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BAHIR DAR UNIVERSITY

ETHIOPIAN INSTITUTE OF TEXTILE AND FASHION TECHNOLOGY

Final Thesis document

One bath one step dyeing of polyester/cotton blend with disperse/vat dye
combination at low temperature using carrier: effect of carrier on cross staining

By: Mekides Mastewal

Masters of Science in Textile Chemistry


Under the guidance of

Tamene Wagaw (Assist. Prof.)

Bahir Dar University


Bahir Dar, Ethiopia
June, 2021
One bath one step dyeing of polyester/cotton blend with disperse/vat
dye combination at low temperature using carrier: effect of carrier on
cross staining
By
Mekides Mastewal
A Thesis Submitted to the Ethiopian Institute of Textile and
Fashion Technology in Partial Fulfillment of the
Requirements for the Degree of Master of Science in Textile
Chemistry
Under the Supervision of
Tamene. W (Assistant professor)
Ethiopian Institute of Textile and Fashion Technology
Bahir Dar University
Bahir Dar
July 2021

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APPROVAL PAGE

I certify that I have supervised / read this study and that in my opinion it conforms
to acceptable standards of scholarly presentation and is fully adequate, in quality and
scope, as a thesis for the fulfillment of the requirements for the degree of MSc.
..................................... .............................. .............................
Supervisor Academic Rank Signature
....................................... ................................... ...............................
External Examiner Academic Rank Signature

.......................................... ................................... ...........................


Internal Examiner Chairman Academic Rank Signature

This thesis was submitted to the Ethiopian Institute of Textile and Fashion Technology,
Bahir Dar University and is accepted as fulfilment of the requirements for the degree of
Masters of Science in Textile Chemistry.

_______________________ ______________ ___________


Postgraduate Studies Director Academic Rank Signature

_______________________ _______________ __________

Scientific Director Academic Rank Signature

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DECLARATION
I hereby declare that the thesis is submitted in fulfillment of the Masters degree is my
own work and that all contributions from any other persons or sources are properly and
duly cited. I further declare that the material has not been submitted either in whole or in
part, for a degree at this or any other university. In making this declaration, I understand
and acknowledge any breaches in this declaration constitute academic misconduct,
which may result in my expulsion from the program and/or exclusion from the award of
the degree.

Name: …………………………………………………………….

Signature: ………………………………………………..

Date: ………………………………………………………………

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Copyright by
© Ethiopian Institute of Textile and Fashion Technology (EiTEX), Bahir Dar
University (BDU) Year 2020.

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ADVISOR APPROVAL

This is to certify that the thesis entitled “One bath one step dyeing of polyester/cotton
blend with disperse/vat dye combination at low temperature using carrier: effect of
carrier on cross staining” submitted in partial fulfillment of the requirements for the
degree of Master's with specialization in Textile Chemistry, the Postgraduate Studies
Program of the Ethiopian Institute of Textile and Fashion Technology, and has been
carried out by Mekides Mastewal ID.No BDU1207585, under my supervision. Therefore,
I recommend that the student has fulfilled the requirements and hence hereby can
submit the thesis to the Institute.

____________________ ____________ ________


Name of major advisor Signature Date

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EXAMINER’S APPROVAL SHEET-I

ETHIOPIAN INSTITUTE OF TEXTILE AND FASHION TECHNOLOGY


(EiTEX)

POSTGRADUATE STUDIES AND PROJECT DEVELOPMENT OFFICE


We, the undersigned, members of the Board of Examiners of the final open defense by
Mekides Mastewal have read and evaluated her thesis entitled “One bath one step
dyeing of polyester/cotton blend with disperse/vat dye combination at low temperature
using carrier: effect of carrier on cross staining”, and examined the candidate. This is
therefore, to certify that the thesis has been accepted in partial fulfillment of the
requirements for the degree of Masters in Science.

______________________ ____________ ____________


Name of the Chairperson Signature Date

______________________ ____________ ____________


Name of Internal Examiner Signature Date

______________________ ____________ ____________


Name of External examiner Signature Date

______________________ ____________ ____________


Postgraduate Studies Director Signature Date

Final approval and acceptance of the thesis is contingent upon the submission of
the final copy of the thesis to the Post Graduate Studies office.

Stamp of Postgraduate Studies Director Date: ____________

Remark
o Use this form to submit the thesis with minor correction suggested by the examining
board

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EXAMINER’S APPROVAL SHEET-II

ETHIOPIAN INSTITUTE OF TEXTILE AND FASHION TECHNOLOGY


(EiTEX)
POSTGRADUATE STUDIES AND PROJECT DEVELOPMENT OFFICE

As members of the Board of examiners of the final Doctoral/Master's degree open


defense, we certify that we have read and evaluated the thesis prepared by
Mekides Mastewal under the title “One bath one step dyeing of polyester/cotton blend
with disperse/vat dye combination at low temperature using carrier: effect of carrier on
cross staining” and recommend that it be accepted as fulfilling the thesis requirement for
the degree of Masters of Science in Textile Engineering with specialization in Textile
Chemistry.

___________ ____________ ____________


Name of the Chairperson Signature Date

____________ ____________ ____________

Name of Internal Examiner Signature Date

____________ ____________ ____________

Name of External Examiner Signature Date

Final approval and acceptance of the thesis is contingent upon the submission of
the final copy of the thesis to the Postgraduate studies office. Thesis approved by
____________ ____________ ____________

Postgraduate studies office Signature Date

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ACKNOWLEDGEMENTS
I would like to thanks first and foremost to my almighty and ever living God for helping in

the whole journey of my life and also thanks to Holly Virgin Mary and His saints too, for

helping during my hard times. Secondly, I would like to express sincere thanks and

gratitude to my thesis advisor Mr.Tamen W (assistant professor) for his guidance,

critical approach, comments, and support, as well as creating a positive atmosphere

throughout my thesis work. I would like to also express my gratitude to Dr. Abera.K, and

Dr. Molla T. for their encouragement and a critical approach towards various

standpoints for my work.

I am particularly grateful for all EiTEX textile chemical processing technical assistances

concerning their support and positive feelings to my questions and laboratory equipment

operations. I would like to thank all who responded to giving materials and other

necessary data’s, which helped in my study. The last I am gratitude to my best friend

Meseret Fatahun, she help me during over all of this research work and all my families

for their never-ending love, good wishes, prayer and moral support. Finally I would like

to thank all persons whom I did not mentioned their name here but who helped me in

any sort towards completing this research work in this way.

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Abstract

Polyester/Cotton blended fabrics are normally dyed by two-bath or one-bath two-step


dyeing method. Usually one -bath dyeing process using disperses and vat dyes at high
temperature and high pressure were employed for the dyeing of polyester/cotton
blends. The cost and energy consumption are quite higher than the one-step or single
bath dyeing at low temperature with carrier methods. In this study, one-bath dyeing
process using disperses and vat dyes at low temperature by using carrier. Polyester
and cotton fabric was carried out in vat and disperse dye bath separately with identical
conditions. The effect of each dyeing parameters (carrier concentration, temperature
and time) on color strength of dyed fabric and color staining of contrary has been
investigated by measuring colo3333333r strength (k/s) value. Carrier concentration and
time have positive effect on color strength and color staining of both polyester and
cotton fabrics. However temperature has positive effect on color strength of both fabric
but it has negative effect on cross staining. The optimum dyeing parameters to dye
polyester and cotton fabric in one bath one step at low temperature were, 5 gpl carrier
concentration, 100oc temperature and 120 min time. The color strength and fastness
properties to washing, light and rubbing as well as hot pressing of dyed fabrics, which
dyed in both one bath one step at low temperature and in HTHP, were evaluated. The
all over color fastness grade of both method have almost similar, ( i.e. the value were
between 4-5 and 5 and light fastness, 7-8 ). The color strength (k/s value) of one bath
at HTHP has a little bite greater than one bath at low temperature.

Keywords: Polyester/cotton blend, One-bath one-step dyeing, carrier, Disperse/vat


dye, low-temperature dyeing, color strength and color staining

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Table of Contents

Approval page.....................................................................................................................i

List of tables.......................................................................................................................v

List of figures.....................................................................................................................vi

List of acronyms...............................................................................................................vii

CHAPTER ONE: I NTRODUCTION..................................................................................1

1.1. Back Ground of The Study...................................................................................1

1.2. Statement of Problem...........................................................................................3

1.3. Objective..................................................................................................................3

1.3.1. Main objective................................................................................................3

1.3.2. Specific objective...........................................................................................4

1.4. Benefits and Beneficiary of the Thesis.................................................................4

1.4.1. Benefits..........................................................................................................4

1.4.2. Beneficiary of the thesis.................................................................................4

1.5. Scope of the Study...............................................................................................4

CHAPTER TWO: LITERATURE REVIE............................................................................5

2.1. Polyester/ Cotton Blended Fabric........................................................................5

2.1.1. Dyeing of polyester/cotton blend...................................................................6

2.1.2. Types of dye combination for dyeing polyester/cotton blend........................7

2.2. Dyeing Methods of Polyester/Cotton Blends.....................................................10

2.2.1. Continuous dyeing of polyester/cotton blends.............................................10

2.2.2. Semi-continuous dyeing polyester/cellulosic blends...................................11

2.2.3. kBatch dyeing methods of polyester/cotton blends.....................................11

2.3. New Approaches of Dyeing of P/C Blend Fabric...............................................14

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2.3.1. Dyeing of p/c blend with reactive disperse dyes in supercritical carbon
oxide………………………………………………………………………………………..14

2.3.2. Dyeing of 80: 20 P/C blend by using azeotropic solvent.............................15

2.4. Literature Gap.....................................................................................................15

CHAPTER THREE: MATERIALS AND METHODS........................................................17

3.1. Material and chemicals.......................................................................................17

3.1.1. Fabrics.........................................................................................................17

3.1.2. Chemicals and reagents..............................................................................17

3.1.3. Machines and instruments...........................................................................17

3.2. Methods..............................................................................................................18

3.2.2. Dyeing method.............................................................................................21

3.2.3. Dyeing process............................................................................................22

3.2.4. Investigation of carrier effect on cross staining...........................................23

3.3. Data analysis......................................................................................................23

3.4. Quality Assessments Taste................................................................................23

3.4.1. Color strength measurement.......................................................................23

3.4.2. Cross-staining of cotton and polyester........................................................23

3.4.3. Color fastness to washing...........................................................................24

3.4.4. Color fastness to rubbing.............................................................................24

3.4.5. Color Fastness to Perspiration....................................................................24

3.4.6. Color fastness to light..................................................................................24

CHAPTER FOUR: RESULTS AND DISCUSSION.........................................................25

4.1. Analyze the effect of dyeing parameters and their optimization for polyester and
cotton dyeing...................................................................................................................25

4.1.1. Dyeing of polyester and cotton fabric with disperse dye....................................25

4.1.2. Dyeing of polyester and cotton fabric with vat dye.........................................37

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Summery..........................................................................................................................49

Future wokrk....................................................................................................................50

Reference........................................................................................................................51

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List of tables

Table 1: Machines and instruments with their specification............................................17


Table 2; Main dyeing parameters and their factorial level and replica............................19
Table 3: experimental design of dyeing parameters by central composite design.........19
Table 4: Dyeing chemicals and their concentration/amounts.........................................22
Table 5: Quality assessment of dyed fabric....................................................................25
Table 6: Experimental result of polyester and cotton dyeing with disperse dye.............25
Table 7: Fit summary table of color strength of polyester...............................................27
Table 8: ANOVA table for color strength of polyester.....................................................28
Table 9: Fit summary table for color staining of cotton...................................................32
Table 10: ANOVA table of color staining of cotton..........................................................32
Table 11: Experimental result of polyester and cotton dyeing with vat dye....................38
Table 12: Fit summary table for color strength of cotton.................................................39
Table 13: ANOVA table for color strength of cotton........................................................40
Table 14: Fit summary table for color staining of polyester.............................................44
Table 15: ANOVA table for color staining of polyester....................................................44

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List of figures

Figure 1: Dyeing processes of polyester/cotton with disperse and reactive dye..............8


Figure 2: Structure of fluoro-triazinyl reactive disperse dyes [45]...................................15
Figure 3: Normal probability plot for color strength of polyester and color sating of cotton
.........................................................................................................................................27
Figure 4: Effect of carrier concentration on color strength of polyester..........................30
Figure 5: Effect of temperature on color strength of polyester........................................31
Figure 6: Effect of time on color strength of polyester.....................................................32
Figure 7: Interaction effect of carrier concentration and temperature.............................32
Figure 8: Effect carrier concentration on color staining of cotton....................................35
Figure 9: Effect of temperature on color staining of cotton.............................................36
Figure 10: Effect of time on color staining of cotton........................................................36
Figure 11: Interaction effect of carrier concentration and temperature...........................37
Figure 12: Interaction effect of temperature and time on color staining of cotton...........37
Figure 13: Normal probability plot for..............................................................................39
Figure 14: Effect of carrier concentration on color strength of cotton.............................42
Figure 15: Effect of temperature on color strength of cotton...........................................42
Figure 16: Effect of time on color strength cotton............................................................43
Figure 17: The interaction effect of temperature and time on color strength of cotton...44
Figure 18: Effect of temperature on color staining of polyester......................................46
Figure 19: Effect of temperature on color staining of polyester......................................47
Figure 20: Effect of time on color staining of polyester...................................................48
Figure 21: The interaction effect of temperature and time on color staining of polyester.
.........................................................................................................................................48

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List of acronyms

ANOVA Analysis of variance

HTHP High temperature high pressure

M. L. R material to liquor ratio

Min minute

gpl gram per liter

gsm gram per square centimeter

owf On the weight of fabric

P/C polyester/cotton blend

K/s color strength

cm centimeter
o
c degree Celsius

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CHAPTER ONE: I NTRODUCTION

1.1. Back Ground of The Study

Dyeing is the process of apply color to a textile material with some degree of fastness or
permanence. Dyes migrate or diffuse into the chemical molecular structure of textile
fibers in order to develop the final color of the textile product. The dye-fiber molecular
association is also responsible for the degree of fastness or permanence of the color
because of the molecular attraction between the specific dye and the specific textile
fiber.

Natural/synthetic fiber blends are becoming more and more important in the textile
industry. The reason for blending is variable but mostly it is to combine comfort
characteristics of natural fibers and performance characteristics of synthetic fibers in a
single fabric [1]. One of the most important practices in blending is the mixing of cotton
and polyester for the production of polyester/cotton blend fabrics. This blend fabrics are
one of widely used clothing industry due to their complementary properties [2] . In
polyester/cotton fabrics, polyester fibers provide crease recovery, dimensional stability,
abrasion resistance, tensile strength and easy-care properties, while cotton with its
hydrophilicity, ability to transport moisture and its anti-static characteristics contributes
to wearing comfort [3].

However, the dyeing process of Polyester/Cotton blends difficult and possess some
challenges to dyer because two fibers show different characteristics. Cotton fibers show
hydrophilic characteristics (and may easily undergo swelling in water. Owing to this
phenomenon, the dyestuff molecules first adsorbed on the fibre surface may diffuse into
the fibre interior. Subsequently, the bonding interactions between the dyestuff and
cellulose may be formed ([4])

may diffuse into the fiber interior whereas polyester fibers show hydrophobic
characteristics and crystalline structure [5]. Polyester fibers show a hydrophobic
character, and swell to a very small extent in the water bath. Hence, the access of the
dyestuff molecules to the fibers inside is very difficult [6]. This fact, together with an
absence of active chemical groups in polyester's macromolecules makes it impossible

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to apply the majority of dyestuffs apart from disperse dyes ([7]. Due to this it is
impossible to dye polyester cotton blended fabric by using same dye class rather with
different class of dyes. Cotton is usually dyed with both water- soluble dyes like,
reactive, direct, and water-insoluble dyes Sulphur, vat dyes [2]. Vat dyes have better
color value, reproducibility of color and color fastness property than other dye class.
Polyester fibers can be dyed using disperse dyes either high temperature high pressure
method or carrier method. The often applied pressure method requires a suitable,
intricate apparatus which causes great energy consumption [8].

During high temperature high pressure method, polyester dyed with dyeing temperature
from 100 to 130 °C under pressure, this method requires high energy for temperature
and pressure [9]. On the other hand, carrier method is advantageous to dyeing
polyester fibers with disperse dyes at the boil, within a reasonable time, particularly for
medium to deep shades since carries increase both rate of dyeing and the dye bath
exhaustion[10].

During dyeing of polyester/cotton blend, polyester component is invariably dyed first


with a mixture of disperse dyes then cotton component dyed with reactive, direct,
Sulphur, vat, or azoic dyes, which is actual select depending on the desired color, the
type of finishing required, the demanded fastness properties, the costs and the type of
machinery available [11]. Cross-staining of the cotton by disperse dyes can be a
problem. The stained cotton has poor light and washing fastness and the weakly held
disperse dyes will transfer color to other synthetic fibers such as nylon during washing.
For deep shades, alkaline scouring, or preferably reduction clearing with alkaline hydros
and a non-ionic detergent, removes the disperse dyes staining on the cotton [12].

Two-bath dyeing method is a conventional method of exhaust dyeing of polyester/cotton


blend to dye each component separately under its optimum conditions. However, these
dyeing methods are relatively long and complicated. To address the issue several
attempts have been made in the past to shorten this to one-bath processes, for example
Meenal and his coworkers have developed one bath method using physical mixtures of
disperse/reactive dyes. This one bath dyeing method requires shorter time of period and

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less consumption of water compared to conventional two bath method but it uses high
temperature and it takes long time for dyeing relative to one bath one step method [12].

The present work involves a method of one-bath one-step dyeing process of P/C blend
with disperse dye and vat dye at low temperature using carrier and determine the effect
of carrier on fabric cross satin of dye.

1.2. Statement of Problem

In textile industry P/C blends have dominant market share having share of 58% in
worldwide market [12]. This the fabric widely used specially in clothing industry due to
their complementary properties. The presence of both polyester/cotton components in
textile causes difficulties in the dyeing process since two fibers show different
characteristics. Polyester/cotton fabrics need to be dyed in two-bath processes and one
bath using disperse dyes for polyester and other dyes for cotton fiber. Two-bath dyeing
method is relatively long and complicated as well as requires high temperature, time
and energy. One the other hand in one bath dyeing method, it can reduce consumption
of water, energy and dyeing time relative to two bath dyeing method.

Conventionally, one bath dyeing method of polyester/cotton blend with disperses /vat
dye combination carried out at high temperature high pressure process. But this
process requires (expensive machine) long process, high temperature and energy. The
aim of this research to carried out one-bath one-step dyeing of polyester/cotton blend
fabrics with disperse and vat dye at low temperature by using a carrier. This method
would reduce the use of expensive machinery, dyeing temperature and save energy
and also simplifies dyeing process.

1.3. Objective

1.3.1. Main objective

 The main objective of this study is to reduce the dyeing temperature of


polyester /cotton blend for one bath dyeing method with disperse/vat dye by
using carrier.

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1.3.2. Specific objective

 To determine the influence of carrier on cross staining property during one- bath
dyeing of polyester/cotton blend fabric.

 To optimize carrier concentration, temperature and time for dyeing.

 To dye polyester/cotton blends in one bath at low temperature.

 To compare the color strength, and color fastness property of this one bath
dyeing of polyester/cotton blend at low temperature with conventional method.

1.4. Benefits and Beneficiary of the Thesis

1.4.1. Benefits

The benefit of this study is saved energy, dyeing time, chemical and water consumption.
In general, it decreases cost of production and simplify operation complexity.

1.4.2. Beneficiary of the thesis

The first beneficiaries of this work are different textile sector which process polyester
cotton blends. For researchers, to give additional information about dyeing method of
polyester/cotton blend fabric and EiTEX institute it will grow the institute’s research
capacity. Finally, researchers himself is beneficiary from this study of polyester/cotton
blends dyeing of one bath one step dyeing methods with disperse/reactive dye at low
temperature, he will get a lot of knowledge and skill.

1.5. Scope of the Study

This study will focus on one bath dyeing of p/c blend in one bath process by using
disperse/ vat dye at low temperature by different carrier concentration as well as identify
the optimal parameter. Measure and compare color strength and light fastness, washing
fastness and rubbing fastness property of one bath at low temperature dyed sample to
conventional one bath at HTHP dyed sample. The effect of carrier on cross stating on
cotton and polyester fabric will be investigated. Polyester fabric will be dyed with vat dye

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and cotton fabric will be dyed with disperses dye. Both fabrics will be dyed at different
carrier concentrations through the same condition then test cross staining on cotton and
polyester dyed fabric.

CHAPTER TWO: LITERATURE REVIE

2.1. Polyester/ Cotton Blended Fabric

Blending is the combining of different fibers together intimately to achieve a desired


product characteristic. Blended fabrics are created when two or more different kinds of
fibers are mixed together and create a new fabric with unique properties[13]. Increasing
the demand for fiber blending can be discussed in terms of its positive impacts on

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achieving economic advantages through blending of expensive fibers with cheaper ones
and developing novel textile products to meet the demand. Many blends provide fabrics
with superior performance. This is particularly true for materials containing a mixture of
natural and synthetic fibers where the desirable properties of both types of fibers
contribute to the quality [14]. For example, the polyester in a cotton/polyester fabric
improves the tensile strength, abrasion resistance and dimensional stability, while the
cotton provides reduced pilling, good moisture absorbency and wearer comfort. The
polyester also minimizes the loss of tear strength and abrasion resistance.

The major commercial blend, estimated to consume about 15% of world fiber production
is polyester/cotton blend [15]. Polyester/ cotton blended fabric made of both the artificial
polyester and the natural cotton. This blend is perfect for clothing as it brings both
benefits of the two fabrics together. The fabric thus remains lightness and coolness of
the cotton and polyester gives the strength and durability hence this blend enhance
comfortable during wearing [16].

2.1.1. Dyeing of polyester/cotton blend

The dyeing properties of polyester and cotton fibers are quite different and most of the
dyeing methods for their unions involve separate steps for the coloring of the two fibers
[17]. The polyester component is invariably dyed first with a mixture of disperse dyes.
For the cotton, there is a choice of dyes, the actual selection depending on the desired
color, the type of finishing required, the demanded fastness properties, the costs and
the type of machinery available[12]. The cotton is usually dyed with reactive, direct,
Sulphur, vat, or azoic dyes[18].The major areas of concern during polyester/cotton
blends are:[19]

(1) Degree of cross-staining: Although disperse dyes will stain cotton, anionic cotton
dyes usually completely reserve polyester. Disperse dyes selected should be those that
give minimal cotton staining;

(2) Interactions between dyes and auxiliaries when present in the same bath. For
example, many disperse dyes are not stable under alkaline reduction conditions used in
loco vat dyeing [7]. The salt and alkali required for dyeing cotton with reactive dyes

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often have a deleterious effect on dispersing agent for disperse dyes and cause particle
aggregation.

(3) The conditions for fixation or after treatment of one type of dye on the other types
often limit the processing methods that are possible.

In polyester /cotton blend dyeing; here are several possibilities for coloring the different
fibers:
(1) Solid shade dyeing – all the fibers are identically colored;
(2) Reserve dyeing – at least one fiber is undyed and remains white;
(3) Cross-dyeing – the different fibers are dyed different hues;
(4) Tone-in-tone dyeing – the different fibers have the same hue but with different
depths.

2.1.2. Types of dye combination for dyeing polyester/cotton blend

There are four main types of dye combination to dye polyester /cotton blend in different
dyeing method i, e disperse /reactive dye, disperse/vat dye disperse/direct and
disperse/Sulphur dye.

1. Disperse/reactive dye combinations

Reactive dyes are the best choice for coloring the cotton in a blend with polyester to
give bright shades and good washing fastness, despite their greater cost for deep
dyeing [17]. Two bath or single bath method can be followed.

Dyeing of polyester/cotton blends fabric in one-bath one step dyeing process using
physical mixtures of disperse/reactive dyes where investigated, the physical mixture of
dyes showed level dyeing having good fastness properties and offers the option of cost
effective and eco-friendly one-bath dyeing process [12].

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Figure 1: Dyeing processes of polyester/cotton with disperse and reactive dye

The major limitation in this method is long time required for removal of hydrolyzed
reactive dyes from cotton. In addition, color reproducibility cotton fibers are more difficult
and also cross-staining of cotton must be minimal because reduction clearing is
impossible because during reduction clearing of disperse surface stain on the fiber,
reactive dye are not stable [20].

2. Disperse/direct dye combinations

There are two major methods for dyeing cotton/polyester with a combination of direct
and disperse dyes. In the two-bath method, the polyester and cotton are dyed
separately using the appropriate dyes[21]. Disperse dyes are used for the polyester,
dyeing at 130 °C under pressure. For medium and heavy shades, an alkaline reduction
process clear with hydros solution reduces and removes azo and anthraquinone
disperse dyes staining the cotton fibers [22].

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In the rapid one-bath dyeing method, dyeing takes place with a mixture of disperse and
direct dyes at 130 °C. Reduction clearing of any disperse dye staining the cotton
destroys the direct dyes. This process is therefore less suitable for deep shades [23].

3. Disperse/Sulphur dye combinations

Because of the low price of Sulphur dyes, this combination is useful for dyeing deep
shades where the fastness requirements are less demanding. A two-bath dyeing
procedure is common, initially dyeing the polyester with disperse dyes under
pressure[3]. The cotton is dyed in the second bath with the leuco Sulphur dye
maintained in solution with some sodium hydro sulphide rather than sodium sulphide,
which can attack the polyester fiber. The reducing conditions help in clearing disperse
dye from the cotton [24].

4. Disperse/vat dye combinations

Cotton/polyester can be dyed with a mixture of vat and disperse dyes using one -bath
dyeing process. Both types of dyes are added at beginning of dyeing cycle and, after
initial temperature increase, dyeing of polyester is completed at 130 °C. After dyeing at
125–130 °C, cotton is already pre-pigmented with vat dye. The bath is then cooled and
reduction of vat dye carried out at around 60–70 °C by addition of caustic soda and
hydros[3]. The chemicals for vatting do not affect disperse dyes since ionic species do
not penetrate into hydrophobic polyester fibers. Reduction of the vat dye to the
substantive leuco compound for dyeing of the cotton and reductive clearing of
superficial vat and disperse dyes from cotton fiber surfaces occur simultaneously. The
dyeing is then rinsed and the leuco vat dye oxidized then usual soaping follows [20].

By using carrier can reduce dyeing temperature in to boil temperature since it can
reduce the energy consumption. The amount of carrier will vary, depending on the
particular disperse dye, the dyeing conditions and the effectiveness of the particular
carrier employed. It is well within the skill of the art to determine how much carrier is
needed to give the desired yield for a given set of conditions [25]. For high temperature
dyeing a carrier may not be needed or may be used in an amount up to about 5%, e.g.
0.2 to 4% by weight, based on the weight of the substrate. For atmospheric dyeing the

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amount of carrier is normally in the range 3 to 12% by weight, based on the weight of
the substrate being dyed [26].

2.2. Dyeing Methods of Polyester/Cotton Blends

2.2.1. Continuous dyeing of polyester/cotton blends

The continuous dyeing of cellulose and its blends can be carried out by a variety of
methods [27]. The general procedure is to impregnate the fabric, in open width form,
with a solution or dispersion of color usually by means of a padding unit. The
impregnated fabric is then subjected to one or more continuous treatments to fix, to
varying degrees, the applied dyestuffs or other coloration compounds [28]. The
conventional fixation process is normally achieved by either a chemical treatment or an
application of some form of energy or a combination of the two. The classical
continuous dyeing processes have used heat as a source of energy usually in the form
of steam or dry heat [29]

Dyeing polyester/cellulosic woven fabrics is the specific purpose for which the pad dry
thermosol-chemical pad-steam range was designed. Given sufficient yardage of goods,
outstanding results are achieved with vat, sulfur and reactive dyes for the cellulosic
portion of the blends [30].

The most interesting aspect of continuous dyeing is the way in which application
technology has been developed to make life easier for those in the dye house. For
example, vat colors are applied as pigment dispersions along with the disperse dyes in
the first pad. The goods pass through pre drying, drying and then thermo fixation where
some of them inevitably stain the polyester quite heavily [10, 29]. Direct and reactive
dyes which are heat stable are also applied in the first pad. They emerge from the
thermosol section of the dye range dried onto the cellulose but not dyed. They then pick
up salt or alkali plus salt respectively in a low volume pad trough before steaming [31]

In continuous method polyester/cotton blend fabric dyed in one bath one step method
by using the pad-dry-fixation process using dichlorotriazine based reactive dye and

10
compatible disperse dye. In this method trichloroacetic acid used to provide an acidic
and basic medium in dye bath [29, 32, 33].

2.2.2. Semi-continuous dyeing polyester/cellulosic blends

This type of process offers high productivity for batches of material that are larger than
is usual for exhaust dyeing but too small to justify fully continuous operation. Cold pad–
batch dyeing of cotton and cotton in cotton/polyester fabric has been a big success and
is widely practiced in semi-continuous method [19]. This method requires little capital
investment since it requires only a suitable dye pad. Insulated batching trucks or beams,
equipment for washing-off the resultant dyeing’s. At this time, the method has been
found exceedingly valuable for use with fiber reactive dyes, where the goods are
padded with dye and alkali, batched, wrapped in plastic to exclude the possibility of
drying, and neutralization of caustic alkali by CO 2 in the air, and left in a constant
temperature environment until the dye-fiber reaction is judged to be complete. This is
normally about 12 hours but can vary widely [19, 20]

2.2.3. Batch dyeing methods of polyester/cotton blends

Dyeing of polyester is invariably carried out at about 130 °C under pressure or at 100 oC
in the presence of carrier. To minimize staining of cotton by disperse dyes; dyeing
solution is drained at high temperature. Under these conditions, most of unexhausted
disperse dyes are still in solution. Cooling bath before draining tends to cause
precipitation of dyes on fabric[34].

The batch dyeing method of polyester/cotton blend are classified in the following three
groups-

a. Two bath dyeing two-step

b. One bath two step dyeing method

c. One bath one step dyeing

a. Two-bath two-step dyeing method

11
In this method dyes are applied in two steps in two different baths to dye blends made
fibers of different nature and dye each component separately under its optimum
conditions [35]. The polyester component was dyed in the first bath by a general
polyester dyeing method (60 min, 130 oC) and cotton component was dyed in the
second bath by a normal reactive dyeing method (90min, 80 oc). More handling of
material, huge water consumption doubled loading/unloading time and more labor
required for this technique [36].

b. One bath two step dyeing method

During this methods dyes are added to the same bath in subsequent steps material
handling is unusually less, as the blend once loaded remain there till completion of
dyeing for both components; the same bath is used for dyeing both these fibers saving
water and energy[7, 36].

Polyester /cotton blend fabric dyed in one bath two step method by using phthalimide-
based azo disperse dyes and conventional reactive dye. In this method azo disperse
dyes incorporating a phthalimide structure undergo ring opening under relatively mild
alkaline conditions and converted to a water-soluble product and dyes display good
alkali-clearing properties that permits an alkaline treatment to be substituted. It gives
good productivity and allows high levels of wash fastness to be achieved, even in heavy
depths [37].

c. One-bath one-step dyeing of polyester/cotton blends

One-bath one-step dyeing method is a new experience for polyester/cotton blended


fabric. During this method all dyes are added in the same bath in one single step the
methods reduces cost of dyeing drastically due to nearly 50% reduction in use of water,
heat, chemicals, time and manpower [38]. This method offers the option of cost
effective and reduce environmental load. Generally, this process used to shorten the
dyeing process, increase yield and reduce the utility and chemical cost [5].

Recent studies have attempted to several approaches to enhance one bath one step
dyeing method of polyester/cotton blend by modification of either polyester fiber or

12
cotton fiber surface property by using different methods. Polyester/cotton fabric in one-
bath one-step dyeing at low-temperature after b-CD/citric acid (CA) modification of
polyester/cotton fabric with cationic dye. The color strength of the dyed polyester/cotton
fibers after modification enhanced from 0.12 to 4 with a good leveling property with
moderate Color fastness property [2].

One bath method dyeing of polyester/cotton blend fabric with sulphatoethylsulphonyl


disperses/reactive dyes after chitin biopolymer treatment of blends were discussed. In
the order to improve the adhesion of chitin to the surface of polyester/cotton fibers, pre-
treatment in NaOH solutions was performed [39]. The polyester part dyed around 90 oc
for 60-120 minute by using carrier compound and cotton part around 60 oc for 60
minutes. The dyed samples showed good rubbing and washing color fastness
properties within the range of color change but medium wet rubbing fastness[39].
Polyester/cotton blends dyed by direct after pre-treatment with biopolymer chitosan and
corona. After pretreatment the surface of polyester and cotton chemically change which
increase wettability and dye ability of fabric [39, 40].

Dyeing of polyester/cotton blends with disperse dyes was studied using sodium 2- (2, 3-
dibromopropionylamino)-5-(4, 6-dichloro-1, 3, 5-triazinylamino)-benzene sulphonate.
Cotton fabrics Modify by using sodium 2- (2, 3-dibromopropionylamino)-5-(4, 6-dichloro-
1, 3, 5-triazinylamino)-benzene sulphonate at room temperature in alkaline condition
and then dyed with four different disperse dyes containing amino groups. The dyeability
of treated fabrics relatively better than un treated cotton fabric [31].

On the other hand some researchers stated one bath one step dyeing of
polyester/cotton blend fabric in one dye class by synthesized dyes which, could be dye
both polyester and cotton part perfectly [41]. On the other hand one-step bath dyeing of
polyester/cotton blends with azo disperse-reactive dyes synthesized from 2-
aminothiazole derivatives where found to give red color with good depth, brightness and
leveling properties on polyester/cotton blends where studied [42]. Monoazo disperse
reactive dyes synthesized which, containing a vinyl sulphonyl group as the coupling
component. Sulphonyl group are absorbed by polyester as disperse dyes from
dispersions In presence of a carrier and as reactive dyes for cellulosic component under

13
alkaline condition then dyed with four different disperse dyes containing amino groups.
The dyeability of treated fabrics relatively better than un treated cotton fabric.

One-bath one step dyeing of polyester/cotton blend with disperse and reactive dye by
physical mixture of both dye at high temperature (120 oc) where investigated. The
physical mixture of dyes showed level dyeing having good fastness properties and
offers the option of cost effective and eco-friendly relatively two bath method [12].
Polyester-cotton blend textile substrates are also dyed with a disperse dye and a sulfur
dye in the same dye bath at a temperature no higher than 105. Dyeing temperatures
maintained by using variable amount of carrier with different dyeing condition [24] . For
the one-bath-one-stage dyeing process under neutral conditions and at 130 o by using
selected disperse and bis-3- carboxypyridinium-s-triazine reactive dyes have been
studied. This dyeing method suitable only for economic production of pale and medium
depths of shade. [43]

2.3. New Approaches of Dyeing of P/C Blend Fabric-

Several approaches introduced for dyeing of P/C blend fabrics, to simplify and short
dyeing process and to reduce environment load and cost.

2.3.1. Dyeing of p/c blend with reactive disperse dyes in supercritical


carbon oxide.

One-bath method for dyeing of polyester/cotton blends using fluoro-triazinyl reactive


disperse dyes as dyestuff and supercritical carbon dioxide as a solvent at 393 K and
20 MPa was successfully Investigated by shingo and his coworkers. Polyester/cotton
blends were treated by N-methyl-2-pyrrolidinone (NMP) solvent before dyeing with
reactive disperses dyes in supercritical carbon dioxide. Dyeing cotton/polyester blend
fabrics with one bath dyes in this method would reduce the use of expensive machinery,
consumption of water, dyes, chemicals, energy and environmental load[44].

14
Figure 2: Structure of fluoro-triazinyl reactive disperse dyes [45].

2.3.2. Dyeing of 80: 20 P/C blend by using azeotropic solvent.

For one bath dyeing of 80: 20 polyester/cotton blend fabric by using disperse and
reactive dyes, polyester/cotton blend fabric was treating with azeotropic ternary mixture
of organic solvents before dying. The solvent treatment has disturbed the crystalline
distribution probably by creating more cavity and pores resulting in opening up of the
structured assembly. The improvement in the dye uptake of solvent-treated fabrics is
due to large increase in intersurface area by swelling and greater segmental mobility of
polymer molecules. The dyeing process of this fabric carried out at low temperature (80-
110oc) for 30-60 minute. The color fastness property improved due to dye-fiber bond
formation. But as treating time increase abrasion resistance decrease and weight loss
increase[46].

2.4. Literature Gap

Some researchers are being performed on one bath dyeing of polyester/cotton blends
by using different dyes class at acidic or neutral conditions, and under different
conditions of temperature. One step dyeing of polyester/cotton blends dyes has an
advantage over the traditional dyeing process by reducing the dyeing cycle time and
utility cost [36, 47].

One-bath-one-stage dyeing process under neutral conditions and at 130 oC, selected
disperse and bis-3- carboxypyridinium-s-triazine reactive dyes. It shown that poor color
yield and color fastness property[47].

Developed new dyeing method, to dyeing of polyester/cotton blends fabric using


disperse and reactive dyes by pretreating the blend fabric with non-aqueous azeotropic

15
solvent mixtures can reduce dyeing temperature but the pretreating process increase
operation time and add additional work for dyers [46].

One-bath dyeing of polyester/cotton blends with reactive disperse dyes in supercritical


carbon dioxide also developed its new innovation technology and water free dyeing
methods. But this method is very expensive and the color fastness of dyed fabrics is
almost satisfactory, but color fastness becomes poor with a decrease in the dyeing
temperature. This method is sensitive to temperature and difficult to control and also it
requires high technology. And also scCO 2 is not suitable for cotton so far without
surface modification or treatment [44].

Polyester/cotton blends could dyed with one dye class by synthesis dyes which, used to
dye both fabric part. But synthesis of those dyes are complicated and not economical
since /their chemicals and intermediates, which, are used to synthesis those dyes are
very expansive and not easily/found in any market [44, 48]. And also, polyester/cotton
blends to dye with the one bath dyeing method using vat and disperse dye
combinations at high temperature high pressure. However, this dyeing method uses
expensive machine since small company’s which are manufacture polyester/cotton
bland cannot dyed with this method and also this method required high energy. To fill
the gap this research will be done on one bath dyeing of polyester/cotton blend at low
temperature by using disperse and vat dye.

16
CHAPTER THREE: MATERIALS AND METHODS

3.1. Material and chemicals


3.1.1. Fabrics
In this study, half bleached and scoured cotton and polyester fabric sample were used.
The structures of both fabrics structures are plain. Cotton fabric which has 27 ends per
centimeter and 20 picks per centimeter with 148 gsm taken from EiTEX chemical
processing lab. Polyester fabric also has 37 ends per centimeter and 19 picks per
centimeter with 209 gsm was bought from market.

3.1.2. Chemicals and reagents

All necessary chemicals and reagents which were used for this study were found in
EiTEX chemical processing laboratory. Reagent quality of sodium hydroxide (99
%),sodium hydro sulphate (hydros), carrier, acetic acid (99.5) and standard soap. Red
vat dye (indanthrene normal) and blue disperse dye were used for dyeing.

3.1.3. Machines and instruments

Some instruments and equipment also used all of the Materials and equipments are
found in EiTEX chemical processing laboratory. Some of them are, measuring cylinder,
beakers, weight balance, pipette, stirrers, spoons, grey scale, blue scale and thermo
meter. The rest machines and instruments were listed in table 1.

Table 1: Machines and instruments with their specification

N Machines and Uses Brand model Location


o instruments
1 Reflectance To Measure color eye 3100 EiTEX
spectrophotometer k/s of dyed
sample
2 Landor- o- meters For dyeing and MESDAN/ AUTOWASH
wash fastens Italy
test
3 High temperature To dyeing MESDAN/ ROTACOLOR

17
high pressure application Italy HT 135
4 Solar box For light Solar box
fastness test 1500

5 Hot pressing For heat TRV


fastness test

6 Crock meter For rubbing MESDAN/


fastness Italy
.

Different softwares have been used for Experimental design, data analysis, and
referencing such as design expert (version 11.03) and EndNote(x7).

3.2. Methods

The experimental part is divided into four main sections.

i. The dyeing of polyester and cotton were done by using disperse and vat dye in a
separate bath to optimize dyeing parameter (temperature, time and carrier
concentration) to get good color strength value of dyed fabric and low staining effect on
the corresponding one.

ii. After dyeing, measured color strength of color strength and color staining of polyester
and cotton by using reflectance spectrophotometer.

iii. After optimization, polyester/ cotton blend dyed with disperse/vat dye one bath one
step with carrier and for comparison polyester /cotton blend also will be subjected to
conventional method, i.e. by using high temperature high pressure process

iv. Finally, properties of the dyed sample within two methods will be evaluated. The
tests are the color strength, fastness to washing, fastness to light, and rubbing fastness.

3.2.1. Experimental Design for Dyeing Parameter Optimization

The experimental setup was based on a central composite design of response surface
methodology. Design expert software used to design the experiment as well as to do

18
analysis of the result. Experiments carried out through three experimental factors
(carrier concentration, temperature and time). Each experiment was performed in
triplicate. It was used to determine the optimum conditions for polyester/cotton blend
fabric dyeing with disperse/vat dye in one bath to obtain good color strength with low
cross staining effect. This design used twice, one for disperse dye and the other for vat
dye.

Table 2; Main dyeing parameters and their factorial level and replica

Factorial levels Replica


Parameters Unit -alpha Low Center High +alpha
Carrier Gpl 0 2 5 8 10 3
concentratio
n
Temperature Degree 70 76 85 94 100
Celsius
Time Min 45 60 83 105 120

Table 3: experimental design of dyeing parameters by central composite design

Factor :1 Factor : 2 Factor :3 Response :1 Response: 2

19
St Run A:carrier B:temperature C:time Color color staining
d concentratio strength of of (cotton and
n (PET or PET)
cotton)

Gpl degree Celsius Min k/s k/s


5 1 8 76 60
10 2 8 94 60
42 3 5 85 120
39 4 5 85 45
30 5 10 85 83
43 6 5 85 83
38 7 5 85 45
21 8 2 94 105
7 9 2 94 60
9 10 2 94 60
19 11 2 94 105
33 12 5 70 83
32 13 5 70 83
15 14 2 76 105
25 15 0 85 83
4 16 8 76 60
34 17 5 100 83
44 18 5 85 83
8 19 2 94 60
31 20 5 70 83
18 21 8 76 105
17 22 8 76 105
41 23 5 85 120
35 24 5 100 83

20
16 25 8 76 105
37 26 5 85 45
45 27 5 85 83
27 28 0 85 83
22 29 8 94 105
26 30 0 85 83
11 31 8 94 60
3 32 2 76 60
6 33 8 76 60
14 34 2 76 105
20 35 2 94 105
24 36 8 94 105
2 37 2 76 60
13 38 2 76 105
29 39 10 85 83
1 40 2 76 60
12 41 8 94 60
28 42 10 85 83
36 43 5 100 83
23 44 8 94 105
40 45 5 85 120

3.2.2. Dyeing method

To find the optimal dyeing parameter, polyester and cotton subjected to dye in vat and
disperse dye bath separately with good color strength and low cross staining effect on
the corresponding fiber. The dyeing condition of both baths identical, except types of
dye. Both dye bath solution prepared with different carrier concentration, dyeing time
and dyeing temperature according to design. Other parameters were constant like,
amount of alkali (sodium hydro oxides), hydros (sodium hydro sulphite), soap,
dispersing agent and dye concentration and MLR.

21
Table 4: Dyeing chemicals and their concentration/amounts.

Sample(PET and cotton ) = 5 gram

Dyeing Tº of PET=70-100ºc
Time =45 -120 min
MLR = 1:30

Chemical used Concentration

Disperse & vat dye(% o.w.f) 3

Carrier (gpl) 0-10 (according to design)

Dispersing agent (gpl) 2

sodium hydro oxides (gpl) 10

hydros (sodium per borate ) (gpl) 10

Soap (gpl) 5

Acetic acid 4.4-5.5

3.2.3. Dyeing process

The dye bath solution prepared by using dye powder and carrier according to required
design in beaker and the ph maintained at 4.5-5.5 using acetic acid buffering chemical
then polyester and cotton sample immersed in prepared dye bath. The bakers loaded in
to laundry-o meter or HTHP machine and dyeing started then raise temperature
according to design.

After half time, the temperature reduced to 70 oc then adds hydros and alkali. The bath
solution become alkaline and continues for the remaining time. Then dyed sample was
rinsed and the leuco vat dye oxidized with air. Soaping of the dyed fabric carried out at
boil for 5-10 min with standard soap. The fabric rinsed and then dried.

22
T
O
4 Key
100 1. Add two dyes, carriers and
other axillaries
1. Add hydros and alkali
2 2. draining
3. soaping and Hot rinsing
70 4. Cold washing

ͦ O
3
5

C 1

0 A 50 % B 100 % C 15 min

Time

Figure 3: Over all dyeing processes of polyester and cotton with disperse and vat dye

in one bath.

3.2.4. Investigation of carrier effect on cross staining

To investigate the effect of carrier on cross staining during polyester/cotton blend


dyeing, polyester and cotton have been dyed with vat and disperse dye in separate bath
with and without carrier under identical condition. Then the cross-staining of cotton and
polyester fabric have been assessed by measuring the color strength (k/s) of dyed
fabric by using reflectance spectrophotometers.

3.3. Data analysis

The test presented by different techniques such as graphs, table and charts. In addition,
the data analyzed by ANOVA, 3D graph and fit summery table from design expert
software.

23
3.4. Quality Assessments Taste

After dyeing of polyester/ cotton blended in both one bath one step method at low
temperature and one bath one step at HTHP method; different dyed fabric will be
measured. Some of major qualities of dyed fabric are described in the following way.

3.4.1. Color strength measurement.

Color strength of dyed fabric samples were measured using spectrophotometer.The test
is done by the procedure set by the Standard - AATCC 6-2003 by using reflectance
spectrophotometers. The color strength values (K/S) have been calculated by applied
the KubelkMunk Equation.

K (1−R) 2
=
S 2R

Where K is the absorption coefficient, R is the reflectance of the dyed fabric and S is the
scattering coefficient.

3.4.2. Cross-staining of cotton and polyester

The cross-staining of cotton component by disperse dye and polyester component by


vat dye was investigated during dyeing of polyester and cotton together. Cross-staining
of cotton and polyester assessed by measure the stained color using
spectrophotometer.

3.4.3. Color fastness to washing

The washing fastness testing determines the resistance of textile colors to domestic or
commercial laundering procedures. Use ISO 105 C06 2002 test method, which is
considered equivalent to AATCC 61 1a 2007 by using Laundry-o-meter. The change in
color and degree of staining was evaluated by using geometric grey scales and
spectrophotometer.

24
3.4.4. Color fastness to rubbing

Rubbing fastness was tested according to AATCC 8 standard by using a crock meter
machine to rub the fabric. Two specimens were taken-one for dry state and one for the
wet state for one sample. The specimens were operated to rub back and forth over a
straight truck for 10 complete cycles at a rate of 1 second for each cycle. Finally, the
white rubbing test cloth removed and the staining was evaluated with standard grey
scale [49].

3.4.5. Color Fastness to Heat

The color fastness to heat of the dyed samples was measured by hot pressing
instrument by the standard method AATCC 133 [50]. After testing, tested fabrics was
assessed and compared with the standard grey scales.

3.4.6. Color fastness to light

Light fastness was tested according to ISO 105 B02 standard [51]. A fabric sample be
prepared where half of its part exposed to light and half of its part will be covered with a
frame which it is mounted altogether with a standard blue scale reference fabric and it
placed in a testing chamber. This blue scale wool fabric consisting of eight dark to light
blue shades used to record the color change of fabric.

The finalized quality assessment and standard method of dyed fabric in both one bath
one step at low temperature and at hthp methods were described in table 5.

Table 5: Quality assessment of dyed fabric

S/n Quality assessments test Standard methods

1 Color strength Cross-Staining of AATCC 6-2003


Cotton and Polyester

2 Wash fastness AATCC-TM 61

3 Light fastness ISO 105 B02

25
4 Rubbing fastness AATCC 8/ISO 105 X 12

5 Hot press fastness AATCC 133

CHAPTER FOUR: RESULTS AND DISCUSSION

4.1. Analyze the effect of dyeing parameters and their optimization for
polyester and cotton dyeing
There are different parameters considered during polyester /cotton blend fabric with
disperses and vat dye in one step one bath at low temperature. Those major significant
parameters are carrier concentration (A), temperature (B) and time (C).

4.1.1. Dyeing of polyester and cotton fabric with disperse dye

When polyester and cotton fabric dyeing with disperse dye, the color strength of cotton
and color sating of polyester were affected by previous listed parameters.

Table 6: Experimental result of polyester and cotton dyeing with disperse dye

Factor 1 Factor 2 Factor Response 1 Response 2


3
Std Run A:carrier B:temperature C:time color strength color
concentration of polyester staining of
cotton
o
Gpl c Min k/s k/s
37 1 5 85 45 1 0.44
40 2 5 85 120 1.48 0.38
16 3 8 76 105 1.18 0.43
39 4 5 85 45 1.28 0.46
23 5 8 94 105 2.37 0.36
1 6 2 76 60 0.44 0.41
8 7 2 94 60 2.21 0.59
38 8 5 85 45 1.15 0.48

26
31 9 5 70 83 0.65 0.37
10 10 8 94 60 1.81 0.53
34 11 5 100 83 3.26 0.46
6 12 8 76 60 0.87 0.42
33 13 5 70 83 0.65 0.36
35 14 5 100 83 3.17 0.49
7 15 2 94 60 1.85 0.53
19 16 2 94 105 2.11 0.42
9 17 2 94 60 2.19 0.57
24 18 8 94 105 2.32 0.36
44 19 5 85 83 1.38 0.39
41 20 5 85 120 1.48 0.44
28 21 10 85 83 1.12 0.36
14 22 2 76 105 0.62 0.42
22 23 8 94 105 2.26 0.4
3 24 2 76 60 0.58 0.43
18 25 8 76 105 1.01 0.42
4 26 8 76 60 0.75 0.39
15 27 2 76 105 0.71 0.42
30 28 10 85 83 1.06 0.43
43 29 5 85 83 1 0.35
5 30 8 76 60 0.71 0.41
27 31 0 85 83 0.58 0.43
11 32 8 94 60 2.07 0.48
17 33 8 76 105 1.12 0.43
26 34 0 85 83 0.65 0.43
25 35 0 85 83 0.58 0.42
20 36 2 94 105 2.12 0.41
32 37 5 70 83 0.65 0.34
42 38 5 85 120 1.52 0.4
2 39 2 76 60 0.45 0.42
29 40 10 85 83 1.31 0.43
12 41 8 94 60 2.13 0.42
45 42 5 85 83 1.11 0.35
21 43 2 94 105 2.35 0.39
13 44 2 76 105 0.65 0.41
36 45 5 100 83 3.1 0.42

The normality assumption was satisfied as the residual plot approximated along a
straight line [52]. The Normal % probability vs residual shows the graph plots of the
normality test for color strength polyester and color staining of cotton fabric (figure 3). It
is observed that in all the graphs, the residuals lie on the straight line, which indicates
that the distribution of residuals for all is normal.

27
a) Color strength of polyester b) Color staining of cotton

Figure 4: Normal probability plot for color strength of polyester and color sating of cotton

Based on fit summary table 7, the model of color strength of polyester is quadratic
which is suggested by software.

Table 7: Fit summary table of color strength of polyester

Source Sequential p- Lack of Fit p- Adjusted Predicted


value value R² R²

Linear < 0.0001 < 0.0001 0.8308 0.8106

2FI 0.5384 < 0.0001 0.8274 0.8158


Quadratic < 0.0001 0.1123 0.9751 0.9660 Suggeste
d
Cubic 0.2058 0.0877 0.9766 0.9649 Aliased

4.1.1.1. Analyze of Variance for color strength of polyester

The ANOVA of color strength of polyester during dyeing of polyester and cotton fabric
together with disperse dye is described in table 8.

The Model F-value of 192.46 implies the model is significant. There is only a 0.01%
chance that an F-value this large could occur due to noise. In this case A, B, C, AB, A²,

28
B², C² were significant model terms because those f-value is less than 0.05. But others
were insignificant model terms to color strength of polyester. The Lack of Fit F-value of
1.97 implies the Lack of Fit is not significant relative to the pure error. There is 11.23%
chance that a "Lack of Fit F-value" is significant, this large could occur due to noise.
Non-significant lack of fit is good and the model is fit. Therefore, it can be concluded
that carrier concentration (A), temperature (B) and time (C) played an important role in
case of color strength of polyester. It implied that a good correlation between input and
output variables could be drawn by the model developed.

Table 8: ANOVA table for color strength of polyester

Source Sum of Df Mean F-value p-value


Squares Square
Model 25.95 9 2.88 192.46 < 0.0001 Significant
A-carrier 0.6290 1 0.6290 41.98 < 0.0001
concentration
B-temperature 21.12 1 21.12 1410.09 < 0.0001
C-time 0.5010 1 0.5010 33.44 < 0.0001
AB 0.1768 1 0.1768 11.80 0.0015
AC 0.0500 1 0.0500 3.34 0.0762
BC 0.0018 1 0.0018 0.1185 0.7328
A² 0.1195 1 0.1195 7.97 0.0078
B² 1.50 1 1.50 99.92 < 0.0001
C² 0.1029 1 0.1029 6.87 0.0129
Residual 0.5243 35 0.0150
Lack of Fit 0.1295 5 0.0259 1.97 0.1123 not
significant
Pure Error 0.3948 30 0.0132
Cor Total 26.47 44

Furthermore, from the fit statistics table of color strength of polyester, the difference
between predicted R² of 0.9660 and adjusted R² of 0.9751 is less than 0.2 and noise
ratio of 47.327 is greater than 4. This model designates an adequate signal to navigate
the design space as well.

The model was developed using quadratic model which is suggested by the software.
The coded equation is useful for identifying the relative impact of the factors by
comparing the factor coefficients. Therefore, the Final design model equation for color
strength of polyester in terms of coded factors was designed as:

29
¿ of polyster (k /s)=1.15+ 0.1236∗A +0.7208∗B−0.0853∗AB−0.0806 A 2+ 0.2891 B 2+ 0.0758C 2
…………. Equation (1)

Where; A= Carrier concentration, B= temperature, AB=interaction of carrier


concentration and temperature, A 2= square of carrier concentration, B 2 squared of
temperature and C2 =square of time.

4.1.1.2. Analyze of single factor effect on color strength of polyester

A. Effect of Carrier concentration on color strength of polyester

Carriers improve color strength of polyester when polyester dye with disperse dye.
Because when polyester fibers absorb the carriers and swell, the glass transition
temperature (Tg) of polyester reduces due to plasticizing effect of carrier [53]. Thus
promote polymer chain movements and creating free volume. This speeds up the
diffusion of the dye into the fibers. Alternatively, the carrier may form a film around the
surface of polyester fiber in which disperse dye solubilized by carrier, thus increasing
the rate of transfer dye into the fiber [54] hence color strength of polyester increases.
But after a certain amount of carrier concentration, color strength of polyester become
constant as shown in figure 4. The increasing effect of carrier concentration decreases,
when temperature increases.

a) at low temperature b) at high temperature

30
Figure 5: Effect of carrier concentration on color strength of polyester

B. Effect of temperature on color strength of polyester

As temperature increases, color strength of polyester increases. Because, temperature


can facilitate the disintegration of dye molecules in solution so that more individual
molecules are available for penetration into the fibers. In dyeing of polyester fibers with
disperse dyes, the dye bath exhaustion of dye increases with increasing temperature
around glass transition temperature [15]. On the other hand, temperature also improves
polymer segmental chain movement of polyester fibers and it creates free volume
according to free volume theory. This improves diffusion of dye molecules from fiber
surface in to polyester fiber. And also, it increases the attraction and reaction between
the dye molecules and fibers. At different carrier concentration, Increasing effect of
temperature also different as shown in figure 5.

a) low carrier concentration b)high carrier concentration

Figure 6: Effect of temperature on color strength of polyester

C. Effect of time on color strength of polyester

As time increases color strength of polyester increases slightly. When the fabrics stay
longer time in the dye bath solution, more dye molecules diffusion in to the fiber surface
then amount of dye in the fiber surface high or this long times gives sufficient time to

31
achieve dye equilibrium. When temperature increases, increasing effect of time
decreases. Because when temperature increase, rate of dyeing increase since with a
minimum time it can achieve high color shade. But relatively to other factors, time has
not statically significant effect on color strength of polyester fibers. Since time interact
with temperature.

Figure 7: Effect of time on color strength of polyester

4.1.1.3. Analyses of the interaction effect on color strength of polyester

As shown figure 7, which is described by 3d and contour plot, the interaction of carrier
concentration and temperatures has effect on color strength of polyester.

a) 3d graph b) contour plot

Figure 8: Interaction effect of carrier concentration and temperature

32
4.1.1.4. Analyze of Variance for color staining of cotton

The ANOVA of color staining of cotton during dyeing of polyester and cotton with
disperse dye is given in Table 10. This shows that, the model F-value of 16.55 and p-
values less than 0.5 implies the model is significant. Therefore, carrier concentration
(A), temperature (B), time (C), interaction of carrier concentration and temperature (AB),
interaction of temperature and time (BC), square of carrier concentration (A²), square of
temperature (B²) and square of time ( C² ) were significant model terms. The Lack of Fit
F-value of 1.76 implies the Lack of Fit is not significant relative to the pure error. Non-
significant lack of fit is good. Therefore, this ANOVA table indicates the process is
significant and the model is fit.

Table 9: ANOVA table of color staining of cotton.

Source Sum of Df Mean F-value p-value


Squares Square
Model 0.1060 9 0.0118 16.55 < 0.0001 Significant
A-carrier 0.0050 1 0.0050 7.03 0.0120
concentration
B-temperature 0.0231 1 0.0231 32.43 < 0.0001
C-time 0.0257 1 0.0257 36.11 < 0.0001
AB 0.0048 1 0.0048 6.77 0.0135
AC 0.0021 1 0.0021 2.88 0.0984
BC 0.0292 1 0.0292 41.06 < 0.0001
A² 0.0093 1 0.0093 13.03 0.0010
B² 0.0066 1 0.0066 9.23 0.0045
C² 0.0152 1 0.0152 21.38 < 0.0001
Residual 0.0249 35 0.0007

33
Lack of Fit 0.0056 5 0.0011 1.76 0.1517 not significant
Pure Error 0.0193 30 0.0006
Cor Total 0.1309 44

According to fit summary table, the model of color staining of cotton was developed
using quadratic model which is suggested by the software.

The Final equation of suggested model of color staining of cotton in terms of coded
factors was designed as the following:

¿ of cotton ( ks )=0.3608−0.011∗A+ 0.0238∗B−0.0251∗C−0.0141∗AB−0.0349∗BC + 0.0225∗A 2+0.0192∗B


…………. Equation (2).

4.1.1.5. Analyze of one factor effect on color staining of cotton

a. Effect carrier concentration on color staining of cotton

Carrier concentration has a negative effect on staining of cotton by disperse dye. Since
carrier concentration increases with constant temperature and time, color staining of
cotton decreases. When carriers make film on the polyester fiber surface, the dye
molecules of disperse dyes is adsorbed and absorbed by polyester fiber. Because,
disperse dyes solubilized by carrier and it has high substantive to polyester fibers.
There for, the dye concentration in the bath gradually decreases. Thus, dye molecules
on the surfaces of cotton is gradually desorbed in to dye bath because disperse dyes
haven’t substantivity to cotton. As a result, staining of cotton by disperses dye
decreases, as concentration of carrier increases.

34
Figure 9: Effect carrier concentration on color staining of cotton

B. Effect of temperature on color staining of cotton

During dyeing of polyester and cotton fabric with disperse dye; temperature has
significant effect on color staining of cotton. As Shown figure 9, temperature has
different effect on color staining of cotton at minimum and maximum time. At minimum
time, if temperature increases, color staining of cotton by dye increases. When
temperature increases dye exhaustion of dye molecules in to cotton surface increases.
Thus much amount of disperses dye on the surface of cotton so color staining effect
increases. But cotton fabric stay for long time in dye bath, dye molecules move from
fiber surface in to dye bath. Because disperse dyes hasn’t substantive to cotton so
color staining of cotton becomes reduces.

a) at minimum time b) at maximum time

35
Figure 10: Effect of temperature on color staining of cotton

C. Effect of time on color staining of cotton

The effect of time on color staining of cotton fabric was described in figure 10. When
time increase color staining of cotton decrease. Because as discussed previous, the
fabrics stay along time in dye bath, polyester fabrics highly absorb disperse dyes from
dye bath. Thus, content of disperse dye on the bath decrease and the dye molecules
move from cotton surface to dye bath. Therefor color staining of cotton decreases as
time increases. It is true at high temperature. But at low temperature absorption of
disperse dye by polyester low since high amount of disperse dye molecules in the dye
bath. When cotton fabric stays a long time on the bath, disperse dye can adsorb on the
surface of cotton. Consequently, sating of cotton by disperses dye becomes increases.

a) At high temperature(94oc ) b) at low temperature (76 oc)

Figure 11: Effect of time on color staining of cotton

4.1.1.6. Analyze of the interaction effect on color staining of cotton

During dyeing of polyester and cotton dyeing with disperse dye, the interaction of carrier
concentration and temperature and the interaction of temperature and time have effect
on color staining of cotton as shown figure 11 and 12 respectively.

36
a) 3D graph b) contour plot

Figure 12: Interaction effect of carrier concentration and temperature.

a) 3D graph c) contour plot

Figure 13: Interaction effect of temperature and time on color staining of cotton

4.1.2. Dyeing of polyester and cotton fabric with vat dye

When polyester and cotton fabric were dyeing with vat dye, the dyeing parameters (I, e
carrier concentration, temperature and time) have an effect on color strength of cotton

37
and color staining polyester. To analyze the effect and optimize of each parameter, the
experimental results were described by table 11.

Table 10: Experimental result of polyester and cotton dyeing with vat dye

Factor 1 Factor 2 Factor Response 1 Response 2


3
St Run A:carrier B:temperature C:time color strength color staining
d concentration of cotton of polyester
Gpl c
O
Time k/s k/s
23 1 8 94 105 2.48 0.47
22 2 8 94 105 2.08 0.65
5 3 8 76 60 1.75 0.49
20 4 2 94 105 2.03 0.5
10 5 8 94 60 2.59 0.64
11 6 8 94 60 2.28 0.58
31 7 5 70 83 1.42 0.53
1 8 2 76 60 1.78 0.53
4 9 8 76 60 1.61 0.48
24 10 8 94 105 2.28 0.56
7 11 2 94 60 2.12 0.74
15 12 2 76 105 1.52 0.5
19 13 2 94 105 2.18 0.68
45 14 5 85 83 2.48 0.5
29 15 10 85 83 1.9 0.45
43 16 5 85 83 2.58 0.6
13 17 2 76 105 2.31 0.72
8 18 2 94 60 2.43 0.69
42 19 5 85 120 2.41 0.74
40 20 5 85 120 2.412 0.73
41 21 5 85 120 2.411 0.75
36 22 5 100 83 3.11 0.58
30 23 10 85 83 1.93 0.45
21 24 2 94 105 2.11 0.59
37 25 5 85 45 2.32 0.76
38 26 5 85 45 2.312 0.75
16 27 8 76 105 1.56 0.61
35 28 5 100 83 3.11 0.56
26 29 0 85 83 1.71 0.53
27 30 0 85 83 1.8 0.55
18 31 8 76 105 1.94 0.55
2 32 2 76 60 1.62 0.54
32 33 5 70 83 1.94 0.54
3 34 2 76 60 1.7 0.54

38
34 35 5 100 83 3.112 0.51
39 36 5 85 45 1.91 0.77
12 37 8 94 60 2.59 0.61
28 38 10 85 83 1.83 0.45
44 39 5 85 83 2.18 0.49
33 40 5 70 83 1.92 0.57
25 41 0 85 83 1.61 0.5
9 42 2 94 60 2.57 0.78
17 43 8 76 105 1.91 0.55
6 44 8 76 60 1.47 0.47
14 45 2 76 105 2.21 0.61

The analysis of diagnostic case statistics of data shows in figure 13. The graph plots of
color strength of cotton and color staining of polyester respectively are used to test the
distribution normality of the residuals. It is observed that in both graphs, the residuals
lie on the straight line is normal distribution of residuals.

a) color strength of cotton b) color staining of polyester

Figure 14: Normal probability plot for

4.1.2.1. Analyze of Variance for color strength of cotton

Table 11: Fit summary table for color strength of cotton

39
Source Sequential p- Lack of Fit p- Adjusted Predicted
value value R² R²

Linear < 0.0001 < 0.0001 0.5007 0.4417


2FI 0.1487 < 0.0001 0.5310 0.4609
Quadratic < 0.0001 0.1015 0.7549 0.6764 Suggeste
d
Cubic 0.1714 0.0986 0.7735 0.6618 Aliased

From fit summary table, the model of color staining of cotton was developed using
quadratic model which is suggested by the software.

According to the ANOVA of color strength of cotton in table 13, the Model F-value of
16.06 implies the model is significant and the P- value of 0.0001 which is less than 0.05.
The parameters having P-value less than 0.05 are said to be significant. In this case B,
BC and A² were the significant model terms, whereas A, C, AB, AC, B2,C2, were the
insignificant terms color strength of cotton. The Lack of Fit F-value of 2.04 showed the
Lack of Fit is not significant relative to the pure error. There is a 10.15% chance that a
"Lack of Fit F-value" this large could occur due to noise. However non-significant lack of
fit is good because the model is geared toward perfect fitness.

Table 12: ANOVA table for color strength of cotton

Source Sum of Df Mean F-value p-value


Squares Square
Model 6.45 9 0.7170 16.06 < 0.0001 Significant
A-carrier 0.0129 1 0.0129 0.2894 0.5940
concentration
B- 4.27 1 4.27 95.63 < 0.0001
temperature
C-time 0.0393 1 0.0393 0.8802 0.3546
AB 0.1291 1 0.1291 2.89 0.0979
AC 0.0012 1 0.0012 0.0263 0.8721
BC 0.3526 1 0.3526 7.90 0.0080
A² 1.15 1 1.15 25.79 < 0.0001
B² 0.0100 1 0.0100 0.2240 0.6389
C² 0.0970 1 0.0970 2.17 0.1495
Residual 1.56 35 0.0446
Lack of Fit 0.3963 5 0.0793 2.04 0.1015 not significant
Pure Error 1.17 30 0.0389
Cor Total 8.02 44

40
Furthermore, the models also check according to fit statics. The residuals between the
predicted and experimental (actual) values were found to be low implying that both the
predicted and experimental responses had strong agreements [52]. The difference
between Predicted R-squared (0.6764) and Adjusted R squared (0.7549) of this model
is less than 0.2. The Adequate Precision measures the signal to noise ratio and the
ratio greater than 4 is desirable. The ratio of this model is 13.469, which is greater than
4 and it indicates an adequate signal. This model can be used to navigate the design,
and the model has a strong enough signal to be used for optimization.

A quadratic model that relates the color strength of cotton (response) and the dyeing
parameters were chosen by the software (Table 13). The final model equation of color
strength of cotton in terms of coded factors was designed as in eq 3.

¿ of cotton ( ks )=2.44 +0.3241∗B−0.1212∗BC−0.2502∗A 2…equation (3)


Where: B=temperature, BC= interaction of temperature and time and A 2=square of
carrier concentration.

4.1.2.2. One factor analysis on color strength of cotton

A. Effect of carrier concentration on color strength of cotton

Carrier concentration has an effect on color strength of cotton. When carrier


concentration increases up a certain point, color strength of cotton also increases.
Conversely, if the concentration further increase, cotton color strength becomes
reduces this described in figure 14. However carrier concentration was not statistical
significant model terms for color strength of cotton relative to others. This didn’t mean
carrier concentration hasn’t effect on color strength of cotton.

41
Figure 15: Effect of carrier concentration on color strength of cotton

B. Effect of temperature on color strength of cotton

During dyeing of polyester and cotton with vat dye, color strength of cotton increases
when temperature increases. Before reduction of vat dye in to soluble or leuco form ,
vat dyes are pre pigmented on the surfaces of cotton at initial temperature, since when
temperature increase, disintegration of dye molecules and uniform fine distribution of
vat pigment on cotton fabric surfaces increases. Then this pre pigmented vat pigments
easily reduced in to soluble (leuco) form when treated with alkaline and hydros
solution[55]. This leuco form dyes have high substantivity to cotton fabric. Generally,
temperature increases color strength (k/s) of cotton increases directly as shown in figure
15.

Figure 16: Effect of temperature on color strength of cotton


42
C. Effect of time on color strength cotton

Time is not statically significant factor on color strength of cotton. Because the effect of
time on color strength of cottons is highly interact with temperature. At low temperature,
when time gradually increase, color strength of cotton also increase. The reverse is true
at high temperature. When the fabrics stay long time in dye bath at low temperature, the
dye molecules adsorb on the surface of the fabric then increase stained color shade
because at low temperature, the dye molecules not disintegrate and exhaustion of dyes
in to the fabric low. But at high, the pigment vat dye reduces in to leuco form and it can
easily exhaust in to the fiber with a small time. However, if the fabric stay long time in
dye bath, desorption of dyes from cotton in to dye bath solution takes place since color
strength (k/s) of cotton decreases. However time is non-significant factor for color
strength of cotton. The effect of time in different temperature is described in figure 16.

a) at low temperature b) at high temperature

Figure 17: Effect of time on color strength cotton

4.1.2.3. Analyze of the interaction effect on color strength of cotton

The Interaction of temperature and time has an effect on color strength of on color
strength of cotton during dyeing of polyester and cotton dyeing with disperse dye are
shown figure 17,which is described by 3D graph and contour plot.

43
a) 3D graphs b) contour plot

Figure 18: The interaction effect of temperature and time on color strength of cotton

4.1.2.4. Analyze of Variance for color staining of polyester

Table 13: Fit summary table for color staining of polyester

Source Sequential p- Lack of Fit p- Adjusted Predicted


value value R² R²
Linear 0.1418 < 0.0001 0.0589 -0.0582
2FI 0.1119 < 0.0001 0.1310 0.0270
Quadratic < 0.0001 0.2741 0.7279 0.6348 Suggeste
d
Cubic 0.2227 0.4053 0.7429 0.6124 Aliased

As shown table 14, the selected model for color staining of polyester is quadratic, which
is suggested by design expert software.

Table 14: ANOVA table for color staining of polyester

Source Sum of Df Mean F-value p-value


Squares Square
Model 0.3440 9 0.0382 14.08 < 0.0001 Significant
A-carrier 0.0330 1 0.0330 12.16 0.0013
concentration
B-temperature 0.0213 1 0.0213 7.86 0.0082
C-time 0.0009 1 0.0009 0.3418 0.5625

44
AB 0.0014 1 0.0014 0.4972 0.4854
AC 0.0049 1 0.0049 1.79 0.1891
BC 0.0493 1 0.0493 18.16 0.0001
A² 0.0065 1 0.0065 2.40 0.1304
B² 0.0001 1 0.0001 0.0421 0.8385
C² 0.1010 1 0.1010 37.18 < 0.0001
Residual 0.0950 35 0.0027
Lack of Fit 0.0174 5 0.0035 1.34 0.2741 not
significant
Pure Error 0.0777 30 0.0026
Cor Total 0.4390 44

As shown from ANOVA table 15, model F-value 14.08 indicates the model which is
significant. There is only a 0.01% chance that an F-value this large could occur due to
noise. In this case A, B, BC, C² were significant model terms, whereas C, AB, AC,
A2and B2 were insignificant terms in color staining of polyester by vat dye. Therefore, it
can be decided that carrier concentration (A), temperature (B), plays an important role
in case of color staining of polyester.

The Lack of Fit F-value of 1.34 implies the Lack of Fit is not significant relative to the
pure error. There is a 27.41% chance that a "Lack of Fit F-value" this large could occur
due to noise. There for, this non-significant lack of fit is good.

From fit statics table, the Predicted R² of 0.6348 is in reasonable agreement with the
Adjusted R² of 0.7279; i.e. the difference is less than 0.2 proves that the model is fitting
the data and can reliably be used to interpolate. The adequate Precision value 12.878
which is greater than 4 suggests that an adequate signal. This model can be used to
navigate the design space and optimization.

The model of color staining of polyester is quadratic which is suggested by software and
the coded equations became:

¿ of polyester ( KS )=0.5334−0.0283∗A+ 0.0229∗B−0.0453∗BC +0.0751∗C ………………….


2

eq (2)

45
Where: A = carrier concentration, B= temperature, BC= interaction of temperature and
time and C2= square of time.

4.1.2.5. Analyze of one factor effect on color staining of polyester

A. Effect of carrier concentration on color staining of polyester

During polyester and cotton dyed with vat dye polyester fabric may be stained by vat
dye. As seen the figure 19 carrier concentrations increases, color staining (k/s) value
decreases. When carries form film around polyester surface, this film prevents
penetration of vat pigment before reduction. And also after reduction of vat pigment in
to leuco form, this leuco (solubilized) vat dye not interacts with the film which is
produced by carrier on polyester fabric surfaces. Because there is no affinity between
carrier and reduce vat dye. However, the reduction effect of carrier concentration on
cross staining of polyester is a little bit different in different time with constant
temperature as shown figure 18. For example at maximum dyeing time, crosses
staining effect increase because when polyester stay maximum time at high
temperature, the segmental chain mobility increase and it can create free volume.
Since vat dyes maybe inter in to fiber surface of polyester so color staining of polyester
increases.

a) at 60 min b) at 105 min

Figure 19: Effect of temperature on color staining of polyester

46
B. Effect of temperature on color staining of polyester

When temperature increases color staining of polyester increase, because, as


temperature increases, segmental chain mobility of polyester increase according to free
volume color theory, then vat dye molecules may be easily penetrate in to fiber it is true
at low time but at high time the reverse is true.

a) At 76 min b) at 105 min

Figure 20: Effect of temperature on color staining of polyester

C. Effect of time on color staining of polyester

When time increase color staining of polyester decrease up to ascertain time. When
time increase further then color staining of polyester increases. At the beginning the
dyeing process, dyes molecules exhaust from dye bath in to fabric surface and then the
dye molecules adsorbed from fabric surfaces when time is gradually increases.
However, when time increase further, chain mobility of polyester increase then vat dyes
may be penetrate in to fabric then color staining increase .The effect range of time on
color staining of polyester with vat in different temperature with constant carrier
concentration is slightly different as shown figure 20.

47
a) At high temperature b) at low temperature

Figure 21: Effect of time on color staining of polyester

4.1.2.6. Analyze of the Interaction effects on color staining of polyester

The Interaction of temperature and time has a significant on color staining of polyester
when polyester and cotton fabric dyeing with vat dye. Figure 21 describes the
interaction effect of temperature and tine on color staining of polyester in 3d and counter
plot graph.

a) 3D plot b) contour plot

Figure 22: The interaction effect of temperature and time on color staining of polyester.

48
Color strength of dyed fabric

To investigate the color buildup properties of polyester and cotton fabric, the k/s value
was measured by using reflectance spectrophotometers. the color strength value of
fabrics which dyed in one bath one step method by using disperse/ vat dye combination
at low temperature with carrier is slightly lower than fabric which dyed in conventional
one bath one step at hthp method as seen in figure 23. This figure describes the
average k/s value of both fabrics which dyed in two different methods from 3 samples
for each fabric.

Colour strength value of dyed fabric

with carrier hthp


4.26
3.56

1.89 2.06

cotton Polyester

Figure 23: Comparison of k/s value of polyester and cotton dyed fabric in two methods

Analysis of Color fastness properties of dyed fabric

different color fastness property of polyester and cotton dyed fabric which were dyed in
one bath one step method with the combination of disperse /vat dye at low temperature
and in conventional one bath one step dyeing method were assessed . It includes
washing fastness, rubbing fastness, hot press fastness and light fastness.

1. wash fastness properties

The colorfastness to washing was assessed by compare color change of dyed sample
and staining of color in polyester and cotton fabric to standard gray scale.

49
Table 15: Wash fastness of polyester and cotton fabric dyed with disperses /vat dye
combination in one bath at low temperature with carrier and conventional HTHP
methods

With carrier method HTHP method


Cotton fabric
No Color Staining on Color Staining on
Change Polyester Cotton Change Polyeste Cotton
r
1 4-5 4 4-5 4-5 4-5
4-5
2 4-5 4-5 4-5 4-5 4-5 4

Polyester fabric
1 4-5 4-5 4-5 4-5 4
4-5
2 4-5 4-5 4 4-5 4-5 4-5

As seen in the Table-16 the color fastness to wash (color change) of one bath one-step
dyed polyester cotton and blend at low temperature is approximately similar with
conventional two one bath one step with HTHP method dyed sample. This is due to
disperse and vat dyes have hydrophobic in nature the tendency of hydrolyzed with
water during washing is less. carrier not affect wash fastness of both polyester and
cotton dyed fabric during dyeing of polyester and cotton fabric in one bath one step at
low temperature.

2. Rubbing fastness

The color staining of wet and dry full bleach cotton fabric is assessed according to
standard gray scale for staining.

3. Hot press fastness

The color change of dyed fabric during hot press was assessed by comparing the color
staining on both wet and dry half bleached cotton fabric with standard gray scale for
staining.

50
Table 16: Rubbing and hot press fastnes of cotton and polyester dyed fabric with
disperses /vat dye at low temperature with carrier and conventional HTHP method bath
dyed.

Rubbing fastness
Within carrier method Within HTHP method
N Polyester Cotton Polyester Cotton
o
dry wet Dry wet dry wet Dry Wet
1 5 4-5 4-5 4 4-5 4 4-5 3-4
2 4-5 4 4-5 3-4 4-5 4-5 4-5 4

Hot press fastness


1 5 4-5 5 4-5 5 4-5 5 4-5

2 5-4 4-5 5 4-5 4-5 4 5 4-5

Table-21 shows that the samples dyed in one bath one-step with disperse/vat dye at
low temperature has approximately similar dry and wet rubbing and hot press fastness
property, compared with conventional one bath one step at HTHP method.

4. light fastness

The light fastness property of polyester and cotton dyed fabric in both method have
good and approximately similar property I,e all dyed fabric in two method almost similar
value I,e between 7- and 8 according to blue scale.

51
Summery

Generally, from the design evaluation, diagnostics graphs, fit summary and ANOVA
statistics, all the models provide a good estimate of the true response surface. The
dyeing process of polyester and cotton fabric optimize by using design expert software.
Since the goals of optimization was to maximize color strength and minimize cross
staining effect on polyester and cotton fabric. When polyester and cotton fabrics
subjected to vat dye, temperature (B) has significant effect on color strength of cotton
whereas; carrier concentration (A) and time (C) haven’t significant effect. Carrier
concentration and time have significant effect on color staining of polyester with vat dye.
When carrier increases, color staining of polyester is decreases. When polyester and
cotton fabrics dyed with disperse dye, all three factors have significant effect on color
strength of polyester and color staining of cotton with disperses dye. In general, based
on experimental result to get good color strength with minimum staining effect, carrier
concentration (5 gpl), time (120 min) and temperature (100 oc) are selected.

52
CHAPTER FIVE: CONCULISSION AND RECCOMANDATION
5.1. Conclusion

Polyester/cotton blend dyeing at low temperature with the combination of disperse and
vat dyes was realized by using carrier for archiving polyester /cotton fabric dyed in one
bath one step method. To analysis the effect of each factor on color strength and color
staining property, both polyester and cotton fabric was subjected to together in a
separate disperse and vat dye bath. The experiment result show that, carrier
concentration has positive effect on both dyed and stained fabric of both polyester and
cotton however temperature have positive effect on color strength of both polyester and
cotton dyed fabric and negative effect on both polyester and cotton stained fabric. The
optimum dyeing parameters during dyeing of polyester and cotton fabric in on bath one
step by disperse and vat dye combination at low temperature were; carrier
concentration (5 gpl), temperature (100 oc) and time (120 min). This optimum parameter
gave good color strength and minimum staining effect on polyester and cotton fabric.

According to color strength and fastness property result of polyester and cotton fabric,
one-step one bath dyed polyester/cotton blend with disperse /vat dye at low
temperature has good and almost similar fastness property and color strength value
compared with conventional one bath with HTHP method dyed fabric. From these
results, practical possibilities in one bath one step dyeing of polyester/cotton blends at
low temperature using disperse/ vat dyes combination can be achieved. One-bath one-
step dyeing of polyester/ cotton blend at low temperature with the combination of
disperses and vat dye method also relatively simple and less requirement of energy,
time, and resource as comparison with the conventional one. In general, this method is
advantages over the conventional one bath one step dyeing of polyester/ cotton blend
with the combination of disperse and vat dye at HTHP method in different way as
discussed in previous.

53
5.2. Recommendations

Dyeing of polyester/cotton blends in one-bath one-step dyeing methods with disperse


/vat dye combination at low temperature by using an organic compound i.e. carrier
methods was studied. Industrial application needs a cost effective process and easily
available machine Even though this process seems to give good color fastness
property. Dyeing of polyester/ cotton blends in this method is more advantages for small
fabric dyeing industry and garment dyeing company relatively the conventional one bath
one step method because this method requires expensive machine that is high
temperature high pressure machine. So I recommended this one bath one step dyeing
of polyester/cotton blend by using the combination of disperse/ vat dye at low
temperature by using carrier to garment dyeing company and small fabric dyeing
industry, since it give deep shade at boil temperature with reasonable time. and also the
process to achieve this temperature not require special machine and special fluid ,
easily achieve by using any machine and water as fluid on the other hand the
conventional one bath one step method requires special machine(HTHP machine ) and
special fluid (oil) and this part, hard over all dyeing process.

54
Reference

1. Forsythe, S.M. and J.B. Thomas, Natural, synthetic, and blended fiber contents:
An investigation of consumer preferences and perceptions. Clothing and Textiles
Research Journal, 1989. 7(3): p. 60-64.
2. Zhang, W., et al., One-bath one-step low-temperature dyeing of polyester/cotton
blended fabric with cationic dyes via β-cyclodextrin modification. Textile
Research Journal, 2019. 89(9): p. 1699-1711.
3. Ibrahim, N., Dyeing of textile fibre blends, in Handbook of textile and industrial
dyeing. 2011, Elsevier. p. 147-172.
4. Legrini, O., E. Oliveros, and A. Braun, Photochemical processes for water
treatment. Chemical reviews, 1993. 93(2): p. 671-698.
5. Foisal, A. and M.T. Ahmed, Dyeing of Polyester/Cotton Blended Woven Fabric in
One Bath.
6. Arslan, I., Treatability of a simulated disperse dye-bath by ferrous iron
coagulation, ozonation, and ferrous iron-catalyzed ozonation. Journal of
Hazardous Materials, 2001. 85(3): p. 229-241.
7. Najafi, H., et al., One bath method dyeing of polyester/cotton blend fabric with
sulphatoethylsulphonyl disperse/reactive dyes treatment by chitin biopolymer.
African Journal of Biotechnology, 2009. 8(6).
8. Pérez, M., et al., Fenton and photo-Fenton oxidation of textile effluents. Water
research, 2002. 36(11): p. 2703-2710.
9. Gejdzicki, B. The dyeing process of textile made from polyester/cellulose fiber
yarn. in Proceeding of the conference of dye and colorists’, zakopane. 1998.
10. Aspland, J., Disperse dyes and their application to polyester. Textile Chemist and
Colorist, 1992. 24: p. 18-18.
11. Oliveria, F.R., et al., Dyeing of cotton and polyester blended fabric previously
cationized with synthetic and natural polyelectrolytes. Procedia engineering,
2017. 200: p. 309-316.

55
12. Meena, C., et al., One-bath dyeing process for polyester/cotton blend using
physical mixtures of disperse/reactive dyes. European International Journal of
Science and Technology, 2013. 2(2): p. 6-16.
13. Sivakumar, R. and K. Pillay, Study of pilling in polyester/cotton blended fabrics.
1981.
14. Hussain, U., et al., Comfort and mechanical properties of polyester/bamboo and
polyester/cotton blended knitted fabric. Journal of Engineered Fibers and
Fabrics, 2015. 10(2): p. 155892501501000207.
15. Broadbent, A.D., Basic principles of textile coloration. 2001: Society of Dyers and
Colourists.
16. Yoon, H. and A. Buckley, Improved comfort polyester: Part I: Transport
properties and thermal comfort of polyester/cotton blend fabrics. Textile
Research Journal, 1984. 54(5): p. 289-298.
17. Yang, Y. and S. Li, One-Step Dyeing of Polyester/Cotton With Disperse/Reactive
Dyes. Textile Chemist & Colorist & American Dyestuff Reporter, 2000. 32(3).
18. Chattopadhyay, D. and T. Shaikh, Dyeing of Polyester/Cotton Blends-An
Overview. MAN MADE TEXTILES IN INDIA, 2002. 45(12): p. 456-469.
19. Broadbent, A.D., Basic Principles of Textile Coloration, Society of Dyers and
Colorists. West Yorkshire, UK, 2001.
20. Chakraborty, J., Fundamentals and practices in colouration of textiles. 2015:
CRC Press.
21. Patil, H.I., V.A. Dorugade, and V. Shivankar, Single and double bath dyeing of
polyester/cotton blended fabric using disperse and reactive dye. International
Journal on Textile Engineering and Processes, 2016. 2(4): p. 29-33.
22. CHALK, R.W. and N.E. HOUSER, Rapid Dyeing Concepts for Polyester/Cotton.
Textile Chemist & Colorist, 1988. 20(11).
23. Aspland, J., Dyeing Blends: Polyester/Cellulose. Textile Chemist & Colorist,
1993. 25(8).
24. Carlough, M.S. and L.A. Meszaros, One-bath dyeing of polyester-cellulosic
blends using disperse and sulfur dyes. 1989, Google Patents.

56
25. Swiderski, Z., The modern dyeing systems for blends of polyester and cellulose
fibers. Przeglad Wlokienniczy, 1981(2): p. 87-91.
26. Chao, Y., et al., Dyeing of cotton-polyester blends with anthraquinonoid vat dyes.
Dyes and pigments, 1999. 40(1): p. 59-71.
27. Bright, L., Trouble shooting continuous thermosol dyeing of polyester fiber and
blends. American dyestuff reporter, 1996. 85(8): p. 60-61.
28. Short, S., Introduction of Instrumentation to the Continuous Dyeing of Polyester
—Cotton Blends. Journal of the Society of Dyers and Colourists, 1979. 95(3): p.
112-115.
29. SHORE, J., Continuous dyeing. Review of Progress in Coloration and Related
Topics, 1979. 10(1): p. 33-49.
30. Hyde, R., Review of continuous dyeing of cellulose and its blends by heat
fixation processes. Review of Progress in Coloration and Related Topics, 1998.
28(1): p. 26-31.
31. Kim, M., et al., Dyeing of cotton and polyester/cotton blend with disperse dyes
using sodium 2-(2, 3-dibromopropionylamino)-5-(4, 6-dichloro-1, 3, 5-
triazinylamino)-benzenesulfonate. Fibers and Polymers, 2006. 7(4): p. 352-357.
32. Elsherbiny, A.S. and M. Kaukab, One-bath one-step dyeing of a polyester/cotton
blend using the pad-dry-fixation process. Fibres & Textiles in Eastern Europe,
2016(2 (116)): p. 113--119.
33. Davis, J., The Preparation and Dyeing of Polyester—Cotton Fabrics. Journal of
the Society of Dyers and Colourists, 1973. 89(3): p. 77-80.
34. Holme, I., Coloration of technical textiles, in Handbook of technical textiles. 2016,
Elsevier. p. 231-284.
35. Wen-chan, C., One-bath-two-step dyeing process of T/C fabric with
disperse/reactive dyes [J]. Dyeing & Finishing, 2013. 3.
36. Prasad, R.K., M.A. Shahid, and M. Dulal, A Comparative Study Between One
Bath Dyeing Method For Polyester Cotton (Pc) Blended Fabric Over
Conventional Two Bath Dyeing Method. European Scientific Journal, 2015.
11(33).

57
37. Kohand, J. and J. Kim, Application of phthalimide‐based alkali‐clearable azo
disperse dyes on polyester and polyester/cotton blends. Journal of the Society of
Dyers and Colourists, 1998. 114(4): p. 121-124.
38. Bana, G.K., G.G. Gelebo, and G.K. Janka, One-bath One-step Dyeing of
Polyester/Cotton (PC) Blends Fabric With Disperse Dyes After Acetylation of
Cotton. 2021.
39. Najafi, H. and R. Assefipour, One bath method dyeing of polyester/cotton blend
Fabric with sulphatoethylsulphonyl groups Disperse/reactive dyes treatment by
chitin Biopolymer. 2008.
40. Ristić, N., et al., One-bath one-dye class dyeing of PES/cotton blends after
corona and chitosan treatment. Fibers and polymers, 2009. 10(4): p. 466-475.
41. Mokhtari, J., et al., Novel hydrolysable azo disperse dyes based on N ‐ester‐1, 8‐
naphthalimide: dyeing of polyester–cotton blends. Coloration Technology, 2008.
124(5): p. 295-300.
42. Imadegbor, F.A., K.A. Bello, and A.R. Giwa, Synthesis of some Azo disperse
reactive dyes from 2–aminothiazole derivatives and their application properties
on Polyester/cotton blend. Journal of polymer and textile engineering1, 2014. 2:
p. 46-52.
43. Bone, J., et al., One‐bath dyeing of polyester/cotton with disperse and bis ‐3‐
carboxypyridinium‐s‐triazine reactive dyes. Part 1: Factors limiting production of
heavy shades. Coloration Technology, 2007. 123(3): p. 152-162.
44. Maeda, S., et al., One-bath dyeing of polyester/cotton blends with reactive
disperse dyes in supercritical carbon dioxide. Textile research journal, 2004.
74(11): p. 989-994.
45. Niwa, T., K. Himeno, and T. Hihara, 1-Step Printing and Continuous Dyeing of
PET/Cellulose Blends Using Reactive Disperse Dyes., Advan. Colour Sci.
Technol. 2 (3), 177-190. 1999.
46. Muralidharan, B. and S. Laya, A new approach to dyeing of 80: 20
polyester/cotton blended fabric using disperse and reactive dyes. International
Scholarly Research Notices, 2011. 2011.

58
47. Bone, J., et al., One‐bath dyeing of polyester/cotton blends with disperse and
bis‐3‐carboxypyridinium‐s‐triazine reactive dyes. Part 2: Application of
substantive reactive dyes to cotton at 130° C and neutral pH. Coloration
Technology, 2008. 124(2): p. 117-126.
48. Croft, S., et al., Neutral‐fixing reactive dyes for cotton. Part 1—synthesis and
application of quaternised S‐triazinyl reactive dyes. Journal of the Society of
Dyers and Colourists, 1992. 108(4): p. 195-199.
49. Rafique, S., et al., Colour fastness properties of polyester/cotton fabrics treated
with pigment orange and various functional finishes. Asian Journal of Chemistry,
2015. 27(12): p. 4568.
50. Mimi, J.F., Study on Test Requirements of Buyer for Jacket Garments. 2019.
51. ČESÁKOVÁ, M., et al. COMPARISON OF DIGITAL AND TRANSFER
PRINTING OF COTTON FABRIC. in 8th CONFERENCE ON INFORMATION
AND GRAPHIC ARTS TECHNOLOGY.
52. Sadhukhan, B., N.K. Mondal, and S. Chattoraj, Optimisation using central
composite design (CCD) and the desirability function for sorption of methylene
blue from aqueous solution onto Lemna major. Karbala International Journal of
Modern Science, 2016. 2(3): p. 145-155.
53. Al-Etaibi, A.M. and M.A. El-Apasery, Dyeing performance of disperse dyes on
polyester fabrics using eco-friendly carrier and their antioxidant and anticancer
activities. International journal of environmental research and public health, 2019.
16(23): p. 4603.
54. Burkinshaw, S.M., Physico-chemical aspects of textile coloration. 2016: John
Wiley & Sons.
55. Moustafa, A., E. Kh, and S. Saleh, Improving dyeability of cotton fabric for vat
dyes. Research Journal of Textile and Apparel, 2011.

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