juice with filter paper................................................................... 20
Figure 8Pre-mordant cellulosic fabric treated with spinach juice ................................................ 23
Figure 9 Finish the pre-mordent cellulosic fabric with spinach juice ........................................... 24
Figure 10 Treated cellulosic fabric with 2gr citric acid and100ml water. .................................... 26
Figure 11 Half bleached cotton fabric treated with 4 gm. of citric acid and 100 ml water. ......... 27
Figure 12 Treated cellulosic fabric with 120ml spinach juice ...................................................... 27
Figure 13 Treated cellulosic fabric with 60ml spinach juice and 60ml water. ............................. 28
Figure 14 Flammability test of the treated fabric......................................................................... 33
Figure 15 Flammability test of control cotton fabric ................................................................... 34

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 LIST OF ABREVATIONS

SJ Spinach Juice
GSM Gram per Square Meter
0
C Degree Celsius
OWF on Weight of Fabric
ML Milliliter
MIN Minute
SEC Second
APS Aluminum potassium Sulphate
AA Aluminum acetate
GM Gram
MLR Material liquor ratio
PH Power hydrogen
TP Pyrolysis temperature
TC Combustion temperature
G/L Gram per liter
E.G. Example
CM Centimeter
LOI Limited oxygen index

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 Chapter-1

INTRODUCTION

1.1. Theoretical background

Flame retardant fabric is a fabric that has been treated and/ or holds the natural properties to self
–extinguish when exposed to an ignition source [1].

Inherent and treated are two terms that are used a lot in the flame resistant world. The term
inherently flame resistant fabric is one that is used for fabrics that do not required the addition of
flame retardant chemicals after the yarns have been spun or the fabric has been woven or knitted.
The yarns of these fabric use only fibers that are naturally flame resistant. Commonly no flame
retardant chemicals are added to the yarn or fabric.

Contrasting inherent fabrics, flame resistant treated fabrics (flame retardant fabrics) have the
flame retardant chemicals added to the fabric after it has been woven or knitted. Most of the
chemicals used for fire retardant finishing of cotton textile are synthetic compounds and they are
available in the market. These chemicals have larger quantity of the toxic formaldehyde and
acidic conditions of phosphorus and nitrogen based propane (tetra hydroxyl methyl phosphonium
chloride) and the pyruvate (N, N dimethyl phosphopropionamide) is widely implemented to
prevent and delay the spread of fire. And their application procedures are hazardous, expensive,
lost tensile strength and non-ecofriendly with the environment [2].

Therefore continuous research is going on to reduce the add-on% required for self-
extinguishment. To this end, researchers have used different Nano metal oxide based
formulations of Nano zinc oxide, Nano titanium, Nano aluminum hydrate, carbon Nano tube etc.,
and Researchers have also used different phosphorous based plasma polymerizing gases for
making fire retardant cellulosic material at low add-on%.

However, these applications are costly and the treated fabric showed poor durability to washing
and rubbing. Plasma exposed fire retardant fabric lost its extinguishment potential with time
duration.

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 Consequently fire protection and retardancy of materials have become a serious issue in many
industries. The textile industry is no exception in this matter and there are ranges of requirements
which depend on where the textile material is utilized.

In the technical textile application, fabrics that have good flame resistance properties are mostly
made of synthetic fibers such as glass, carbon and aramids. These high-performance fabrics are
commonly used in special technical requirements and purposes such as materials used in high
load bearing application in building infrastructures, marines and aerospace industries.

At present, spinach is one of the most important and common vegetable in the country. The crop
can be grown throughout the country. It grows wild and also cultivated on a large scale as a field
crop as well as backyard crop in household. Spinach leaves are abundantly available in the
country and it is normally considered as edible material. It is ecofriendly and available from
renewable source. In this work, spinach leaves juice extracted from the costa leaves will used as
flame retardant of cotton fabric and used for all such application areas, who are directly engaged
in oil, gas, and petroleum industries. Because their advantages of comfort, soft-feel, good
moisture management property, eco-friendliness and bio-degradability.

Actually this thesis continued that spinach juice production not only useful on fire retardant but
also has economic significant for country development. Market point flame retardant cellulosic
fabric with phosphorus and nitrogen propane can affect human health and wild life so flame
retardant of cellulosic fabric with spinach leave is a better and feasible one.

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1.2. Problem Statement of the Study

In most cases there is occurrence of fire accident in different work sectors in unexpected time.
During this time if the fabric has no fire resistance treatment that person may be easily exposed
to injury. This leads people to lost a number of things and affect their morals. Not only this but
also persons, who cannot be expected to respond effectively when they find their cloth catching
on fire, such as children and hospital patients, and for clothing of workers routinely exposed to
heat and fire such as kitchen workers, industry worker fabrics etc. If the fabric was treated before
it can decrease the level of injury. But this treatment was made before by using different
chemicals such as phosphonium chloride salt and N-alkyl phosphopropionamide derivatives are
widely dominating the commercial scenario [3].

However, as such formulations need to be applied in an acidic condition, due to which cotton
fabric loses its tensile strength and becomes stiffer. Besides, such a treatment is expensive and
non-ecofriendly due to the involvement of a large amount of chemicals, high temperature curing
process and the emission of formaldehyde during the treatment if the process has not been
controlled properly, this leads to high effect on the environment due to its acidity which causes
effect on change of environmental conditions.

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1.3. Objective

1.3.1. General Objective

 The general objective of the thesis is the production of flame retardant spinach juice from
spinach leaves to substitute synthetic flame retardant chemicals.

1.3.2. Specific objective

 To study the effect of temperature, time, pH and MLR on the performance of treated
fabric.
 Evaluation of the flammability of treated and control cellulosic fabric.
 Testing of tensile strength of treated cellulosic fabric
 To study the washing durability of treated fabric.
 To study the effect of crossing-linking agent and mordant on durability of the flame
retardant finish.

1.4. Significance of the study

This project focuses on production of spinach juice as substitution of hazardous synthetic flame
retardant chemicals. This spinach juice is essentially used to resist the spread of fire which
affects human and materials like children clothing, hospital patient uniforms, industry worker
dresses, fire fighter uniforms, kitchen wear materials, etc. It is economical due to its easily
availability of raw material and have no residual effect on human health, and environment. This
makes spinach leave the best, reliable substitute to hazardous flame retardant chemicals. Spinach
leave based flame retardant is easy to prepare, cheap and highly effective and thus constitute an
important source of fire retardant for economically poor people.

The chemical constituents are found in the leaves of spinach as vitamin, vitamin C, vitamin K,
and vitamin E as electrolytes, sodium, potassium, as mineral, calcium, copper, iron, magnesium,
manganese, and zinc as energy carbohydrate fat and protein. Due to thus chemicals present in the
juice of the spinach leave cellulosic fabric show fire retardancy.

1.5. Scope of the study

This project deals with an extraction of juice from the spinach leaves in order to resist the
flammability of cotton fabric and enhance washing, rubbing and light fastness oftreated cotton

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fabric that substitute non-ecofriendly fire retardant chemicals such as phosphorous, nitrogen,
halogen in the firm. This natural product contains different chemicals potassium, iron, calcium,
magnesium; zinc, copper etc. are the main components of the juice that serve as durability of
washing and light fastness and delay flame retardancy. This spinach juice is compatible and
ecofriendly with the environment and human health. Finally, this project goes up to characterize
and standardize the treatment effect of spinach juice on cotton fabric and characterize if there is
any changes on the treated cotton fabric.

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 Chapter -2

LITERATURE REVIEW
Ignitability of the fabric as well as combustibility is the indicators of fabric flammability
characteristics, Kasem and Route (1972).The combustibility of the fabric is stated as the rate at
which the flame (or the afterglow) is able to propagate [4]. Ignition of the fabric is described as a
more complex phenomenon, (Tesoro et al (1976). Ignition involves the transfer of heat with
‘thermal decomposition governed by fluid mechanics and chemical kinetics [5] . The burning
process of textiles as stated, (Reeves, Drake and Perkins (1974) involves the release of heat,
decomposition of the material, combustion and propagation of the flame.

The decomposition of the material is explained as the breakdown of the hydrogen bonds that
make up the composition of the fabric. The Flame proofing of Textiles (2000) explains that the
fabric is broken down into gaseous, liquid and solid composites, which further fuel, the
combustion process, (Professor Pail Thorpe). His theory is in agreement with Lewin (1985) who
provides a diagrammatical representation of the burning process. When discussing the
combustion process, (Perkins et al 1974) includes the notion of flaming, glowing and
smoldering. Glowing is explained as the release of radiant heat and the existence of a
luminescence without the flame. The reaction is exothermic and occurs in conditions of high
oxygen levels. The slow suppressed exothermic reaction, termed smoldering, occurs beneath the
surface of the fabric at low oxygen levels [6].

Flammability of textiles is a measurement of the ease with which fabric can be ignited and how
effectively it burns. Kasem and Route profess, that ignitability of the fabric as well as
combustibility are the indicators of fabric flammability characteristics. The combustibility of the
fabric is stated at the rate at which the flame (or the afterglow) is able to propagate. Backer eta.
Described ignition of the fabric is as a more complex phenomenon. The earliest attempts at
making fabric fire resistant were in 1632 when it was suggested that fireproofing the textiles
would reduce fire risks in theaters. The first materials used in this process were clay and plaster
of Paris. The 18th century saw the inclusion of alum and ammonium phosphate in the attempts at
making fabrics fire retardant. In 1820, chemist Gay-Lussac conducted the first serious
experimentation into making fabrics flame retardant. Gay-Lussac determined that there were two

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types of salts capable of making fabrics somewhat flame resistant. The first salt was low melting
and able to form a glassy layer over fabrics and the second broke down into a non-flammable
vapor when it was heated. By the early 20th century other chemists further perfected Gay-
Lussac’s method by incorporating stannic oxide into fabrics to make them flame retardant[7].The
Flammable Fabrics Act of 1953 brought about a change in how clothing was manufactured and
sold commercially. As a result of this legislation, clothing could no longer be made out of
dangerously flammable textiles. In order for a textile to be made into clothing it needed to pass
Consumer Product Safety Commission tests before it could be sold. Special regulations have
been created to ensure that children’s sleepwear is made of flame retardant fabrics.

As the use of synthetic fibers in textiles became dominant, cotton producers were forced to find a
new method of promoting their product. The Army’s Quartermaster Corps' search for flame
retardant uniforms brought about further research into flame resistant clothing. The advancing
technologies of the 20th century allowed scientists to begin the process of chemically modifying
the cellulose molecules with flame retardants both on the surface and within the cotton fiber. In
order to make this process commercially viable, the scientists had to find a chemical combination
that maintained the cotton’s strength and durability without being too expensive [8].

2.1. Mechanism of imparting flame retardancy

The decomposition of materials due to fire is called Pyrolysis. All textile fibers in their natural
form are inherently fire retardants. Almost all known fibers have high flash point or melting
point. However, when the surrounding temperature reaches above the flash point temperature of
fibers, they catch fire. Cellulose like cotton is solid and has appreciably low vapor pressure. They
do not burn, but decomposes into flammable fragments, which generate heat. This heat further
decomposes the cellulose to carry on the decomposition process. Thermal decomposition of
cellulose leads to the formation of products like liquids, tar and solid materials. Bond rupture,
bond reformation, volatilization and many exothermic reactions occur simultaneously. Catching
of fire and its progress in textiles is mainly due to the formation of various gases and liquids
during burning of fiber [9].

Carbon and oxygen react to form carbon monoxide (CO). It is an exothermic reaction and energy
liberated is 26.4 kcal. The char becomes ash in afterglow process by conversion of CO to C02 in

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presence of excess oxygen. This reaction is also an exothermic reaction and the energy involved
[8].

In order to understand the mechanisms of effective flame retardants better, the mechanism of
combustion should first be clarified. Combustion is an exothermic process that requires three
components, heat, oxygen and a suitable fuel.

When heat is applied, the fiber temperature increases until the pyrolysis temperature, Tp, is
reached. At this temperature, the fiber undergoes irreversible chemical changes, producing non-
flammable gases (carbon dioxide, water vapor and the higher oxides of nitrogen and sulfur),
carbonaceous char, tars (liquid condensates) and flammable gases (carbon monoxide, hydrogen
and many ox disable organic molecules).

Eventually, the combustion temperature, Tc, is achieved. At this point, the flammable gases
combine with oxygen in the process called combustion. The heat generated by the combustion
process provides the additional thermal energy needed to continue the pyrolysis of the fiber,
thereby supplying more flammable gases for combustion and perpetuating the reaction. The
burning behavior of textiles is determined more by the speed or rate of heat release than by the
amount of this heat [10].

Attempts to disrupt this cycle for textile substrates have focused on several approaches, such as:-

First method: To provide a heat sink on or in the fiber by use of materials that thermally
decomposes through strongly endothermic reactions. If enough heat can be absorbed by these
reactions, the pyrolysis temperature of the fiber is not reached and no combustion takes place.
Examples of this method are the use of Aluminum hydroxide or ‘alumina rehydrates’ and
calcium carbonate as fillers in polymers and coatings.

Second method: To apply a material that forms an insulating layer around the fiber at
temperatures below the fiber pyrolysis temperature. Boric acid and its hydrated salts function in
this capacity. When heated, these low melting compounds release water vapor and produce a
foamed glassy surface on the fiber, insulating the fiber from the applied heat and oxygen.

Third method: To achieve flame retardancy is to influence the pyrolysis reaction to produce less
flammable volatiles and more residual char. This ‘condensed phase’ mechanism can be seen in
the action of phosphorous-containing flame retardants which, after having produced phosphoric

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acid through thermal decomposition, crosslink with hydroxyl-containing polymers thereby
altering the pyrolysis to yield less flammable by-products.

Fourth method: To preventing combustion is to interfere with the free radical reactions that
provide the heat needed for the process to continue. Materials that act in this ‘gas phase’
mechanism include halogen containing compounds which, during combustion, yield hydrogen
halides that form relatively long lived, less reactive free radicals, effectively reducing the heat
available for perpetuating the combustion cycle, and which decrease the oxygen content by flame
gas dilution.

2.1.1. Testing of the flame retardancy

It is generally understood that flammable fabrics are those fabrics, which ignite when subjected
to a small flame for durations of up to 12 seconds. Most of the work on flammable fabrics is
therefore concerned and directed towards the observation and measurement of ease of ignition,
the rate and extent of flame spread, the duration of flaming and measurement of heat release and
heat of combustion [11].

2.1.2. Spinach leaves (Spinacia Oleracea)

100 g of farm fresh spinach has 47% of daily recommended levels of vitamin-C. Vitamin-C is a
powerful antioxidant, which helps the body develop resistance against infectious agents and
scavenge harmful oxygen-free radicals.

Its leaves also contain a good amount of minerals like potassium, manganese, magnesium,
copper and zinc. Potassium is an important component of cell and body fluids that helps
controlling heart rate and blood pressure. The human body uses manganese and copper as a co-
factor for the antioxidant enzyme, superoxide dismutase. Copper is also required for the
production of red blood cells. Zinc is a co-factor for many enzymes that regulate growth and
development, digestion and nucleic acid synthesis. Spinach is made up of 91.4% water, 3.6%
carbs, 2.9% protein, and 0% fat.

Spinach is one of the best sources of potassium [12].Fresh 100 g of spinach contains about 25%
of daily intake of iron, one of the highest for any green leafy vegetables. Iron is an essential trace
element required by the human body for red blood cell production and as a co-factor for an
oxidation-reduction enzyme, cytochrome oxidase during the cellular metabolism. Spinach leaves

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are an excellent source of vitamin-K. 100 g of fresh greens provides 402% of daily vitamin-K
requirements. Vitamin-K plays a vital role in strengthening the bone mass by promoting
osteoplastic activity in the bones. Additionally, it also has an established role in patients
with Alzheimer's disease by limiting neuronal damage in the brain.

Spinach is also effective in treating burns. For this purpose, it’s recommended to use a special
spinach paste, which can be prepared by boiling spinach leaves in olive oil. The resulting mix is
applied to the burned areas.

Mordant

Natural dyes also define as mordant dyes; do not readily adhere to cotton so mordant are used.
Mordanting or fixing agents have been used since antiquity in dyeing both cellulose and protein
Fibers, resulting in greater depth of shade and colorfastness (Cardon, 2007; Cassel man, 1993).

Chemically, mordant are defined as polyvalent metallic compounds that can form coordinate and
covalent complexes with certain dyes and fibers (Baker, 1958). Thus, the metal atom typically
forms both a covalent bond with hydroxyl (or carboxyl) oxygen on the dye (or fiber) and a
coordinate bond with an adjacent lone pair of electrons on double bonded oxygen. Mordents can
chelate several dye molecules together to create a larger complex and provide a link between the
dye and fiber. These complexes help the fiber retain color, thus increasing depth of shade and
fastness to wet and mechanical treatments (Gordon & Gregory, 1983). However, mordents also
can influence light fastness.

Most mordanting agents are metallic salts of chromium, tin, iron, copper, and aluminum, Copper
and chromium containing compounds (e.g., copper sulfate and potassium dichromate) were
widely used as mordents, but their usage has declined because of toxicity concerns. Likewise,
iron and tin mordents (e.g., iron sulfate and tin chloride) can affect the color and tactile qualities
of the dyed textile. Aluminum mordanting agents are commonly used and considered among the
safest in the application of natural dyes to cellulosic textiles.

Aluminum Mordant

Aluminum is the most abundant of the earth’s metals and is a constituent of most silicon-
containing soils and rocks, such as clay, feldspar, and bauxite. Various aluminum compounds
(e.g., APS, AA, aluminum sulfate, and aluminum hydroxide) have been used as mordents in
textile dyeing throughout history (Liles, 1990; Wipplinger, 2004). Aluminum ions have a strong

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affinity for both cellulose and protein fibers and readily serve as a bridge between multiple dye
molecules and/or between the fiber and dye.

Aluminum potassium sulfate.

Since antiquity, APS (AlK (SO4)2, also referred to as alum, potassium alum, potash alum, or
potassium aluminum sulfate, has been used in textile dyeing. APS is a mineral salt historically
obtained from natural deposits of aluminous rocks (e.g., slate and shale) (Cardon, 2007). Today,
it is made by the refinement of bauxite, an unprocessed form of aluminum ore (Burgess,
2011).Improve colorfastness to laundering and light of fastness on cotton print cloth.

Aluminum acetate mordant-

Improved the colorfastness to laundering and resulted in slightly lower fastness to light

2.1.3. Mordanting for cotton fabrics

The renewed interest in natural dyes, especially for cellulosic fibers, has been attributed to the
potential health and environmental risks of synthetic dyes, emphasis on 'eco-friendly' textiles,
and developing markets for alternative cellulosic fibers. Because most natural dyes are water-
soluble compounds, except for indigo and other vat dyes, they usually are applied in conjunction
with mordanting agents to increase affinity, substantively and fastness properties. Aluminum
containing mordant agents, aluminum potassium sulfate (APS) and aluminum acetate (AA), is
the most widely used for dyeing cotton with natural dyes. While APS has been used as a mordant
for both protein and cellulosic textiles, AA has been recommended as a better mordant for cotton
Textiles (Brown, de Souza, & Ellis, 2010; Dean, 2009; Liles, 1990; Wipplinger, 2005).
However, no reports were found that compared the aluminum mordant agents for colorfastness
properties. The purpose of this study was to determine if an AA mordanting agent could enhance
the colorfastness to both laundering and light of natural dyes on cotton compared to APS.

Common types of Mordant used for natural dyeing

Metallic mordant are in the form of salt, such as chrome, copper, tin, iron and aluminum.

Organic, inorganic not metal mordant are like tannins, cream of tartar, baking soda and vinegar.

Why use natural dye?

Because they are safe and non‐toxic

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Why use mordant?

Because-The mordant has a chance to “bite” into the fiber,

Addition of a mordant to an appropriate dye solution results in a very sudden, dramatic change in
[Link] to fix the color in dyeing or fabric printing especially for fabrics of plant origin
(cotton)

2.1.4. Method of mordanting for cellulosic fabric

The percentage of chemicals and the weight of the material to be dyed are very important.

In the application of mordant, the concentration, temperature and time are the important
parameters to be maintained.

Mordant and dyes may be applied in three ways.

[Link]. Pre‐mordanting- where the mordant is applied first, followed by dyeing.

[Link]. Post‐mordanting- where the dyeing is done first and then mordanting is carried out.

[Link]. Simultaneous mordanting-where mordant and dye are mixed together and applied
simultaneously.

The effect of mordant on cotton fabric

Treatment of the cotton fabric with mordant shows gradual increase in dye uptake and
enhancement of fastness properties of cotton fabric.

Pre‐mordanting,-

For each of the selected mordents, 2% and 3% of each mordant was dissolved water. The half
bleached cotton sample was heated for 30 minutes at a temperature of 100°C in the mordant
solution. The fabrics were dried without washing. The dried pre-mordant fabrics were then
placed in a juice dye bath, gradually raising the temperature to 100°C and allowed to boil for 60
minutes showed in figure 1. The dyed fabrics were removed and cool washed at 30oC in a 2g/L
detergent solution.

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Simultaneous mordanting

For each of the selected mordents, 2% and 3% of each mordant was dissolved in juice dye bath
solution. The dry half bleached cotton fabric sample was placed in 60 minutes.

The dyed fabrics were removed and cool washed at 300C a 2g/L detergent solution.

Diagram must

Post -mordanting:

The dried bleached cotton fabrics were placed in a juice dye bath, gradually raising the
temperature to 100°C and allowed to boil for 60 minutes. The dyed fabrics were dried. For each
of the selected mordents 2% and 3% of each mordant was dissolved in water the dyed cotton
fabric was mordent in the solution at 1000c for 50 minutes. The dyed fabrics were removed and
cool washed at 30°C in a 2g/L detergent solution.

2.5. Literature gap of the study

As per literature, the application of spinach juice was done on cotton fabric. However the
application of spinach juice in order to increase the durability of the treated fabric was not
mentioned anywhere. So in this work the application of spinach juice along with cross-linking
agent and mordant was carried out in order to increase the durability of the treated fabric.
Treatment of cotton fabric with hazardous chemical can affect human health and wild life so
self-extinguishing cellulosic fabric from spinach leave is a better and feasible one.

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 Chapter 3

MATERIALS AND EXPERIMENTAL METHODS

3.1. Materials

3.1.1. Fabric Materials

The natural spinach leaves needed for the extraction of spinach juice bought from local market
available in Kombolcha.

The plain woven half bleach cotton fabric with 260 GSM was used. The construction of fabric
was 30 EPI (ends/inch), 40 PPI (picks/inch) with 25s warp and 30s weft counts.

3.1.2 Mordanting Agents

[Link]. Aluminum potassium sulfate/potassium Aluminum sulfate

Aluminum potassium sulfate, since antiquity, APS (AlK (SO4)2, also referred to as alum,
potassium alum, potash alum, or potassium aluminum sulfate, has been used for the treatment.
Aluminum ions have a strong affinity for both cellulose and protein fibers and readily serve as a
bridge between multiple dye molecules and/or between the fiber and dye. Aluminum mordanting
agents are commonly used and considered among the safest in the application of natural dyes to
cellulosic textiles.

[Link]. Citric Acid

Citric acid was used as a crosslinking agent. This acid may cross link with spinach juice and the
cotton fabric.

3.2. Equipment
The equipment used during our project is:-Weight balance- for measuring the weight of samples,
Cylinder- for measuring volume of juice. Drying chamber (oven)/temperature-for drying the
treated sample, Magnetic stirrer- for stirring the treated sample, Filter paper- for filter the juice
from its residue, Cutter or blade, -for cutting the required sample, PH meter for measure the

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 acidity and basicity, Dye bath-for dying the required sample with spinach leave, Water bath-for
washing the fresh spinach leave and the treated sample, thermometer for measuring the
temperature of sample during the process.

3.3. Process flow chart of spinach juice extraction

Spinach-purchase Wash with water Remove moisture

from local market from spinach leaves

Squeeze spinach Crushes spinach leave

Got spinach juice Avoid stem
leave by hand with mechanical disc
with foam from spinach
leave

Filter spinach juice with

Spinach juice
filter paper

Diagram 1: Extraction process of spinach juice

3.4. Application (treatment/finishing) methods of cotton fabric are:-

 Direct application and

 Using mordant application methods

3.2.2. Direct application methods on cotton fabric (fabric and spinach juice only)

Without washing
MLR=1:20 Boil in 45min. Dry in 1hr.
Treating chamber
(fabric and juice)

Test flammability of treated

cotton fabric.
Diagram 2: Treatment methods of cotton fabric with spinach juice

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 3.5. Application methods of cotton fabric (spinach juice and mordant or binder)

Treating chamber (fabric MLR 1: 20 Boil in 45 min Dry in 115 Wash with
+juice+binder or mordant) 0
c water

Test flammability
cotton fabric.

Diagram 3: treatment methods of cotton fabric with (spinach juice and mordant or binder)

Optimization parameters
 Temperature
 Time
 Concentration of juice (extract),
 Concentration of mordant.

3.6. Method of raw material collation and extraction of spinach juice

3.6.1. Raw material collection

Fresh spinach leaves were bought from local market. The 260 GSM plain woven half bleach
cotton fabric of 30 EPI (ends/ inch), 40 PPI (picks/inch) with 25s warp and 30s weft counts were
available in our textile LAB was used for the application.

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 Figure 1 :Collections of fresh costa plant leaves

3.6.2. Raw material preparation

The costa leave was separated from natural and add impurities (dust, wax, mote, grass and soils).
Then, it was washed with water to remove other fine impurities present on it.

Figure 2:Washing fresh costa leaves

3.6.3. Eliminate the prepared leaves moisture

The moisture was removed from spinach leaves by drying in sunlight for 25-30min at normal
temperature.

Figure 3:dried the spinach leaves with sunlight

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 Evaporated moisture

Sunlight or Oven Spinach leave without

Moisture spinach
temperature moisture
leave

Diagram 4 :Eliminate spinach leaves moisture with oven

3.6.4. Remove the stem parts of the leave

The stem in fresh spinach leave was eliminated in order to get pure costa leave.

Spinach leave without Eliminate spinach leave stem Costa leave without
moisture manually stem

Diagram 5 Eliminate spinach leave stem manually

Figure 4: Eliminate spinach leave stem manually

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3.6.5. Size reduction
1500gm. spinach leave without stem was crushed using mechanical pressing to increase
extraction process and surface area, due to the surface area increases the product yield (juice).

Pure fresh spinach Mortar crushing Crushed

leaves/1500gr spinach leave

Diagram 6: crushing of pure spinach leave with mechanical disc

Figure 5:Crushing of pure spinach leaves with mechanical disc

3.6.6. Squeeze the crushed spinach leave

The crushed spinach leave was squeezed manually to produce juice/solution.

Crushed spinach Squeeze manually/Hand held Spinach solution or

leaves juice with foam

Diagram 7: squeezing crushed spinach leave manually

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Figure 6: squeezing the crushed spinach leave manually

3.6.7. Formation of spinach juice/solution

2200mlSpinach juice with foam and crushed leave was filtered using dense fabric. Here, about
2065ml clean spinach juice was obtained.

2100ml spinach juice Filtrations of spinach juice 2065ml pure spinach

with foam with filter Fabric paper juice

Diagram 8: filtration of spinach juice filter paper

Figure 7 :Filtrations of spinach juice with filter paper

Raw material collection and extraction of spinach juice from spinach leave are finished. Then the
experimental works are done for the following way.

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3.7. Experimental work of the study

Table 1: Parameter of the treatments

Parameter Values

MLR 1:20

pH 8.6

Temperature 85-900C

Time 30-45min

Table 2: Mordant and its concentration the treatment

Mordents used Concentration (% o.w.f)

Aluminum potassium Sulphate 10 and 20 gm.

Citric acid 2 and 4 gm.

3.7.1. Experimental design of the study

The laboratory experiment was done based on three treatment factors such as concentration of
the juice, temperature, and time.

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 Table 3: Treat cotton fabrics at different concentration parameter
Test Citric AlK Water Juice Treating Time Treating Curing
acid (SO4)2 (ml) (min) temperature temperature
(gm.) (gm.) (0C) (0C)

1 10 - 120 12 920C 1150C

2 20 - 120 13 970C 1150C

3 2 - - 120 12 950C 1350C

4 4 - - 120 10 980C 1350C

5 - - - 120 15 86oC 1000C

6 - - 60 60 16 840C 1000C

3.7.2. Experimental work options of the study are

 Experiment- one
 Experiment- two
 Experiment- three

[Link]. Experiment-one

[Link].[Link]-1

6gm. of half bleached cotton fabric sample was treated with 10gm. of aluminum potassium
Sulphate in 100ml water (i.e. 10%). Treatment was carried out at temperature 950Cfor 12min.
Then this mordant treated 6gm. half bleached pre-mordant cotton fabric sample was treated with
120ml spinach juice at temperature of 97oCfor the time of 14min. Then after spinach juice
treated sample without washing was dried at room temperature and then cured 115oC for 5min.

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Diagram 9: Pre-mordant cellulosic fabric

Figure 8: Pre-mordant cellulosic fabric treated with spinach juice

[Link].2. Option -2
6gm. of half bleached cotton fabric sample was treated with 20gm. of aluminum potassium
Sulphate in 100ml water. For the treatment temperature and treating time was maintained at 970C
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and 13 min respectively. Then, the pre-mordant fabric was treated with 120ml spinach juice with
the treating temperature and time of 950c and 16min respectively. Then after treatment sample
was taken out and cured115oC for 5min.

Diagram11: Pre-mordent cellulosic fabrics with aluminum potassium Sulphate.

Diagram 12: Finish the pre-mordent cellulosic fabric with spinach juice

Figure 9: Finish the pre-mordent cellulosic fabric with spinach juice

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[Link]. Experimental-two

[Link].1. Option -1

6gm. of half bleached cotton fabric was treated with120ml extracted spinach juice and 4gm of
sodium chloride salt at treating temperature and treating times of 950c and 12min. Then sample
was taken out and dried.

The above cotton fabric sample was treated with 2 gm. of citric acid in 100 ml of water for 5 min
at room temperature. Then squeeze, dry and cure it in 1350c for 3 min.

Diagram 13: Post- mordant cellulosic fabric with spinach juice.

Diagram14: Treated cellulosic fabric with 2gr citric acid and100ml water.

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 Figure 10: Treated cellulosic fabric with 2gr citric acid and100ml water.

[Link].2. Option -2

6 gm. of half bleached cotton fabric was treated with120 ml extracted spinach juice and 4 gm. of
sodium chloride salt at treating temperature and treating times of 950c and 12 min. Then sample
was taken out and dried.

The above cotton fabric sample was treated with 4 gm. of citric acid in 100 ml of water for 5 min
at room temperature. Then squeeze, dry and cure it in 1350c for 3 min.

Diagram15: Half bleached cotton fabric treated with spinach juice.

Diagram: 16: half bleached cotton fabrics treated with 4 gm. of citric acid and 100 ml
water.

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Figure 11: Half bleached cotton fabric treated with 4 gm. of citric acid and 100 ml water.

[Link]. Experiment- three

[Link].1. Option-1

6gm of half bleached cotton fabric sample was treated with 120mlof spinach juice. The treated
fabric was dried with 1000c for 4min.

Diagram17:Treated cellulosic fabric with 120ml spinach juice

Figure 12:Treated cellulosic fabric with 120ml spinach juice

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[Link].2. Option-2

6gm. of half bleached cotton fabric sample was treated with 60ml spinach juice and60ml water.
The treated fabric was dried at 1000C for 4 min.

Diagram 18 :Treated cellulosic fabric with 60ml spinach juice and 60ml water.

Figure 13: Treated cellulosic fabric with 60ml spinach juice and 60ml water.

Treatment of half bleaching cotton fabric with the extracted spinach juice, cross-linking agent
and mordant to resist flammability and to enhance durability has done by this way.

3.8. Evaluation method of treated and untreated cotton fabrics are:

3.8.1. Methods of flammability tests

 450c flammability test

 900c/vertical flammability test
 Limited oxygen index(LOI)
 Horizontal flammability test

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[Link]. Evaluation of the flammability of treated and control cellulosic fabric.

In this study, the flammability of the samples is measured by using vertical flammability testing
machine and indicated as burn rate (cm/min). The untreated cotton fabric being pure cellulosic in
nature has a high burn rate of 10.4 and 8.56 cm/min in warp and weft direction, respectively.
However, after application of spinach juice in the cotton samples, the burn rate is found to be
slow significantly. It is observed that the untreated sample ignites rapidly, and burns entirely
with flame within 1min20 seconds. Among the seven different samples, the three different
treated samples S5, S6, and S7, are burnt initially with flame. The sample S3is burnt with
afterglow and the sample S1is partially burnt with afterglow. The samples S4 and S2 area self-
extinguished.

[Link]. to study the washing durability of treated fabric

Among the six treated samples, the treated fabric sample number-2 is the best flame retardant
fabric. In order to determine the durability of the enhanced flame retardant finish on the treated
fabric sample number-2, washing test is carried out with detergent/soap. In this study, hand wash
method is used because (limitation) there was no washing machine in textile LAB. After
washing, the burn rate of the sample fabric is determined.

The results are shown in Table 5. It can be observed that the flame retardant ability of the treated
fabric declines after washing. It may be the fact that the active compounds of spinach juice
molecules are partially removed by washing. It may be unforgettable that the cotton fabric
treated with SJ cannot resist to washing. The test results indicate that the SJ treated fabric can
only be used as temporary flame retardant fabric.

[Link]. To study the effect of mordanting agents on durability of the flame

retardant finished

Mordanting agents have been used since antiquity in dyeing both cellulose and protein fibers.

Mordanting agents like aluminum potassium sulfate in three concentrations (5%, 10%, and 20%
o.w.f) were evaluated for colorfastness to laundering and light of natural dye extracts on cotton
fabric.

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Aluminum containing mordant agents, aluminum potassium sulfate (APS) and aluminum acetate
(AA), is the most widely used for finishing cotton with natural dyes. While APS has been used

As a mordant for both protein and cellulosic textiles, AA has been recommended as a better
mordant for cotton textiles.

Chemically, mordant are defined as polyvalent metallic compounds that can form coordinate and
covalent complexes with certain dyes and fibers.

Mordant can chelate several dye molecules together to create a larger complex and provide a link
between the dye and fiber. These complexes help the fiber retain color, thus increasing depth of
shade and fastness to wet and mechanical treatments. Mordant also can influence light fastness.

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 Chapter-4

RESULTS AND DISCUSSION

Spinach juice extract was applied to the cotton fabric with cross-linking agent and mordant. The
treated fabrics were tested for the flame retardancy. All the tests performed above are described
with their result and at the end of this chapter the results are discussed as result observed.

[Link] of the study

[Link] of the flammability of treated and control cellulosic fabric

Table 4 Treat cotton fabric at different concentration parameter

Test Citri AlK Water Juice Treating Treating Curing Burring time in State of burring
c (SO4) (ml) Time temperature temperatur min
acid 2 (min) (0C) e
(gm. (gm.)
) (0C)
1 10 - 120 12 920C 1150C 1min22sec Extinguishable

2 20 - 120 13 970C 1150C 1min35sec Extinguishable

3 2 - - 120 12 950C 1350C 1min22sec Extinguishable

4 4 - - 120 10 980C 1350C 1min11 sec Extinguishable

5 - - - 120 15 86oC 1000C 0min45 sec Burn

6 - - 60 60 16 840C 1000C 0min37sec Burn

7 - - - - - - 0min 28sec Burn

As observed from the result above of table 4the maximum burned time among the treated fabric
is at test number 2 which has 1min 35sec burning time with concentration of 20 gm. APS and
120ml SJ on the 6gm half bleached fabric and the minimum burned time is test number 6. The
average burning time of control fabric is 0 min 28 sec whereas those of the treated fabric are
1min 14sec.

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4.2. To study the washing durability of treated fabric

Table 5: Washing durability of treated fabric

Test Washed Burring time State of

treated in Seconds flammability
fabric in gm.
1 6 51 Burn

2 6 43 Burn

3 6 58 Burn

4 6 48 Burn

Among the six treated samples, the treated fabric sample number-2 in above table 4 is the best
flame retardant fabric. In order to determine the durability of the enhanced flame retardant finish
on the treated fabric sample number-2, washing test is carried out with detergent/soap. In this
study, hand wash method is used because (limitation) there was no washing machine in textile
LAB. After washing, the burn rate of the sample fabric is determined.

The results are shown in Table 4. It can be observed that the flame retardant ability of the treated
fabric declines after washing. It may be the fact that the active compounds of spinach juice
molecules are partially removed by washing. It may be unforgettable that the cotton fabric
treated with SJ cannot resist to washing. The test results indicate that the SJ treated fabric can
only be used as temporary flame retardant fabric.

4.2. Discussion of the study

Under the extraction of the spinach juice the percentage yield was considered the leaf of the plant
to produced optimum amount of juice. The add-on of the treated fabric has a number of factors
but for our case we used half bleach fabric so it has no effect, but it may decrease for finished
fabrics which were treated before by other. The results of the flammability test for both the
control as well as the treated samples were putted below. In case of SJ treated fabric no flame
has been observed. However, afterglow present and propagates slowly at the rate of 33.5mm/min

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and the fabric is burnt. It is also observed that here char mass produced is more blackish and
harder rather than the control fabric, which will be discussed below in coming sub topic of char
analysis. Here, during vertical burning we have recorded the time to burn of treated fabric is
average of 32s. Therefore, it was very much helpful for the users in the real life situation, as they
were get much longer time to escape from the fire hazard-zone or to extinguish the flame if they
wear garment which is treated before. In contrast, the user will be getting hardly any time to
escape from a fire hazard environment with temperature of ~400ºC, if the fabric is not flame
retardant. One disadvantage of this treatment is that, the SJ treated fabric is burnt with afterglow
and it propagates with very slow rate. It limits the application of the treated fabric commercially.
Therefore, for stopping the afterglow, 2-4% citric acid acid is used in the SJ formulation which
can stop the glow and help in enhancing self-extinguishing property of the treated fabric. As a
result, the treated fabric shows the specific char length after vertical

Figure 14 Flammability test of the treated fabric

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 Figure 15 Flammability test of control cotton fabric

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 Chapter –5

CONCLUSION AND RECOMMENDATION

5.1. Concussion

This study has shown the flame retardancy effect of spinach leave juice (SJ) on the cellulosic
cotton textile. The mechanism of imparting the flame retardancy to the cotton fabric by
application of SJ has been supported by mordant and cross-linking agents.

From this study we can conclude that the SJ treated fabrics have good flame retardant properties,
with burning time of average of 1 min 14 sec, showing an increase by round 2.6 times compared
to the control fabric with burning time of average of 28 sec. As a result, the treated fabric does
not catch flame easily and in the vertical flammability test, it burns with an afterglow and a
propagation rate of 33.5 mm/min, which is almost 4 times lower than that observed with the
control fabric. Therefore, the application of SJ in cotton textile for coloration as well as
functionalization is an attractive proposition for value-addition to textiles using natural products.

5.2. Recommendations
Application of spinach juice produced little colour on the treated fabric. So this application may
be used for medium to darker shades. Cross-linking agent increase the durability of the flame
retardant properties. Other researches can work on more cross linking agents and mordant go get
the desired effect. The researchers who want to do further on this may use natural mordant.
After finishing the color of treated cotton fabric is green, therefore further researches may be
done to remove the coloring part of juice.

After washing the flame retardant durability of treated cotton fabric is decline, so further
researches may be done to enhanceflame retardant durability of treated cotton fabric after
washing.

There are different species of the plant costa (spinach) those have different concentration of
phosphates and nitrates, therefore researchers may use different species from different areas to
get better result especially those from desert results and matured spinach.

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[Link], C.Q. and Qiu, X., 2007. The Use of a Hydroxy- Functional Organophosphorus
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