Sodium Sulphate in Digital Fabric Dyeing
Sodium Sulphate in Digital Fabric Dyeing
BATCH: 2014-15
GROUP NO. 5
SUMAIYA ALTAF
TS-14020
Certificate
Effect of Sodium Sulphate on Colour Strength and Dye Fixation of
Digitally Printed Cellulosic Fabrics
Examiner – 2 Examiner – 3
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Acknowledgement
To begin with, we would thank our University for providing us with the great opportunity
for conducting researches and for providing us the resources. We hold immense gratitude
towards the system of NEDUET.
It is an honor to have very diligent internal advisor like Dr. Saira Faisal, Assistant
Professor, Department of Textile Engineering, who supported us throughout for sharing
her vast knowledge in the respective field and for always steering us in the right
direction. We also acknowledge Dr. Salma Farooq, the Chairperson, Department of
Textile Engineering, for providing us the opportunity of growth and exposure in our field
through the projects.
We would like to express our great gratitude to Mr. Idrees Bashir, Assistant manager
laboratory, Lucky Textile Mills for giving us access to their wet processing laboratory
and enabled us to work among very helping and cooperative staff. We further extend our
gratitude to Mr. Azeem, Syntech fibres private ltd. for granting us the facility of printing
our samples, in spite of being busy with their pivotal work still managed to facilitate us.
Finally, we must express our very profound gratitude to our Families for providing all us
with unfailing support and continuous encouragement throughout our period of research
and work on this project. This accomplishment would not have come this far without
their support.
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Abstract
Sodium sulphate is widely used in reactive dyeing of cellulosic materials, in which it
helps in even dye exhaustion and migration of dye to fibre. It also helps in fixation of the
dyestuff to the cellulose materials. This project was designed in order to find out, if the
same results are obtained when Sodium sulphate is added in pre-treatment liquor of
digital printing. The versatility of digital printing is evidence for rapid growth in textile
industries for which it holds great importance. To study the effect of sodium sulphate on
colour strength, % fixation and ink penetration of digitally printed cellulosic fabrics that
are Cotton and Lyocell, a number of experiments were conducted. The results showed
that by varying the quantities of factors (Thickener, Urea, Alkali, Salt) to an optimum
level, the results were improved.
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TABLE OF CONTENTS
CERTIFICATE ................................................................................................................... ii
ACKNOWLEDGEMENT ................................................................................................. iii
ABSTRACT ....................................................................................................................... iv
CHAPTER 1 INTRODUCTION ..................................................................................... 1
AIMS AND OBJECTIVES ............................................................................................ 1
SCOPE OF THE PROJECT ........................................................................................... 1
PROJECT LAYOUT ...................................................................................................... 1
CHAPTER 2 LITERATURE REVIEW ...................................................................... 3
2.1. INK JET PRINTING ............................................................................................... 3
2.2. HISTORY OF INKJET PRINTING: ....................................................................... 4
2.3. TYPES OF INKJET TECHNOLOGIES ............................................................. 5
2.3.1. Continuous Inkjet (CIJ): ............................................................................................ 5
2.3.2. Drop on demand technology (DOD) ........................................................................ 5
2.4. PRINT HEADS OF DIGITAL PRINTER ........................................................... 7
2.5. DIFFERENCE BETWEEN SCREEN PRINTING AND DIGITAL PRINTING7
2.5.1. Time consumption ratio ........................................................................................... 8
2.6. ADVANTAGES OF DIGITAL PRINTING ....................................................... 9
2.7. LIMITATIONS OF DIGITAL PRINTING ....................................................... 10
2.8. PRINTING INKS ............................................................................................... 10
2.8.1. Pigment Ink: ........................................................................................................... 10
2.8.2. Acid Ink ................................................................................................................... 11
2.8.3. Reactive Inks .......................................................................................................... 11
2.9. GLOBAL SCENARIO OF DIGITAL PRINTING ............................................ 14
2.10. PRE-TREATMENT ....................................................................................... 15
2.10.1. Reasons for pre-treatment .................................................................................... 15
2.10.2. Chemicals and auxiliaries ....................................................................................... 15
[Link]. Thickener............................................................................................................ 15
[Link]. Alkali ................................................................................................................... 16
[Link]. Urea.................................................................................................................... 16
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LIST OF FIGURES
Figure 1-1: Gantt chart .................................................................................................... 2
Figure 2-1: General principle of operation of Inkjet Technology ................................ 3
Figure 2-2: Continuous Inkjet (CIJ) .............................................................................. 5
Figure 2-3: Drop on Demand (DOD) ............................................................................. 6
Figure 2-4: Process flow Screen vs. Digital .................................................................... 8
Figure 2-5: Route of Pigment printing process ............................................................ 12
Figure2-6: Route of Reactive printing process ............................................................. 13
Figure 2-7: Mechanism of reactive ink fixation .......................................................... 13
Figure 2-8: Sample design .............................................................................................. 21
Figure 3-1 Bar chart for colour strength ...................................................................... 34
Figure 3-2: Bar chart for dye fixation. .......................................................................... 35
Figure 3-3: Bar chart for Ink Penetration .................................................................... 35
Figure 3-4: Bar chart for colour strength ..................................................................... 36
Figure 3-5: Bar chart for % Fixation ............................................................................ 36
Figure 3-6: Bar chart for Ink penetration .................................................................... 37
Figure 4-1 Graph of Effect on ink penetration of salt ................................................. 43
Figure 4-2: Graph of Effect of Alkali on ink penetration ........................................... 44
Figure 4-3: Graph for effect of thickener on Ink penetration .................................... 44
Figure 4-4: Graph for effect of Urea on Ink penetration. ........................................... 45
Figure 4-6: Graph for effect of salt of %Fixation ........................................................ 46
Figure 4-7: Graph for effect of thickener on % fixation ............................................. 46
Figure 4-8: Graph for effect of urea on % fixation ..................................................... 47
Figure 4-9: Graph for effect of salt on colour strength ............................................... 47
Figure 4-10: Graph for effect of alkali on colour strength.......................................... 48
Figure 4-11: Graph for effect of thickener on % fixation ........................................... 48
Figure 4-12: Graph of effect of Urea on colour strength ............................................ 49
Figure 4-13: Graph of effect of salt on Ink penetration .............................................. 51
Figure 4-14: Graph of effect of alkali on ink penetration ........................................... 51
Figure 4-15: Graph of effect of thickener on ink penetration .................................... 52
Figure 4-16: Graph of effect of urea on ink penetration ............................................. 52
Figure 4-17: Graph of effect of salt on %Fixation ....................................................... 53
Figure 4-18: Graph of effect of alkali on % fixation .................................................. 54
Figure 4-19: Graph of effect of thickener on %Fixation............................................. 54
Figure 4-20: Graph of effect of urea of %Fixation ...................................................... 55
Figure 4-21: Graph of effect of salt on colour strength ............................................... 55
Figure 4-22: Graph of effect of alkali on colour strength ........................................... 56
Figure 4-23: Graph of effect of thickener on colour strength ..................................... 56
Figure 4-24: Graph of effect of urea on colour strength ............................................ 57
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LIST OF TABLES
Table 4-3 recipes of padding liqour and results of ink penetration, % fixation and
colour strength ................................................................................................................ 50
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CHAPTER 1 INTRODUCTION
AIMS AND OBJECTIVES
The pre-treatment process in inkjet printing is an essential prerequisite. The main aim of
this project was to study the effect of sodium sulphate. The main objective was to
enhance the colour strength, % fixation and ink penetration. The sharpness of print and
brilliancy of colours were also evaluated visually. Sodium sulphate has been used in
dyeing for a long period of time since it increases dye exhaustion and colour yield.
With its prolonged usage in dyeing, it will be observed that whether the same salt can be
used in pre-treatment of inkjet printing fabric and shows any significant difference or
improvement in the colour strength, % fixation and ink penetration. This was observed on
two types of fabric namely: Cotton and Tencel A300.
The scope of the project is immensely broad since inkjet printing is taking over the textile
industries rapidly. The need for sharpness of prints and enhanced penetration is
increasing with new fashion trends and mass customization [1] [2] [3]. This project was
done in two phases. In first phase, the preliminary work was done to check if sodium
sulphate has positive or negative effect on Lyocell. In the second phase, further
experimentation was done with sodium sulphate on Cotton as an ingredient in the recipe
of pretreatment liquor to study its effect on Colour strength, % fixation and ink
penetration.
PROJECT LAYOUT
The project started with literature review of the previous work done by scholars. The
chemicals and material were procured. The pretreatment was done at Lucky Textile Mills
while digital printing was done at Syntech Fibres. The evaluation of the printed samples
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was done on Spectrophotometer. From the reflectance value, colour strength, % fixation
and ink penetration were calculated using formulae discussed in Chapter 3.
Results
Evaluation
Digital printing
Pre-treatment
Recipie designing
Pre-screening
Selection of fabric
Selection of chemicals
Literature review
0 1 2 3 4 5 6 7 8
Jan Feb Mar Apr May Jun Jul Aug
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The printers used in textile printing usually do not have a wide range of colours in inks
rather they have only three or four coloured ink heads that produce a wide gamut by
combination of these colours. The inkjet printer has different types and working that will
be discussed further on. The textile market still uses screen printing for up to 85-90% of
production. However, inkjet printing has been advancing into the industry [4] due to its
unlimited shade range, its use of advanced design software, its fine spray technology that
gives sharp and detailed prints and quicker production [5].
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1980 was the year when Japans largest digital printer, Seiren began the
development of an inkjet printer that could directly print on fabric. In 1989 they
undertook the building of a facility for inkjet printing of fabric [2] [6] .
In the late 1990 the use of electrophotography for garment printing was
introduced for pastel colours on cotton and PC blends called “Natura” .
In ITMA 1999 Storks displayed its full line of digital printer; they also introduced
Amethyst, a seven-colour continuous inkjet printer [2] [6].
SGIA (Specialty Graphic Imaging Association) 2004, the USSPI (Screen Printing
Institute) introduced its Fast T-Jet TM garment printing device [6] [8] .
Other than these advancements, many more inventions and improvements were carried
out by printing companies and textile manufacturers in later years on platforms like
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ITMA 2003, Drupa 2004, SGIA 2005. However, the progress is ongoing till date [2] [4]
[6].
The ink is poured out by the nozzle at constant speed and pressure. The jet of ink is
unstable and breaks into droplets as it leaves the nozzle and are deflected to a gutter for
recirculating them according to the design that needs to be printed. The drops are
electrically charged by applying an electric field to control the trajectory. The drops are
ejected at all times that is why this type is continuous. [2]
The main attribute of DOD ink jet is that its drops are only ejected when they feel the
necessity to form the image. Among the two main mechanisms used to generate drops,
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the piezoelectric ink jets (PIJ) and thermal ink jet (TIJ) mark themselves as a sole and
preferred option.
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The KJ4A Series are for UV-curable inks and high viscosity inks. It is used for
label/packaging, sign graphics and offsets surprint.
The KJ4B Series are high speed printing of water-based inks. These series are used in
transaction printing, document printing, textile printing.
The KJ4C Series are for high viscosity oil-based inks with ink circulation feature. Used
for ceramic tile printing which requires large drop volume [9].
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Digital printing has flexible applications i.e. set up banner, a stand banner, flag of
any enterprise, wall covering, carpet, lower back-lit body,
curtains, building wrap, bed cover, a garment and many others.
In 2015, the industry is valued at approximately US$7.5 billion globally. It is
predicted that the digital printing market for garments, upholstery and technical
applications will be progressing to about 34% until 2019. [11]
Following factors have been readily reduced in industries by the invent of digital
printing
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[Link] INKS
In that context the pigment’s particle size can be 0.005-15 micron. 0.005-5 micron would
be a good particle size, next best would be 0.005-1 micron and the best size for the most
stable ink dispersion would be 0.005-0.3 micron. Brownian law of motion keeps the
particles moving and prevents them from flocculating and it is also seen that finer
particles give the best pigmentation [13] .
Pigments are not just directly applied by water solution but need assisting agents to keep
the particles suspended in solution and also preservation agents to keep the ink from
drying out or bulking up and depositing in the print head [14].
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Acid dyes are used for fibres like silk and wool etc. Acid dyes are highly soluble in
water and give the ink solution a negative charge. These dyes are applied in heavily
acidic pH medium and also called leveling dyes. One of the main draw back or limits of
the ink is that it has poor wet fastness. These cannot be used on cotton fabric [6].
Cellulosic fibres are mostly printed with reactive dyes for a number of reasons, as it
bonds with fibre leaving permanent colour, gives deeper and brighter shades and gives
good wet fastness. Similarly, reactive inks perform best in chemically bonding with
cellulosic pretreated materials. Cellulosic fabrics printed with reactive inks show high
light fastness, wash fastness and high crock.
Among the two main classes of Reactive dyes: - Monochlorotriazine (MCT) and
Monofluorotriazine (MFT), the former is preferred in digital printing because of its low
reactivity which gives stability for the storage of inks hence the chances of dye hydrolysis
are lesser.
Few properties that are important for dyes to give better results, and should be considered
before selection are as below:
[Link].Low reactivity
Dyes of low reactivity are preferred in inks as they help give stability to inks during the
storage as they are less likely to be hydrolyzed unlike in high reactive dyes.
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[Link].High Solubility
High solubility helps diffuse inks rapidly in to fibres which subsequently results in better
migration. Solubility can be increased by increasing temperature or with the addition of
more urea.
[Link].High diffusion
This property is very important in dyes; high diffusion gives good penetration of dyes in
the fabric.
[Link].Low substantivity
Dyes with higher molecular weights increase substantivity of dyes which affection the
staining of dyes on the other areas of prints during washing, to avoid such effect dyes of
lower substantivity are preferred because it decreases the chances of staining or re
absorbing of dyes on other prints. [15]
When cotton is being printed, either pigments or reactive dyes are being used. In case of
pigment printing the process is comparative short that is:
The method is economical but the only problem is appearance of duller shades and
clogging of nozzles so the run ability is also poor. However, in case of reactive printing,
the process is:
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Reactive printing by ‘all in one’ method is usually done in screen printing. In inkjet, the
process is two-phase since fabric needs to be pre-treated prior to printing.
Reactive inks give vibrant shades on cotton, silk, rayon, hemp and polyester and
reproduce wide gamut of colours [16].
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Nowadays, approximately four fabric collections are launched each year by different
brands in Pakistan. If we talk about printing heads, then digital printing with Kyocera
KJ4B print head is common for Italian digital printing machinery. Reggiani, MS, Mimaki
and Durst are some leading manufacturers whose machines are widely being used in
several textile industries in Pakistan. [4]
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2.10. PRE-TREATMENT
Ink requires the additional use of some polymeric materials for padding of substrate with
some chemicals, which is known as Pre-treatment. These chemicals cannot be added in
the inks hence the fabric is pretreated. This gives colour fastnesses, dye fixation and
important print definition to the fabric.
[Link]. Thickener
Thickener is used to give required viscosity to the pre-treatment liquor. It holds the
ingredients of the pre-treatment liquor on the fabric. It also affects the rheological
behavior of the print formulation which in turn controls penetration and migration
resistance of the colour. Thermocol MIN is the aqueous solution of an acrylic polymer.
Synthetic thickeners with anionic charges show great potential [17].
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[Link]. Alkali
Reactive dyes react with cellulose under alkaline conditions to form covalent bonds
between fibre and dye. The main function is to maintain pH. It also develops the colour
or printed fabric. It fixes dye on the fabric permanently. Sodium bicarbonate is generally
recommended for ‘all-in’ pastes and inks as it causes least hydrolysis of the dye on
storage [17].
[Link]. Urea
Urea is a hygroscopic agent and acts as a solvent for the dye and accelerates migration of
the dye from the thickener film into the cellulosic fibre. Urea is necessary for optimal
fixation of reactive dyes in hot air or superheated steam. Urea also reduces the yellowing
of cellulose under hot, dry, alkaline conditions, thus it helps in the production of bright
colours. It is inactive during printing and activates while steaming. It acts as humectant
i.e. swells the fabric to aid in the penetration of ink into the fabric. It also accelerates the
migration of dye from the thickener film into the fabric [18].
Reduction inhibitor is added to protect the colour of dye i.e. against shade changes in
printing, hence achieving excellent dyeing with good reproducibility.
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2.11. SALT
Salt is an ionic compound that is formed when acid reacts with base which is termed as
neutralization. There is a wide range of salts due to the high number of acids and bases
available. It finds application in various fields.
Salt has an extremely high affinity for water. Salt is necessary in three ways in the
process of dyeing.
It helps to drive the dye into textile during the dyeing process in textile.
The use of salt results in optimum exhaustion of dye molecules.
Salt is used as an electrolyte for migration, adsorption and fixation of the dyestuff
to the substrates, which is usually cotton or any cellulose material. [7]
Both sodium chloride (table salt) and sodium sulphate (Sodium sulphate) are used for
dyeing.
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Due to its low aquatic toxicity and the natural cycle, wide dispersive usage of sodium
sulphate does not give any major hazard to the environment, but excess concentrations
may cause damage. Sodium sulphate is not considered carcinogen nor a reprotoxic. It can
be expected that sulphate concentrations may occasionally reach levels that are high for
un-adapted organisms. At a local or small scale, the estimated concentrations are within
the natural background concentration range and far below levels that would cause severe
toxicity.
In industrial use the release of sodium sulphate goes for waste water treatment. The levels
of this salt are very low for environmental concerns and become part of Sulphur cycle.
Inhalation of dust can occur during preparation of powdered form of sodium sulphate, but
it doesn’t involve health risks. However, it can cause slightly eye irritation [19].
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During printing of a cellulosic fabric with reactive dye both the negative ions of dye
and cellulose repel each other. This happens because of the absence of salt which in
turn results in very little or no exhaustion. But in the presence of salt, it will ionize as
follows:
Then, the salt neutralizes the negative ion of the cellulose and in turn promotes attraction
of dye and fibre that aids in better exhaustion:
The presence of salt in the reactive dyeing increases the affinity of the dye towards the
cellulosic substrate. Since reactive dyes have low affinity for cellulose, the fixation can
be optimized or improved by exhausting the dye bath by adding Sodium sulphate before
fixation. [7]
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Since, the most desired characteristics of printing and especially inkjet printing is the
sharpness of the print. However, it is not the only parameter that is tested in printing,
sharpness can be places under the category of aesthetic property whereas the
serviceability parameters of the print need to be considered as well.
Any change in the recipe of the pretreatment liquor can be either positive or negative. It
can either improve print or give better durability. In case of adding sodium sulphate, it
should be noted that the ink is evenly migrated and colour is consistent. A sample design
is designed for following assessment:
For testing of the parameters and characteristics, an A4 sized design sample is made. For
objective assessment sharp-edged alphabets, edged symbol or numbers are added. For
this, the font selected is Time New Roman.
Fine lines are also added in both warp and weft direction, this is done to clearly observe if
any scattering is observed and its direction. The dimensions of the line should also be
known to evaluate dispersion visually. Solid colour filled rectangular blocks are added
for rub and washing test. If we take some localized print the rubbing test might not work
as the print will transfer to the white or non-printed area of the fabric so solid blocks are
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preferred. Also, the solid blocks are kept according to standard size. The sample size will
be taken from standards of rubbing fastness. In case of crock meter, rectangular sample of
10x4” is used.
Some important things that should be considered while designing the sample are:
Keep all the content of the design away from the selvedge i.e. nothing should get
printed at the edge.
There should be enough space in between each object or block that it has room to
be cut without cutting any other part of the design unnecessarily.
The design should not be overly populated.
Objects preferably should be with sharp edges for better objective assessment.
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In 1995 Sarah O and John R published their work on their contribution to the
optimization of inkjet printing pretreatment process to get an enhanced print and colour
yield in the localized area on fabric using quaternary ammonium compound, acting as a
colour enhancing agent used in the pretreatment in composition with other chemical and
auxiliaries.
After drying, the sheets were assessed for difference in colour yield and the results
showed better colour yield by increasing the use of colour enhancement agents [20].
In June 2004, Mehmet Kanik, Peter J. Hauser, Parrillo-Chapman and Alan Donaldson
published their work on effect of cationization on inkjet printing properties of cotton
fabric.
The cotton fabric underwent cationization process that includes cationic reagent and a
sodium hydroxide, padded with 100% wet pick up which is then wrapped in plastic and
stored at room temperature for 24 hours then washed with warm water, neutralized then
cold rinsed and dried. The cationized fabric is then pre padded with soda ash, urea and
different concentration of alginate thickener.
After printing and drying, it was observed that increasing the concentration of the
thickener increases the colour strength thus decreasing the penetration of the print that
gives a higher surface colouration and excellent wash and crock fastnesses [21]
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printer to achieve the same colour tone as of screen print and the results for stiffness, air
permeability and colour volume were superior for inkjet printing [22].
Looking for more unusual additions done to the inkjet fabric preparation process we
found out that,
In 2008, ELLIS, Scott W and LI, Xiaoqing did research based on to see if any changes or
improvement in print results occurred by modifying pretreatment as an aqueous solution
made of nonionic latex polymer along with a multivalent cationic salt solution, drying it
and then digitally printing the pretreated fabric.
This salt added to promote exhaustion. When all the samples were printed and tested,
wash fastness and crock fastness both wet and dry when compared with a fabric that was
not pretreated, it was seen that the results for all the tests were improved [23].
Also to be in touch with the effects on our concerned fabric some researches were seen
that took place,
In 2009, Kaimouz, A. W worked on Lyocell fibres (Standard Tencel and Tencel A100)
and its comparison with cotton based on its printing with digital printer using reactive
dye. The effect of each chemical, the levels of the addition, the concentrations and the
compatibility with each other was investigated. Along with, the steaming time used for
dye fixation. The result is as follows:
When the levels of the pre-treatment chemicals were varied, differences in responses
were observed. Colour strength was improved using longer steaming time and an
elevated level of migration inhibitor. Increasing urea concentration enhanced colour
strength on both Lyocell fibres, but caused a decrease on cotton. Urea had a negative
effect on dye fixation on cotton and Tencel A100, but a positive effect on standard
Tencel. The excessive amount of alkali may have an adverse effect on fixation,
particularly for inkjet printing on cotton [24].
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To keep on looking for more information from the aspect of fabric and the effect on our
required or categorized fabric we found that some scholars tried to eliminate pre-
treatment process since it is not environment friendly.
One cotton fabric was treated with dendrimer with composition to other chemicals and
the other with sodium alginate, sodium bicarbonate and urea by padding.
The fabrics were tested and showed that the dendrimer treated fabric was strongly
antimicrobial. At higher temperature, modified cotton showed better thermal stability
than unmodified cotton. Increasing the concentration of dendrimer along with Ph of the
ink, excellent properties were achieved. The value of light fastness obtained was
satisfactory [25].
In the same year work was done to enhance the migration of dye but was done in dyeing,
since the same element i.e. sodium sulphate was used in our work. Apart from the
previous researches where different elements were added for colour improvement or
migration enhancement but most of them required some extra process step or are not
applicable on industrial scale. According to a few previous researches to enhance
migration of colour in dyeing process salts like sodium sulphate, calcium or magnesium
salts were added.
To understand the effect of the salt and if it can be used for fabric pretreatment of inkjet
printing we can reference the research put out,
In 2014 by Shekh [Link] Khalid and fellow authors in which they compared the
dyeing results and behavior when added electrolytes on reactive dyeing on cotton fabric;
namely Common salt, Vacuum Salt and Sodium sulphate.
The functions of salt in dyeing is to assist in maximum exhaustion and to promote fabric-
dye interaction by cancelling out the repulsive charge of the medium by making a
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cooperative environment they were put to test. A 100% cotton jersey fabric was dyed
with reactive dyes and fellow auxiliaries: detergent, anti-foaming agent, sequestering
agent and leveling agent as the basic recipe with three solutions made and each solution
was then added with a different salt as electrolytes.
After drying the samples were tested for dyeing properties, colour fastness and pH of
solution of each salt was also tested and it was seen Sodium sulphate shows best
exhaustion for reactive dyes. It also reduces the TDS of solution by 15-20% in turn least
hardness of solution was observed in Sodium sulphate [15].
In 2016, Lei Wang, Kelu Yan, Chunyan Hu proposed an Eco steam method to print on
cotton fabric, the fabric was pre-treated and was immediately printed in wet state and
steamed directly under different conditions of steaming.
The K/S value increased for 3 mins and constant after 10 mins. Dye fixation increased
rapidly by increasing steaming time and temperature. The whitening index decreased by
increasing temperature since cotton tends to tender at high temperature. By increasing
relative humidity the K/S value and absorbed dye fixation increased.
When all the tests were compared for conventional and Eco steam process, the later
obtained high values and it is a more economical and cost friendly method [26].
So, as provided it is safe to say that the use of sodium sulphate in pretreatment of Cotton
and Lyocell fabric in inkjet printing was not done before as per our research. Even though
use of similar elements and work on the same objective has been done vastly but the
exact work on the specific fabric was not seen or found.
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CHAPTER 3 EXPERIMENTATION
3.1. MATERIALS
3.1.1. Fabric
[Link]. Cotton
The Cotton fabric used has following specifications:
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[Link].T400 Lycra:
T400 is a special type of synthetic finer that is made by combination of two different
polymers. Because of the mixing of these two polymers the product has twisted or
curled structure. The garments made by incorporation of T400 have a comfortable
stretch to them without adding any other elastic component to the fabric. It has been
noted to have very good resistance to chemicals, UV radiation and also chlorine.
While dyeing its behaviour is similar to that of textured polyester [27].
The fabric we are using is a heavier fabric that has the aesthetic like denim or jeans
fabric and has the following specifications:
GSM 320
TEAR STRENGTH:
Warp 41.5
Weft 24.3
3.1.2. Chemicals
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3.2.1. Material
The preliminary work was done on two fabrics to select the best one between them for
further research.
1. Tencel A300
2. Tencel A400
3.2.2. Recipes
Initially, five recipes were generated where all the chemicals were kept constant and only
salt was varied. For each recipe three samples of lyocell (Tencel A300) and one sample
of Tencel A400 in accordance to the provided amount of fabric were examined.
3.3. PROCEDURE
All the chemicals of the padding solution were gradually added to make the liquor up to 1
litre after adding water to the solution. Liquor was made by firstly adding urea 250 g/l
into water and stirred till totally dissolved. Sodium Bicarbonate (Alkali) and Revatol-S
(reduction inhibitor) were added 70 g/l and 15 g/l respectively, after which Sodium
Sulphate (salt) was added in 5 concentrations (10 g/l,20 g/l,30 g/l,40 g/l ,50 g/l) followed
by Thermocol MIN (Thickener) 200 g/l. the volume was made up to 300 ml for each of
the salt concentration liquors.
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3.3.2. Padding
Pad the fabric with the pretreatment liquor at padder speed of 3.0 m/s and padder pressure
of 2.9 bar to achieve 75% pickup. The padder used is MATHIS.
3.3.3. Drying
The padded fabric was dried at 120oC for 40 seconds. The dryer used was MATHIS LB-
002-016 Thermosol. After drying the fabric was wrapped in aluminum foil to keep the
pretreatment conditions optimized.
3.3.4. Printing
The printer used was TESCO printer with Kyocera print heads. Magenta reactive dyes
from SPG were used. The print design was provided by students. The DPI of image is
1200 and numbers of passes were two. The printed samples were air dried.
3.3.5. Steaming
The printed fabric needed steaming so that the ink can be fixed and properly penetrated
into the fabric. During this process, steam condensed on the fabric and was absorbed by
the thickener and urea in the printed areas. The steamer used was MATHIS LB-002-015.
The fabric was steamed at 1020C for 8.5 minutes.
3.3.6. Washing
All unfixed dye and pretreatment liquor needed to be washed off of the fabric so the
actual results could be more visible. Washing was done in following steps:
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3.4. EVALUATION
The assessment of the printed fabrics was done on data colour (D650). The aperture size
was 0.6mm. Samples were given two folds. The standard light D65 and observer 10o were
used. The samples were evaluated before and after washing to calculate reflectance
values and whiteness index.
From this reflectance value, Colour strength, dye fixation and ink penetration were
calculated. Three readings were taken from each sample to calculate the mean.
The K/S value was calculated at a single wavelength. Using Kubelka-Munk theory, the
colour strength was calculated according to the equation:
𝐾 (1 − 𝑅)2 (3.1)
=
𝑆 2𝑅
Where, R = Reflectance
[17]
[28]
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Penetration occurs when ink migrates into the capillary structure of fabric. There are
several factors on which it depends:
The pretreatment process – The quantity and appropriate selection of chemicals play a
vital role in enhanced ink penetration.
The ink properties – The viscosity of ink should be enough to penetrate inside the fabric.
Substrate structure – The weave structure of the substrate that is cotton and lyocell also
plays an important role in penetration of the ink.
𝐾
100 ( )
𝑆 𝑏
% 𝑝𝑒𝑛𝑒𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑛 = (3.3)
𝐾 𝐾
0.5[( ) + ( ) ]
𝑆 𝑓 𝑆 𝑏
[29] [30]
Where the respective K/S values are for the front and back of the fabric.
The transfer of colour from the surface of digitally printed sample to adjacent fabric
attached to it during washing is known as colour fastness to washing. This test was
performed according to standard ISO 105 CO6 A1M.
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[Link].Procedure
Prepare the liquor by dissolving 4g of detergent in 1000 ml water.
The liquor was mixed thoroughly.
A specimen of 10x4 cm was cut. The face of the specimen was attached to the
DW Multifibre strip of same dimension.
Each sample along with 10 steel balls and 150 ml of liquor were added in the 500
ml cannister.
The cannister was then sealed and placed inside the laundro meter for 45 mins at
40oC according to the standard.
The sample was then rinsed and air dried
[Link].Evaluation
The change in colour in printed sample and the staining on multi fibre were evaluated
objectively using Grey scale for colour change and Grey scale for staining respectively.
The transfer of colour from the surface of printed sample to other surface by means of
rubbing is known as colour fastness to rubbing. Both dry and wet crocking tests were
performed according to standard AATCC TM 08. In this test, a coloured specimen is
rubbed with a white crock test cloth under controlled conditions. Two specimens were
used each for dry and wet rubbing.
[Link].Procedure
[Link].1. Dry rubbing
The printed test specimen was placed on the crock meter with its diagonal
direction in the direction of rubbing.
The white test cloth was mounted with the weave parallel to the direction of
rubbing using the special spiral wire clip.
The machine covered 10 cycles in back and forth motion.
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[Link].Evaluation
The amount of colour transferred from the specimen to wet and dry test squares was
evaluated using Grey Scale for staining.
3.6. EQUIPMENT
3.6.1. Stirrer
It was used for optimum mixing of all the ingredients of the pretreatment liquor for a
required amount of time.
A pendulum tear tester was used to determine the initial tear strength of both the fabrics
in warp and weft directions
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3.7.1. Bar Charts showing the colour strength, Ink penetration and % fixation
of digitally printed Tencel A300
For Tencel A300 it can be seen in Fig 3-1 that a trend of gradual increase and decrease is
seen in K/S values. Where the highest amount of salt i.e. 50 g/l has shown some increase
in colour strength as compared to the sample with 0 g/l salt. It can be seen that adding salt
did affect the results in respect of colour strength.
K/S
19
18
K/S
17
16 K/S
15
0 10 20 30 40 50
Salt %
For %Fixation in Tencel A300 an almost gradually increasing trend can be seen in Fig 3-
2. If we see the result of 0g/l salt and 40 g/l i.e. the highest observed result it can be seen
that fixation has increased by salt addition.
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Fixation
2
1.5
1
Fixation
0.5
0
1 2 3 4 5 6
Fig 3-3 shows the penetration behaviour on adding salt in different concentrations to the
pre-treatment liquor. It was observed that the ink penetration was effected y salt addition.
The bar chart showed visible increment in salt added samples where, the penetration has
increased from 19% (0 g/l salt) to about 37% (40 g/l salt).
% Penetration
0.4
% Penetration
0.3
0.2
0.1 % Penetration
0
0 10 20 30 40 50
Salt %
By observing the figures 3-1 to 3-3 it can be said that the k/s and fixation have increased
by adding salt but most noticeably it can be seen that the ink penetration has improved.
So, the fabric can be advanced to full experimental work.
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3.7.2. Bar Charts showing the colour strength, Ink penetration and % fixation
of digitally printed Tencel A400
If we observe the trend of Fig 3-4 it is noticeable that addition of salt has an adverse
effect of the colour strength when applied on T400. Seeing at the K/S it is clear that the
result is better in 0 g/l salt recipe i.e. 15.9 and about 15.3 in 50 g/l salt recipe
K/S
25
20
15
K/S
10
5 K/S
0
0 10 30 50
Salt %
In Fig 3-5 the effect on % fixation on T400 is noted. Minute differences were seen that
were toward decrement same as seen above in colour strength. In the figure it can be seen
that fixation is best when there is no salt added in the pre-treatment liquor.
% Fixation
1.5
% Fixation
1
0.5
% Fixation
0
0 10 30 50
Salt %
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Ink penetration as shown in Fig 3-6 is the only factor that showed any improvement on
the fabric T400. Where at 0 g/l had 2.5% penetration and 30 g/l showed 14% ink
penetration .
% Penetration
% Penetration 0.15
0.1
0.05
% Penetration
0
0 10 30 50
Salt %
It is evident from the figures 3-4 to 3-6 that a decreasing trend is both colour strength and
%fixation but a noticeable improvement was observed in ink penetration at 30 g/l , when
sodium sulphate is added along with other chemicals to the pretreatment liquor in case of
digitally printed Tencel A400. It can be said that Sodium Sulphate (salt) might be added
to pretreatment liquor of Tencel T400 if good penetration is desired but, the increment in
penetration may cause loss of colour strength and ink fixation. It would be un needed to
decrease two characteristics to achieve good ink penetration when a better result can be
achieved without addition of salt.
By the above preliminary work it can be observed that Tencel A300 gives gradual
inclination toward increase in K/S, Ink penetration and %Fixation and further work on it
can be done to see if the trend of increment continues. But in T400 the results were
mostly decreasing so it won’t be further experimented with.
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3.7.3. Evaluation
The Data Colour D650 was used to measure the reflectance values of the printed samples
before and after wash under the standard light D65 and observer 10o. From this
reflectance value, Colour strength, dye fixation and ink penetration were calculated.
The pretreatment liquor had urea (150 g/l, 200 g/l and 250 g/l) [29] followed by Sodium
Bicarbonate in quantities of 30 g/l, 50 g/l ,70 g/l [29], salt in quantities of 0 g/l, 50 g/l
and100 g/l and Thermocol Min 150 g/l, 200 g/l and 250 g/l [31] [18]. Reduction inhibitor
was kept constant. Different liquors of 300 ml were prepared.
The remaining procedure was same as that of preliminary work which can be referred
from Topic 3.3, Evaluation from Topic 3.4 and Testing methods from Topic 3.5.
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Table 4-1 Recipes of pre-treatment liquor and %fixation, ink penetration, colour strength results. Dry/wet crocking ratings of
digitally printed cotton fabric
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In the Table 4-1, it can be seen that the addition of salt had not affected much on the dry
and wet crocking fastness of the printed samples. This indicated that no adverse effect on
the colour fastness was observed after the addition of salt. The colour strength , ink
penetration and % fixation were varied but mostly in range of 15-19,31-77 and 0.71-
0.91% respectively. The effect on penetration, fixation and colour strength are further
discussed.
Table 4-2 Grey scale staining on Multi fiber and colour change on printed samples
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23 4-5 5 4-5 5 5 5 5
24 4-5 5 4-5 5 5 5 5
25 5 5 4-5 5 5 5 5
26 5 5 4-5 5 5 5 5
27 4-5 5 4-5 5 5 5 5
28 4-5 5 4-5 5 5 5 5
29 5 5 4-5 5 5 5 5
30 4-5 5 4-5 5 5 5 5
31 4-5 5 4-5 5 5 5 5
In table 4-2, the ratings observed on grey scale for colour change and staining were
noted. It was seen that very minute or barely noticeable colour change occurred after
washing and the multi fibers had no staining except for a slight tint on the cotton fabric.
This can be taken as an indication that addition of salt has not affected the washing
fastness of the printed cotton.
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[Link]. Salt
In Fig 4-1 an increasing trend can be seen with added amount of salt. It can be seen the
addition of salt in pre-treatment shows a noticeable improvement in penetration. The best
result is seen on 100 g/l salt which is 65% whereas on 0g/l the fixation% is 51%. The
increment of about 15% is seen which is due to the salt acting as a migrating agent and
high amount of salt promotes even more migration beyond the surface i.e. inside the
fibre.
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[Link]. Alkali
The variation in amount of alkali shows an increase then decline as the amount is
maximized. The best penetration was achieved at 50 g/l alkali that is 55% which is better
as compared to 45% and 35% at 30 g/l and 70 g/l respectively as shown in fig. 4-2. The
improved penetration among the three quantities is noticeable.
[Link]. Thickener:
A dip was seen by the effect of thickener on penetration. The highest amount 250g/l
showed highest penetration i.e 57.9% whereas 55.6% was shown on 200 g/l. The change
in penetration was minute at the different values of thickener. The results obtained from
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Department of Textile Engineering
150g/l and 250g/l of thickener were almost same as the difference between the two is
negligible thus 150 g/l is preferred.
[Link]. Urea
The different quantities of urea showed minor dip followed by gradual increase as seen in
Fig 4-4. The higher amount of urea, 250 g/l aided the fiber swelling at a higher level and
resulted in better penetration, 77%, as compared to 150 g/l and 200 g/l where the
penetration is 58% and 56% respectively.
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Added salt showed a dip in %fixation and then slight increment. The difference is very
small i.e. at 0 g/l, the fixation is 0.819% and on 100 g/l, it is 0.81%. The dip at 50 g/l is at
0.755%. It can be concluded that the values of % fixation can be neglected.
[Link]. Alkali
Alkali is basically used to aid dye fiber interaction at fixation stage and according to Fig
4-6 it can be seen that adding high amounts of alkali had no improved effect on fixation.
The maximum fixation was achieved at the lowest amount, 30 g/l. Excess amount of
alkali can cause the faster ionization which can cause unnecessary hydrolyzation. So,
minimum amount of alkali is preferred.
[Link]. Thickener
Fig 4-7 shows that the fixation is highest at 200 g/l. However, it is then decreased with
further addition of thickener. High amount of thickener can cause adverse effect on the %
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Department of Textile Engineering
fixation as a thicker layer of thickener may block the ink and prevent it from bonding
with the fabric.
[Link]. Urea
In Fig 4-9, it was seen that high amount of salt increased the colour strength. The graph
has a curvature that goes towards increment of K/S (18.5) at 100 g/l of salt as compared
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to 0 g/l which gives 17.0. The change is noticeable so the addition of salt can be done in
pretreatment since it enhanced colour strength of printed fabric.
[Link]. Alkali
In Fig 4-10, it is observed that addition of alkali shows a curvature. The best result is seen
at 30 g/l alkali where colour strength is about 18.00. However, at highest amount i.e 70
g/l, the colour strength has increased to 17.5 but the difference is not exceptional. This
might be due to the fact that less amount of alkali provided optimum ink-fiber interaction
and less hydrolyzation of the ink.
[Link]. Thickener
Fig 4-11 shows that added amount of thickener has decreased the colour strength
whereas, the maximum colour strength is seen at 200 g/l at 36.4. More thickener can form
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Department of Textile Engineering
a heavier layer on the fabric and can swell up and block the fabric surface in fixation
stage. Since the ink is not allowed to interact with the fabric, this results in lower colour
strength.
[Link]. Urea
Increased amount of urea has adverse effect on colour strength as seen in the graph in Fig
4-12. Although urea had good results for fixation at higher quantity but it has a
decreasing trend in colour strength. Maximum colour strength is seen at 150 g/l as 18.0.
This might be due to the higher amount of alkali causing hydrolyzation of ink which in
turn washed off most of the ink resulting in low colour strength.
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Table 4-3 recipes of padding liqour and results of ink penetration, % fixation and colour strength
Recipe Ink % %
U A T S Penetration Fixation Penetration
1 150 30 250 0 20.11 1.19 20.11
2 150 50 200 50 17.16 1.21 17.16
3 200 50 200 50 20.28 1.23 20.28
4 250 70 250 100 49.38 1.60 49.38
5 200 50 200 50 19.71 1.17 19.71
6 250 50 200 50 33.22 1.33 33.22
7 250 70 150 0 38.63 1.18 38.63
8 200 50 200 50 45.04 1.87 45.04
9 150 30 150 100 36.59 1.50 36.59
10 200 50 200 100 41.99 1.55 41.99
11 150 30 150 0 28.16 1.32 28.16
12 150 70 250 100 42.45 1.39 42.45
13 250 30 150 0 50.41 1.13 50.41
14 250 30 250 0 38.23 1.24 38.23
15 150 70 150 100 37.47 1.51 37.47
16 250 30 250 100 51.63 1.13 51.63
17 250 70 150 100 - - -
18 200 50 200 50 39.73 1.29 39.73
19 200 50 200 50 28.15 1.25 28.15
20 250 30 150 100 30.29 1.24 30.29
21 200 50 200 50 23.21 1.20 23.21
22 200 30 200 50 23.52 1.24 23.52
23 150 70 150 0 19.20 1.30 19.20
24 150 70 250 0 15.74 1.26 15.74
25 200 50 200 50 29.81 1.33 29.81
26 200 50 250 50 24.86 1.21 24.86
27 200 70 200 50 50.69 3.26 50.69
28 150 30 250 100 51.47 3.05 51.47
29 200 50 200 0 56.67 3.98 56.67
30 200 50 150 50 58.57 3.19 58.57
31 250 70 250 0 45.01 3.09 45.01
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The graphs of ink penetration, % fixation and colour strength are discussed in 4.3. The
physical testing i.e. rubbing fastness and washing fastness of Tencel A300 could not have
been done due to short time frame.
40
38
36
%P
34
32
30
28
26
0 50 1 00
Salt- g/l
In figure 4-13, it can be seen that the penetration goes from 30% to 28% and then
gradually increases to 41% at 100 g/l. This occurs because the added amount of salt
assists in diffusing the ink into the fabric. The salt acts as an electrolyte and when added
to the pretreatment liquor, it increases attraction between the fabric and ink.
.
[Link]. Alkali
28.0
27.5
%P
27.0
26.5
26.0
25.5
30 45 60
Alkali - g/l
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In Fig 4-14, it can be seen that the addition of alkali has shown a downward trend when
added in maximum quantity. But, the peak of curve is observed at almost 45 g/l which
means equilibrium is achieved and further addition of alkali will decrease the penetration.
Alkali is used to increase the attraction between reactive groups of ink and hydroxyl
groups of cellulose and helps on the steaming stage.
[Link]. Thickener
In Fig 4-15, it can be seen that the addition of thickener has shown a downward trend
when added in maximum quantity. However, the peak of curve is observed at 150 g/l
which means more than this amount of thickener, penetration will rather decrease.
[Link]. Urea
30.0
27.5
%P
25.0
22.5
20.0
1 50 200 250
Urea - g/l
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Urea showed an increase in penetration that is due to the property of urea to swell fibers
to help dye penetration. It can be seen that addition of 250 g/l urea has shown an
increased penetration of up to 32.5% due to maximum swelling of fibers as compared to
150 g/l which shows below 20% penetration according to Fig 4-16.
0.78
0.76
0.74
%F
0.72
0.70
0.68
0.66
0 50 1 00
Salt - g/l
.
Figure 4-17: Graph of effect of salt on %Fixation
In Fig. 4-17, the % fixation shows initial increase then a decreasing slope at maximum
amount of 100 g/l which in turn means that if salt is added more than 50 g/l it would
decrease the fixation. This might be due to the salt’s reaction mechanism since salt helps
to migrate the ink into the fiber but excessive amount of salt might excites the ink which
might rush to the fiber but not get space to fix or spread throughout.
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[Link]. Alkali
Effect of Alkali on %Fixation
0.82
0.81
0.80
0.79
%F
0.78
0.77
0.76
0.75
30 50 70
Alkali - g/l
In Fig 4-18 it can be seen that by the addition of alkali, a decreasing trend for % fixation
is observed where the maximum fixation is at 30 g/l i.e. 0.819% and lowest at 70 g/l,
0.75%. This might have been due to the fact that higher amount of alkali can increase the
rate of interaction between ink and fiber that it becomes excessive and the dye starts to
hydrolyze in turn does not fix and washes off later.
[Link]. Thickener:
0.790
0.785
%F
0.780
0.775
1 50 200 250
Thickener - g/l
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[Link]. Urea:
0.80
%F
0.79
0.78
0.77
1 50 200 250
Urea - g/l
In Fig 4-19, the inclined graph shows that % fixation increases as the amount of urea is
increased in the pretreatment liquor. It is maximum at the highest amount of 250 g/l
which is 0.81%.
In Fig 4-21, it has been observed that a uniform curvature is obtained which means that
the colour strength at 0 g/l and 100 g/l both give same colour strength which may be
taken as an evidence that added salt will not affect the colour strength but can enhance
the fixation and penetration as seen in fig 4-17 and 4-13 respectively.
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[Link]. Alkali
Higher amount of alkali shows downward trend as seen in figure 4-22, where best result
is at 30 g/l. The reason being same for colour strength too as the hydrolysis of ink effects
the k/s equally.
[Link]. Thickener
In Fig 4-23, the best result is seen at 200 g/l of thickener where it gives 16.49 K/S. The
decreasing trend seen in colour strength at high level of thickener can be attributed to
excessive swelling.
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[Link]. Urea
Fig 4-24 shows that best result is achieved on 15 g/l of urea and further addition of urea
has caused the graph to adopt a slope which gradually decreases to 16.3 at 250 g/l.
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CHAPTER 5 CONCLUSION
In this project, the colour strength, % fixation and ink penetration by the addition of
sodium sulphate was studied.
To achieve the objective of the project, practical work was highly essential as it led to
results that can be compared to conventional pretreatment and noted for any differences
that are either positive or negative.
Evaluation of printed samples showed that the use of sodium sulphate in pre-treatment
has given different results for both the fabrics. According to the graphs, it is evident that
% Fixation, penetration and colour strength are increased for cotton fabric which may
allow further work. But, the results for Tencel A300 were not noticeable enough to carry
out further research. The usage of sodium sulphate in digital printing is justified for
cotton as it can be used to enhance observed parameters.
The following recipes can be deduced after carrying out all the experiments and studying
the results:
Cotton (100 g/l salt, 150 g/l urea, 30 g/l alkali and 200 g/l thickener).
Tencel A300 (100 g/l salt, 250 g/l urea, 30 g/l alkali and 150 g/l thickener)
FUTURE WORK
Further working on this project can be carried out. Cost Analysis for the process of ink jet
printing after addition of sodium sulphate can be done. Image analysis for sharpness can
also be done. The dispersing of print with added sodium sulphate along with effluent
treatment ac also be studied. Moreover, the optimized recipes can be varied for more
accurate results.
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[30] "Catal DO, ÖZGÜNEY AT, KUMBASAR E. THE INFLUENCE OF RHEOLOGICAL PROPERTIES OF
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