Professional Documents
Culture Documents
By
March 2011
“This copy of the thesis has been supplied on condition that anyone who consults it is
understood to recognise that the copyright rests with its author and that no quotation from
the thesis and no information derived from it may be published without the prior written
consent of the author”
ii
Abstract
This project was an effort towards improving the durability of flame retardant finish
on polyester cotton blended fabric by using a compatible cross linker with the finish. The
purpose was to check whether the addition of cross linker to the recipe of flame retardant
improves the washing durability of the flame retardant finish on polyester cotton blended
fabric.
The fabric selected was Polyester Cotton (50/50) blend. In the practical work the
samples were treated with different concentrations of both the cross linker and the Flame
Retardant. From each recipe the samples were cured at three different temperatures. The
purpose of cross linker was to improve the durability and the purpose of varying curing
temperatures was to improve the fixation and washing durability. Although the Flame
Retardant finish didn’t prove to be durable to washing but some interesting results and
conclusions were obtained.
iii
Dedication
Dedicated to
AND
Those who love me for what I am.
iv
Acknowledgements
Selecting this project was not less than a challenge for me, as in the initial stages I got
some discouraging comments from the people around. But after discussing it with the
HEAD OF THE DEPARTMENT Dr. Rashid Masood, I was quite keen to do this
project. Mr. Rashid really motivated me by explaining what research is and how brave
you have to be without thinking about the results much. I would like to thank Dr. Rashid
Masood as he was always very helpful when ever I went to ask for the right direction.
As this project was carried out under the supervision of Mr. Qummer Zia, I really
want to thank him as he explained me the steps and the guidelines to achieve the project.
And last but not the least I would like to thank the Staff of Textile Processing
Laboratory, as they were very helpful and polite.
v
Table of Contents
Table of Contents................................................................................................................vi
Introduction:.........................................................................................................................1
Background:.....................................................................................................................1
Area of research:..........................................................................................................1
Research problem:.......................................................................................................2
Significance of the project:..............................................................................................3
Theory:.............................................................................................................................3
The fire triangle:..........................................................................................................4
Hazards of textile burning:...........................................................................................5
Burning behavior of textiles materials:........................................................................6
Mechanism of combustion:..........................................................................................8
Textile flame-retardants:................................................................................................10
History:......................................................................................................................10
Functioning of flame retardants:................................................................................10
Polyester cotton blend:...................................................................................................14
Polyester:....................................................................................................................14
Cotton:........................................................................................................................15
Blend benefits:...........................................................................................................15
Blend cons:.................................................................................................................15
Uses:...........................................................................................................................15
Literature review:...........................................................................................................16
Significant researchers and their findings:.................................................................16
Flame-retardants under study:....................................................................................18
Further identified areas of studies:.............................................................................19
Objective and scope of the project:................................................................................19
Objectives:.................................................................................................................19
Scope of the project:..................................................................................................19
Experimental......................................................................................................................21
Materials:.......................................................................................................................21
Fabric specifications:.................................................................................................21
List of chemicals and auxiliaries used:......................................................................21
Machinery & equipment:...............................................................................................28
Application equipment:..............................................................................................28
Testing equipment:.....................................................................................................29
Methods:........................................................................................................................29
Application methods:.................................................................................................29
Testing methods:........................................................................................................30
Project work plan:..........................................................................................................31
Results and discussions:.....................................................................................................35
Results............................................................................................................................35
Results for Flame Retardancy:...................................................................................35
Results for tear strength:............................................................................................38
Results for Tensile Strength:......................................................................................42
Overall discussion:.........................................................................................................46
Summary:...........................................................................................................................47
vi
Key findings of the project:...........................................................................................47
Implications of the findings:..........................................................................................48
Suggestions for the future work:....................................................................................48
References:.........................................................................................................................49
vii
List of Tables
viii
List of figures
ix
Chapter 1
Introduction:
Background:
Area of research:
Textile finishing:
Mercerizing, singeing, flame retardant, water repellent, water proof, antistatic finish,
peach finish etc are some of the important finishes applied to textile fabric [3].
The properties of synthetic fibers like polyester, polyamide etc are essentially
different from natural fibers like cotton and wool. Hence the finishing sequence is
different for both natural and synthetic fiber.
• Bio-polishing
• Mercerisation
• Raising
• Peach Finish
• Fulling Calendering
• Sanforizing
• Crease Resist Finishing
• Anti-Microbial Finishing
• Flame Retardant Finishing
• Heat Setting
• Filling Process
1
• Hydrophilic Finishes
• Anti-Pilling Finish
• Anti-Static Finish
• Non-Slip Finishes
• Flame Retardant Finishing
• Anti-Microbial Finishing
In order to induce flame retardancy in a fiber or fabric the burning cycle must be
interrupted in one or more of the three steps of burning cycle [12].
Research problem:
The gains in textile performance obtained from blending polyester and cotton are
not carried over into the flame retardant performance of the textile. This is due to the
thermosetting properties of polyester. Also cotton is hydrophilic so when a flame
retardant finish is applied, it is absorbed only by cotton not by polyester.
2
Due to this better or durable flame retardant results are not achieved on pc blend
fabric. Also by the application of flame retardant finish on pc blend certain properties of
the fabric are affected i.e. loss of strength, change in color etc
The main focus in this research is to achieve the same degree of flame retardancy
properties in pc blend fabrics as achieved in 100% cotton or 100% polyester alone.
Theory:
For many years such finishes for textiles there, which would not burn when
exposed to flame or heat. Such finishes are called flame retardant finishes.
After the Second World War the flame retardant finishes have become
established, this due to the recognition of different hazards of burning of textiles. Also the
need to produce effective durable finishes for textiles, which not affect the handle,
comfort, and aesthetics of the fabric rather impart good flame retardancy in the fabrics.
Fire:
Fire is our oldest technology and has been crucial to each step in our
development. Now fire, through controlled burning, provides most of our energy,
which in turn causes nearly all the world's air pollution [1].
Unwanted fires, ranging from the burning of textiles to a major fire disaster
resulting in hundreds of deaths, are a growing problem. The desire for textiles having
3
a reduced tendency to ignite and burn has been recognized for considerable time
during man’s recorded history. The use of asbestos as flame-resistant material has
been recorded in Roman times [3].
Fuel:
There must be a source of fuel for any fire to take place. In most cases the fuel
does not itself burn (except if it is a gas) but breaks down under the influence of the
applied or generated heat to produce combustible volatiles that are then burnt. This is
important in terms of how some materials may initially ignite but then form a ‘char
layer’ that prevents the formation of further gases and further combustion.
Oxygen:
This is a basic component of combustion.
Ignition source:
The ignition source is needed to heat up the fuel sufficiently to generate volatiles
and then to ignite them. In the case of a gas the ignition source can act directly on the
gas.
Fuel
Ignitio Air
n
source (O2)
(Heat)
4
How does fire initiates?
At first the fuel molecules react slowly with oxygen, generating heat, which
warms the rest of the material [3]. As they react, they form unstable radicals, capable
of reacting billions of times faster than ordinary molecules. Radicals are fragments of
molecules that are capable of reacting with other stable molecules, forming even
more radicals. This starts a chain reaction and the radical concentration increases.
This makes the reaction go faster still, increasing the radical concentration
exponentially. When it reaches a certain value, ignition occurs. Flames contain high
radical concentrations.
Fires tend to grow in stages [3]. The graph shows that fires start with a slow
induction period, but once ignition is reached they grow very quickly, until they are
limited by the access of oxygen, reaching a steady state. Once the fuel is consumed,
the fire decays.
5
burning of tents. After that in 1998 fire retardant tents were used this worked very well
[4].
Cotton and cellulosic materials are the mostly flammable but at the same time
cotton is used almost in every other textile. So to avoid any hazards there is a requirement
of flame retardancy on textiles made up of cotton or any other natural or synthetic
material.
6
concentration that they induce as a function of their concentration. The limiting
oxygen index (LOI), also called the critical oxygen index (COI) or oxygen index
(OI).
The LOI values of some main textile fibers are given in the table. Wool has LOI
value higher than the oxygen contents of normal air, which suggests that wool fibers
are inherently less flammable than most other textile fibers [4].
Construction of fabric:
The flaming properties of fabric also depend upon its structure and nature of its
surface as well. For the rapid burning of a fabric its fibers must have ready excess to
oxygen (air) to allow burning to continue after initial ignition. Fabrics with compact
weave, high twist yarn and close structures are relatively less flammable. Knitted
fabrics having air trapped in their loops catch fire more readily than woven fabrics.
Generally, we may say that an open mesh fabric will burn very readily [7].
7
Also, if the fabric surface has been brushed or otherwise given a pile character
with a large amount of air trapped between the protruding fiber ends then this will
much assist the fabric to burn rapidly. Cotton flannelette is of this type and it will
allow the flame to spread exceptionally rapidly over its surface. The protruding fiber
ends will burn before the real burning of fabric itself starts [7].
Mechanism of combustion:
In order to understand the mechanisms of flame-retardants, the mechanism of
combustion should be clarified first. Cellulose combustion is a process that occurs in
stages:
Pyrolysis:
When heat is applied, the temperature of the fiber increases until pyrolysis
temperature, TP, is reached. Due to the action of heat, the fiber undergoes
irreversible chemical changes and produces non-flammable gases (carbon dioxide,
water vapours and higher oxides of nitrogen and sulfur), carbonaceous char, tars
(liquid condensates) and flammable gases (carbon monoxide, hydrogen and many
oxidisable organic molecules). For cotton, the temperature at which rapid pyrolysis
is triggered is 300oC [3].
Combustion:
The temperature continues to rise and the tar also pyrolyse, producing more non-
flammable gases, char and flammable gases. Eventually, the combustion
temperature, TC, is achieved. In combustion process, the flammable gases combine
with oxygen and a series of gas phase free radical reactions take place. These are
highly exothermic reactions and produce large amount of heat and light. The heat
produced during combustion is used for further pyrolysis of the fiber [3].
Post- combustion:
After the repeated cycles of pyrolysis ad combustion, a carbonaceous residue
(char) remains [6]. It undergoes slow oxidation (also exothermic) and continues to
glow until it has been completely burned up [3].
8
Classification of burning fabric into different zones:
A fabric undergoing combustion will present the following zones [13]:
Heat Radiation
Flammable gases
Non-flammable gases
Fibre
Heat
Figure 1.3 Combustion cycle for fibers
9
Textile flame-retardants:
Flame retardants are materials that inhibit or resist the spread of fire. These can be
separated into several categories: *Minerals such as asbestos, compounds such as
aluminium hydroxide, magnesium hydroxide, hydromagnesite, antimony trioxide,
various hydrates, red phosphorus, and boron [15].
History:
Chemical flame retardants have been used since Roman times when they
prevented siege towers from catching fire. However, the first patent on a flame retardant
was the British Patent 551, patented by Obadiah Wilde in 1735 to flame retard canvas for
use in theatres and public buildings. In the plastics industry, brominated flame
retardants were first used in cellulose nitrate which is extremely inflammable [15].
In the early 1970’s, the increasing use of flammable materials such as plastics in
electrical equipment or synthetic fibers in sofas and curtains led to the wider use of flame
retardants. At this time, manufacturers of appliances and furniture began such as plastics
for appliances and polyurethane foam and fiber-based fillings for furniture, moving away
from traditional materials such as wood and metals. While these new materials provided
many benefits, they had one problem - they were far more combustible than the materials
they replaced. Flame Retardants are able to contribute greatly to reducing the risk of fires
providing safety in the home and in public places [15].
The effective fire retardants work in a number of ways to disrupt this cycle. We
broadly classify the working mechanisms of flame-retardants into following two classes
[8].
10
1) Condensed phase mechanism
2) Gas / vapour phase mechanism
Working mechanisms of flame-retardants
11
Coating insulating material:
In this approach, a material is applied that forms an insulating layer around the
fiber at temperatures below the fiber pyrolysis temperature. Generally, boric acid and
its hydrated salts are used in this capacity. These are low melting point compounds
and when heat is applied, they release water vapour and produce a foamed glassy
surface on the fiber. In this way fiber is insulated from the applied heat and oxygen
[8].
Actually, these phosphorous esters catalyse the dehydration and prevent the
formation of undesired levoglucosan, which is the precursor of flammable volatile.
12
350 oC
Levoglucosan
MX HX + M*
{MX is halogen-containing compound}
*
H + HX H2 + X*
HO* + HX H2O + X*
RH + X* R* + HX
R* + X* RX (not flammable)
13
Free radical reactions during combustion of halogen (X) containing material
Sb + HO* SbOH
SbOH + H* SbO + H2
SbO + H* SbOH
SbX3 SbX2 + X*
RH + X* R* + HX
R* + X* RX (not flammable)
Fabrics made of a polyester cotton blend are exactly what they sound like, made
from fibers of both the natural cotton and the synthetic polyester. While both fibers have
pros and cons, a blend is often used in garments to give the consumer the benefits of
both.
Polyester:
Polyester is a manmade polymer material. It is made from coal, air, water and
petroleum products. Polyester is a strong fiber that keeps its shape and therefore resists
wrinkling. The fiber does not withstand medium to high temperatures and melts and
burns at the same time, therefore ironing polyester must be done at a cool temperature, if
at all. Threads of polyester last for a long time and wear well, so are used for many
14
garments and sewing projects. Polyester does not shrink like its natural counterpart and
holds dye extremely well, a good thing for textile artists, but bad for stain-removal from
polyester items. Polyester was extremely popular in the 1950s but since then is used more
as a blend than the main fiber used for garments or fabric [1].
Cotton:
Cotton is an all-natural fiber made from the pod of a cotton plant. It is the
principal fiber used in making the world's clothing. Cotton is known for being light, cool,
comfortable and absorbent. Many people describe cotton as a fabric that "breathes." It is
also easy to dye and to clean, though dyes do not hold as fast to natural fibers as to the
synthetic fibers of polyester. Cotton can withstand high temperatures, but does wrinkle
easily and shrinks with washing [1].
Blend benefits:
A polyester cotton blend can be versatile, as it most likely retains the coolness and
lightness of the cotton fiber, but also adds the strength, durability and wrinkle-resistance
of polyester. A polyester cotton blend should only shrink slightly in comparison to a
garment or fabric that is 100 percent cotton. This blend is often preferred by at-home
sewers and quilters as it is extremely easy to sew [1].
Blend cons:
Adding polyester to cotton can cause unattractive pilling of the fabric and make
the fabric not withstand high temperatures as well. Many people prefer pure cotton to a
polyester blend cotton in clothing that they need to breathe, as the blend does not breathe
or stay as cool as pure cotton [1].
Uses:
Polyester cotton blend is mostly used in the garment industry to make clothing
that people want to be able to wash and wear without having to iron and that will be
tougher than a 100 percent cotton blend and withstand more washing. Many home sewers
15
prefer polyester cotton blends as it is more forgiving and easy to sew than pure cotton, as
it wrinkles and shrinks less [1].
Literature review:
Peter J. Wragg CCol. ASDC. CText.ati. OF Schill & Seilacher explains the criteria to
be considered in the flame retardant treatment of textiles. There is much to be achieved
by using topical treatments to FR treat textiles and Schill & Seilacher believe that they
have a proper place in the textile industry. The requirement to control the hazard involved
in using textiles must be reconciled with our natural desire to enhance our living and
working environments. Topical flame retardant treatments will have an increasing role to
play in the future [5].
Judi Barton, profiles the market for flame retardant chemicals. J. Barton discusses the
market share of different flame retardants. The market share of Bromine flame retardants
is 39%, phosphore flame retardants 24%, inorganic flame retardants 27%, chlorine 6%
and melamine 4% [9].
Thomas Paulini. Found that FLAMMEX DS is a new, durable flame retardant that is
specially designed for the flame proof finishing of polyester. If properly applied the
product is durable up to 50 launderings or 10 chemical dry cleanings [6].
Thomas Futterer, Chemist Fabrik Budenheim Germany, presented recent flame
retardancy solutions for PP (polypropylene) based on ammonium phosphates (specially
treated to improve thermal stability, facilitating processing of plastics containing the
product) and for PBT, PET (polyamides and thermoplastic polyesters) used particularly
in automotive parts, based on melamine polyphosphate. These flame retardants act by
accentuating charring of the plastic surface in contact with a flame, enabling the material
to be self-extinguishing (ignition resistant) and also reducing smoke emissions [10].
Rudi Borms, Dead Sea Bromine Group, presented developments in “reactive”
brominated flame retardants for fire safety treatment of soft and rigid foams (PUR =
polyurethane) for furniture, building and other applications. These molecules react with
the foam polymer molecules themselves, thus being fixed into the foam matrix. Tests
show zero leaching of the flame retardant out of the treated foam, even with strong
16
chemical solvents. The most recent developments in such reactive molecules enable fire
safety to be achieved whilst offering good material quality (foam flexibility, durability),
without “scorching” in application [10].
Reiner Saurwein, Nabeltec GmbH, presented recent developments in mineral flame
retardants, showing both the importance of quality/characteristics of aluminum hydroxide
(ATH) and the potential of flame retardancy synergies with other minerals such as
boehmite (aluminum oxide hydrate) and zinc borate. New ATH products without organic
post-treatment but with good powder properties enable good product handling and
improved treated polymer viscosity, rheology and extrudability to be achieved. Boehmite
has proven an effective synergist for ATH in certain polymer (e.g. vinyl acetate free
polyolefin’s), enabling mineral loadings to be reduced and polymer properties to be
improved [11].
François Minec & P. Lambert of Atofina presented developments in TV fire safety
specifications. The authors presented a new halogen-free V1 flame resistant polystyrene
system for TV casings, capable of achieving fire resistance comparable to V0, and
useable in manufacturers’ existing polystyrene (HIPS) processing equipment [11].
Sebastian Haröld, Clariant GmbH, presented a new generation of flame retardants for
polyamide polymers (PA66) based on phosphinates. These compounds enabled UL94-V0
classification to be achieved in glass fibre reinforced polyamides at relatively low flame
retardant addition levels (15-18% by weight) with good mechanical properties, including
electrical non conductivity, being maintained, compatible with injection moulding for
demanding applications in the electrical and electronics industries[11].
Alexander Morgan, Dow Chemicals, also discussed the use of nano particles of clay as a
flame retardant additive to plastics, considering both natural and synthetic clays, and also
organically treated clays. These authors again indicated that nano clay addition could
reduce peak heat release, but accelerate the reaching of the peak. The organo-clays
offered somewhat better flame retardancy properties than either natural or synthetic
untreated clays, but in no case were able to alone achieve UL94-V0 fire safety. The
mechanism of fire retardancy of the nano clays is hypothesized as resulting from
synergistic accentuation of base polymer charring [10].
17
Birgit Östman, Trite Sweden, presented ongoing developments in know-how concerning
flame retardancy for wood and timber. Ordinary untreated wood will generally achieve
Euro Class D for reaction to fire performance [10].
INTUMESCENT SYSTEMS:
These consist of an acid source, a carbon supplier and an expansion agent. The
effect of the system is based on the formation of a heat insulating, carbon rich foam
layer and on foam expanding or swelling the mixture [7].
18
PERMANENCE OF FLAME-RETARDANTS:
Permanence can be achieved by reactant cross linker, self-cross linker, migration
or ion-pair bonding [7].
To introduce an application procedure which has less waste, gives good results
and should be environment friendly.
Objectives:
19
The flame retardant properties in pc-blended articles will avoid the hazards of
burning.
Also there is a scope to look into the application of flame retardant finishes. As
some of the flame-retardants are not environmental friendly i.e. Halogen containing
flame-retardants. So there is a scope in this project to look into the chemistry and
application of flame-retardants to avoid the environmental hazards.
Also the properties of the substrate that get modified after the application of
Flame retardant finish can be analyzed and compared.
20
Chapter 2
Experimental
Materials:
The substrate used for the application of chemicals was 50/50 polyester/cotton
blended fabric.
Fabric specifications:
Brief Description of the chemicals and their compatibility table is given on the
next page:
21
Compatibility check:
22
Pyrovatex CP:
It is a fiber reactive organic phosphorus compound. As this flame retardant is
phosphorus based so it work as a condensed phase flame retardant.
Ecology/toxicology:
Toxicologically and dermatologic ally tested.
Application:
Dissolving/diluting:
• PYROVATEX® CP NEW durable flame retardant is added to cold water
with stirring, a homogeneous distribution in the bath must be guaranteed.
23
• Softeners such as ULTRATEX® FSA NEW or TURPEX® ACN NEW
are added diluted with an equal amount of water.
Required amount:
The required amount of PYROVATEX® CP NEW durable flame retardant
depends on the standard to be met, the type of fiber, area weight and construction of
the goods as well as on a possible blend with synthetic fibers such as polyester.
Process:
Impregnation:
• The goods are impregnated on a pad mangle.
Drying:
• Drying on stenter should be carried out with maximum overfeed.
• The temperature in the other zones should not be higher than 130 °C to
minimize migration.
• If the goods are not cured immediately, they must be prevented from
absorbing moisture from the air by being rolled up and wrapped in plastic
film.
Curing:
• In the curing oven 5 min at 150 °C must be guaranteed.
24
• In the case of curing on stenter 30 to 60 sec at 170 °C are sufficient.
• It is advisable to check the curing effect at regular intervals.
Washing off:
• The phosphoric acid used as a catalyst for cross linking must be removed
from the substrate, washing off is indispensable.
• Usually, they are washed off in an open width washing machine with not
less than 5 boxes, or in a winch. Smaller lengths of material can be washed
off in a jig.
• Alkali is added to the washing bath to neutralize the goods and to make
the goods alkaline and therefore reduce hydrolysis of the finish during
storage of the finished goods. With a continuous process using open width
washing machines, alkali must be added in proportion to the rate of fabric
throughput.
• After neutralizing and rinsing, they should be slightly alkaline and have a
pH of 8–9.
Knittex RCT:
Well balanced and highly reactive cross linking agent with low formaldehyde
content for easy care finishes with highest effect level at low curing temperatures.
25
• The properties are retained even after several washes respectively
dry cleaning cycles
Application:
The product is normally applied by padding.
Dissolving/Diluting:
KNITTEX® RCT cross linking agent can be diluted with cold water.
Application:
• Padding with a liquor pick-up of 60–90 %
• Bath temperature approx. 20 °C
Curing conditions:
• On a baker/hot flue (after previous separate drying)
• Curing: 2–3 min at 130 °C (air temperature)
• Drying and curing (controlled by fabric temperature) on stenter
• Curing: 50–70 sec at 130 °C (fabric temperature) or
• 20–30 sec at 140 °C (fabric temperature) or
• 10–15 sec at 150 °C (fabric temperature)
Invadine PBN:
Special wetting agent for finishing
Application:
The product is normally applied by padding.
Dissolving/diluting:
26
• INVADIN® PBN special processing agent is diluted with an equal
amount of cold water.
Required amount:
5–15 ml/l INVADINE® PBN
Uses:
Additive and softener for crease-resistant, shrink proof, non-iron, wash and wear
finishes on natural and regenerated cellulose fibers and their blends with synthetic
fibers
Application:
TURPEX® ACN NEW textile softener can be applied by padding, dip spin or
minimum application techniques.
Dissolving/diluting:
• TURPEX® ACN NEW textile softener can be diluted with cold water.
27
• If combined with cellulose cross linking agents, filler, additives, etc., these
products must be pre-diluted; TURPEX® ACN NEW textile softener
should be added last.
Required amount:
Padding
5–60 g/l TURPEX® ACN NEW
Application:
• Padding with a liquor pick-up of 60–90 %
• Bath temperature: about 20 °C
• Drying at 110–130 °C
• Beakers
• Stirrer
• Pippets
• Funnel
• Padder
• Stenter
Application equipment:
28
• Laboratory stenter manufactured by TSUJI DYEING MACHINE
MANUFACTURING CO. LTD. OSAKA, JAPAN
Testing equipment:
Methods:
Application methods:
PAD-DRY-CURE
Firstly the recipe was made according to the required concentrations of chemicals.
The pick-up on the padder was set on 75%. The prepared solution was taken in the
trough of the padder and one complete length of fabric was passed through it.
Padding:
Padding was done on the padder installed at NTU lab manufactured by TSUJI
DYEING MACHINE MANUFACTURING CO. LTD. OSAKA, JAPAN. The liquor
pick up at the padder was set from 70-75%. The nip pressure was adjusted by the
pressure gear system. After dipping in the given recipe, the specimen was placed
between the nips of rollers. The extra amount of the liquor was squeezed out of the
fabric and required amount picked up.
Drying:
After padding the sample was taken to stentter for drying. The stentter installed at
NTU LAB is TSUJI DYEING MACHINE MANUFACTURING CO. LTD. OSAKA,
JAPAN. The drying temperature was set at 130ºC and the time given for drying was 2
minutes for each sample. During the drying process water present in the fabric
specimen was evaporated and specimen fully was dried at this stage. So that there
29
must not be any water or moisture during curing process which effect the cross
linking of the resin.
Curing:
After padding the samples were cured at the stenter. Different samples were cured
at different temperatures i.e. 150ºC, 170ºC and 190ºC. The samples were cured for 90
seconds each. During the curing process the Finish with the help of cross linker, cross
linked with the substrate.
Neutralization:
After curing the samples were neutralized with in 24 hrs to remove the phosphoric
acid used as a catalyst. A neutralization solution of liquor ratio with 35 g/l Na2CO3
was made and the fabric sample was immersed in that solution at 60ºC. After that
another solution was made with 12 g/l soda ash and the same sample was immersed
in it for 2 minutes.
Then the fabric sample was washed with simple water and at last the sample was
rinsed with a solution of 1-2 g/l H2O2 to remove the odor.
Washing/laundering:
The fabric samples were washed 5 times before doing the durability testing. The
washing recipe was made with 2 g/l detergent and 5 g/l soda ash. The fabric was
given 30 minutes at 60ºC.
Testing methods:
Project Plan:
This idea was taken from some of the seniors in NISHAT Textiles mills. The
discussion started with the application of FLAME RETARDANTS on polyester
30
Cotton fabrics, because it is quite difficult to achieve the FLAME RETARDANT
result on a PC blended fabric. But at the same time it has demand in the market i.e.
apart from protective clothing in apparel and children wear.
After discussions with my supervisor and HOD I came to the conclusion that i
will try to improve the durability of FLAME RETARDANT on PC blended fabric by
using a suitable i) Cross linker and ii) Binder.
All the other chemical concentrations i.e. Softener, Phosphoric Acid were kept
constant. The drying temperature was also kept constant i.e. 130ºC.
Total number of recipes was 9. Three samples were padded with one recipe and
then dried at 130ºC for 2 minutes on the stenter. After drying first sample was cured at
150ºC, second one at 170ºC and the third one at 190ºC. All three samples were given 90
seconds curing time.
After curing the samples were neutralized with in 24 hrs. After neutralization
wash the fabric samples were washed for durability and finally following tests were
performed on the samples:
• Flame Retardancy
• Tear Strength
• Tensile Strength
31
Design of experiments:
Below is the design of the experiment (DOE):
Note:
Wetting Agent = 10g/l
32
Softener = 15 g/l
Phosphoric Acid 25 g/l
33
Figure 2.1 Recipes keeping Flame Retardant Concentration 400 g/l
34
Chapter 3
Results and discussions:
Results
Results for Flame Retardancy:
Unwashed:
Table 3.1 Results for Flame Retardancy
Note:
Wetting Agent = 10g/l
Softener = 15 g/l
Phosphoric Acid 25 g/l
35
Main Effects Plot for Char Length unwash (cm)
Data Means
15.0
14.5
14.0
13.0
12.5
12.0
11.5
350 400 450
Flame Retardant g/ l
Discussion:
The unwashed samples that were tested after neutralization showed Flame
Retardancy. The Figure 3.1 shows that by increasing the concentration of Flame
Retardant the char length is decreasing i.e. less burning. Although the unwashed
samples showed the Flame Retardancy in acceptable limits but in most of the samples
an After Flame was there.
13.5
Char Length (cm)
13.0
12.5
12.0
11.5
60 70 80
Crosslinker g/ l
36
graph we can say that cross linker helps in fixation but at the same time reduces the
Flame Retardancy.
13.1
13.0
Char Length (cm)
12.9
12.8
12.7
12.6
12.5
150 170 190
Temperature ºC
Note: The samples which were burnt for testing became more like a
membrane after burning.
Washed:
All the samples were given 5 washes and then tested for flame retardancy.
Discussion:
Unfortunately not even a single sample turned out to be durable to washing. Some
of the samples were completely burnt, but samples with the higher concentrations of
Flame Retardant burnt slowly due to the After Flame.
The appearance of the sample after being burnt was like a mesh with polyester
content being burnt and cotton content left.
37
Although no significant results were obtained from the tests after washing but still
the conclusions obtained from these tests can help in future studies on Polyester
Cotton Flame Retardant fabrics.
Flame Retardant g/l Cross linker g/l Temperature ºC Tear Strength (g)
Warp Weft
450 80 170 1480 1320
350 70 190 1520 1180
450 70 190 1480 1200
450 60 190 1640 1040
400 70 150 1820 1360
350 80 190 1440 1100
450 60 170 1520 1380
350 70 150 1780 1340
400 60 150 2000 1440
400 70 190 1720 1300
350 80 150 1640 1280
400 80 190 1480 1160
400 60 170 1840 1520
350 80 170 1480 1140
400 80 170 1560 1380
450 60 150 1550 1100
450 80 190 1200 900
350 70 170 1580 1220
450 70 150 1440 1240
350 60 150 2460 1800
350 60 170 2020 1620
400 70 170 1520 1360
450 70 170 1440 1260
350 60 190 1400 1280
400 60 190 1380 1160
400 80 150 1840 1440
450 80 150 1920 1520
Note:
Wetting Agent = 10g/l
Softener = 15 g/l
Phosphoric Acid 25 g/l
38
Main Effects Plot for Tear Strength(Warp)
Data Means
1700
1650
Tear Strength (g)
1600
1550
1500
350 400 450
Flame Retardant g/ l
Discussion:
The Figure 3.4 shows the relation between the concentrations of Flame
Retardant and Warp Tear Strength of the Fabric. It can be seen in the above graph
that on increasing the concentration of Flame Retardant there is a loss in the Warp
Tear Strength of the Fabric. At higher concentrations of the finish the strength loss is
high.
1320
1300
Tear Strength (g)
1280
1260
1240
1220
1200
39
The Figure 3.5 shows the relation between the concentrations of Flame Retardant
and Weft Tear Strength of the fabric. All the values of Weft tear strength are less than
the Warp Tear strength. On increasing the concentration of Flame Retardant the Weft
Tear Strength decreases and on higher concentrations the strength is the most.
1750
1700
Tear Strength (g)
1650
1600
1550
60 70 80
Crosslinker g/ l
1350
Tear Strength (g)
1325
1300
1275
1250
60 70 80
Crosslinker g/ l
Discussion:
The Figures 3.6 & 3.7 shows the relation between the concentrations of cross
linker and Warp and Weft tear strength respectively.
40
It can be seen in the graphs that Warp Strength values are much higher than the
Weft strength values. But in both the graphs on increasing the concentration of cross
linker the tear strength of both warp and weft decreases.
1800
1750
Tear Strength (g)
1700
1650
1600
1550
1500
1350
Tear Strength (g)
1300
1250
1200
1150
It can be seen in the graphs that on increasing the curing temperature from 150 to
170ºC, the strength loss is more on warp of the fabric compared to the strength loss
on weft of the fabric. But in both the cases on increasing the curing temperature
41
strength loss is lost. And on higher curing temperatures i.e. 190º C the strength loss is
the most.
Note:
Wetting Agent = 10g/l
Softener = 15 g/l
Phosphoric Acid 25 g/l
42
Main Effects Plot for Tensile Strength (Warp)
Data Means
34.5
34.0
33.0
32.5
32.0
31.5
31.0
21.4
21.3
Tensile Strength (kg)
21.2
21.1
21.0
20.9
20.8
20.7
350 400 450
Flame Retardant g/ l
43
Main Effects Plot for Tensile Strength (Warp)
Data Means
34.5
34.0
33.0
32.5
32.0
31.5
31.0
60 70 80
Crosslinker g/ l
21.3
Tensile Strength (kg)
21.2
21.1
21.0
20.9
20.8
60 70 80
Crosslinker g/ l
44
Main Effects Plot for Tensile Strength (Warp)
Data Means
34.5
34.0
Tensile Strength (kg)
33.5
33.0
32.5
32.0
31.5
31.0
150 170 190
Temperature ºC
21.20
Tensile Strength (kg)
21.15
21.10
21.05
21.00
20.95
20.90
45
Overall discussion:
From all the test results, values and graphs it has been observed that Flame
Retardant applied to the Polyester Cotton blended fabric (50/50) gives some resistance to
burning before washing. The cross linker, higher finish concentrations and higher curing
temperatures don’t help much in making the fabric durable to washing.
By increasing the Flame retardant concentrations the fabric Flame retardancy does
improve but at the cost of loss in tear strength. The cross linker used also reduces the tear
strength but at the same time both Flame Retardant and cross linker when fixed to the
fabric increases the Tensile strength of the fabric.
This is because cross linking of the finish with the fabric makes the polymer
chains brittle and hence they are easy to tear. But in case of tensile strength the surface
coating due to the cross linking of finish increases the tensile strength of the fabric.
The increasing curing temperatures do help in fixation but at the same time a lot
of strength loss occur and even the fabric becomes yellow. But after neutralization wash
this yellowness of the fabric reduces.
Overall adding a cross linker to the Flame Retardant finish doesn’t help much in
increasing its durability and at the same time gives strength loss
46
Chapter 4
Summary:
Key findings of the project:
Though the Flame retardant finish didn’t prove to be durable on Polyester Cotton
blended fabric after washing, but still there were some findings and conclusions made
from this project:
Addition of the cross linker to the Flame Retardant recipe i.e. Pyrovatex CP
can only help finish to crosslink with the cotton content of the fabric.
• The Finish applied to the Polyester Cotton blended fabric can give Non
durable finish on the fabric.
• The fabric when burnt gives a mesh like appearance, half of the content
being burnt and half of the content remaining.
• In some recipes where the concentration of Flame Retardant was high, the
fabric didn’t burn at once but due to the after flame.
• After the neutralization wash, the yellowness of the fabric was reduced.
• The best results were obtained at 450 g/l Flame Retardant, 70g/l Cross
Linker and 170 ºC curing temperature.
• Overall the addition of a cross linker and raising the curing temperatures
doesn’t really help in improving the durability of the fabric and also
reduces the strength of the fabric.
47
Implications of the findings:
As polyester cotton blended fabric is mostly used in apparel and kids wear, this
finish can be applied on polyester cotton blended fabrics which are to be used for such
purposes. But this can only give a non durable finish, can not withstand washing.
But still work should be carried on to make the polyester cotton blended fabrics to
make them durable to washing because there is a demand of such fabrics these days in
apparel and kids wear industry.
• Instead of adding other auxiliaries with the finish, the chemistry of the
finish should be looked into and work should be done to make a durable
finish for Polyester Cotton Blended fabric.
• A two bath process can be done too, with first padding the fabric with the
finish suitable for cotton, drying and curing it. After curing the fabric
should be padded again with the finish suitable for polyester and then
giving the required drying and curing. Though the process will prove to be
an expensive one but it gives some acceptable results.
48
References:
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16th February,2011)
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2010)
49
16. Web page of “Bolton’s Fire Materials Laboratory” (Accessed on 3rd July, 2010)
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19. Benisek L, ‘Antagonism and flame retardancy’, Textile Research Journal, 1981,
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50