Table of Contents

Abstract ......................................................................................................................................................... 5

Chapter # 1 ................................................................................................................................................ 6
Introduction ................................................................................................................................................... 6
Antimicrobial Finish ..................................................................................................................................... 7
History ...................................................................................................................................................... 7
What Are Microbes? ................................................................................................................................. 7
Effects of Microbes on Textiles And Human Beings ............................................................................... 7
Mechanism of Antimicrobial Finishes .......................................................................................................... 8
Textiles Normally Subjected To Antimicrobial Finishes.............................................................................. 9
Benefits of Antimicrobial Finishes ............................................................................................................. 10
Requirements for Effective Antimicrobial Finishes ................................................................................... 10
Chemistry of Antimicrobial Finishes for Textiles ...................................................................................... 11
Application of Antimicrobial Finishes on Textiles ..................................................................................... 11
Surface Application ................................................................................................................................ 12
Chemical Bonding .................................................................................................................................. 12
Internal Antimicrobial Release ............................................................................................................... 12
Microencapsulation ................................................................................................................................. 12
Durability of Antimicrobial Textiles........................................................................................................... 13
Evaluation of Antimicrobial Finishes ......................................................................................................... 13
Problems With Anti Microbial Finishes ..................................................................................................... 15
Considerations for Antimicrobial Textile Product Development ............................................................... 16
Different Antimicrobial Finishes/Agents .................................................................................................... 16
Chitosan (Antimicrobial Finish) ................................................................................................................. 20
History .................................................................................................................................................... 20
Chitin and Chitosan................................................................................................................................. 21
How Chitosan Formed? (Crustacean) ..................................................................................................... 23
Properties of Chitosan ............................................................................................................................. 24
Physical Properties of Chitosan .............................................................................................................. 24

1
 Chemical Properties of Chitosan ............................................................................................................ 24
Electric Properties of Chitosan ............................................................................................................... 26
Deodorant Properties of Chitosan ........................................................................................................... 26
Application of Chitosan in Textile Wet Processing .................................................................................... 26
Chitosan Use in Printing ......................................................................................................................... 26
Chitosan Use in Dyeing .......................................................................................................................... 27
Chitosan As Shrink-Proofing Agent ....................................................................................................... 27
Chitosan Use in Finishing ....................................................................................................................... 27
Chitosan Use in Medical Field ................................................................................................................ 28
Dissolving of Chitosan ................................................................................................................................ 28
Dissolving in 1, 2, 3, 4-Butanetetracarboxylic Acid (BTCA)................................................................. 28
Dissolving in Citric Acid ........................................................................................................................ 28
Dissolving in Acetic Acid ....................................................................................................................... 29
Citric Acid Results .............................................................................................................................. 29
Effect of Molecular Weight on Activity of Chitosan .................................................................................. 29
Flame Retardant Finish ............................................................................................................................... 30
Fabric Flammability ................................................................................................................................ 30
Flame Retardancy of Fabrics .................................................................................................................. 30
Categories of Flame Retardants .............................................................................................................. 31
Types of Flame Retardants ..................................................................................................................... 32
How do Flame Retardants Work? ............................................................................................................... 32
Mechanism of Flame Retardancy ............................................................................................................... 33
Mechanisms of Flame Retardants ............................................................................................................... 33
Endothermic Degradation ....................................................................................................................... 33
Dilution of Fuel ....................................................................................................................................... 34
Thermal Shielding................................................................................................................................... 34
Dilution of Gas Phase ............................................................................................................................. 34
Gas Phase Radical Quenching ................................................................................................................ 34
Application of Flame Retardants on Textiles ............................................................................................. 34
An Ideal Flame Retardant for Cotton Should Posses the Following Properties: ........................................ 35
Pyrovatex® CP New (Flame Retardant Finish) .......................................................................................... 36
History .................................................................................................................................................... 36
Properties ................................................................................................................................................ 36

2
 Swisstex Chemicals ................................................................................................................................ 36
Cotton Fiber ................................................................................................................................................ 37
Properties of Cotton Fibres ..................................................................................................................... 37
Length of Cotton Fiber........................................................................................................................ 37
Fineness of Cotton Fiber ..................................................................................................................... 37
Strength And Extension of Cotton Fiber............................................................................................. 37
Elastic Properties of Cotton ................................................................................................................ 37
Cross Section ...................................................................................................................................... 38
Appearance ......................................................................................................................................... 38
Crimp .................................................................................................................................................. 38
Why Cotton is Used for Antimicrobial & Flame Retardant Activity Instead of Polyester? ................... 38

Chapter # 2 .............................................................................................................................................. 39
Experimental Work ..................................................................................................................................... 39
Application of Leaching Antimicrobial Finishes ........................................................................................ 39
Mode of Application ................................................................................................................................... 40
Apparatus (Laboratory Preparation) ....................................................................................................... 40
Chemicals................................................................................................................................................ 41
Pretreatment ............................................................................................................................................ 41
pH of Bath ............................................................................................................................................... 41
Application Way ..................................................................................................................................... 41
Procedure ............................................................................................................................................ 42
Drying & Curing ................................................................................................................................. 42
Precautionary Measures .............................................................................................................................. 43
Advantages.................................................................................................................................................. 44
Application of Non-Leaching Antimicrobial Finishes ................................................................................ 44

Chapter # 3 .............................................................................................................................................. 45
Testing of Anti Microbial & Flame Retardancy ......................................................................................... 45
Verification Tests of Antimicrobial Finish ................................................................................................. 45
Verification Test for the Application of Finish ....................................................................................... 45
BPB (Bromo Phenol Blue)...................................................................................................................... 45
Test for Dark Substrates.......................................................................................................................... 46

3
 Field of Detection ............................................................................................................................... 46
Test for Light Substrate....................................................................................................................... 48
Field of Detection ............................................................................................................................... 48
Test Method ........................................................................................................................................ 48
The “BPB Color Test Scale”:...................................................................................................................... 49
Conclusion .................................................................................................................................................. 49
Quantitative Test ......................................................................................................................................... 50
Future of Antimicrobial Finishes ................................................................................................................ 50
Verification Tests of Flame Retardancy on Cotton Fabric Samples ........................................................... 50
NFPA 701 Test ....................................................................................................................................... 50
16 CFR 1610 Test ................................................................................................................................... 51
Purpose................................................................................................................................................ 51
Testing Procedure ............................................................................................................................... 52
Conclusion .......................................................................................................................................... 52

Chapter # 4 .............................................................................................................................................. 53
Samples & Conclusions .............................................................................................................................. 53
Conclusion of Testing Results of Antimicrobial Activity........................................................................... 58
Conclusion .................................................................................................................................................. 64
References ................................................................................................................................................... 65

4
 Abstract

Innovations resulting from technological advancements represent the best strategy for success in
the increasingly competitive textile industry. The fabric production rate is very tremendous and
the market has limited scope which can be multiplied by value added finishing to textiles like
anti microbial finish or flame retardant finish which counts more value in the current scenario of
market. Recently, special finishes have become available that can be readily added on the textiles
and after finishing and fixation; we can get benefit from them.

Here in this thesis, we have discussed the combined application of antimicrobial and flame
retardant finishes on the same cotton fabric. Chitosan is used as antimicrobial finish and
Pyrovatex® CP New as flame retardant finish. Both finishes were applied by Pad – Dry – Cure
method.

Antimicrobial activity and flame retardancy of treated fabric was investigated against different
concentration of Chitosan, Pyrovatex® CP New and Knittex CHN. It was concluded that

5
 Chapter # 1

Introduction

Days are gone when quality product was the only criterion to eye a product by a consumer.
Earlier were the times when sheer competitiveness in the domestic market was very confined.
But, during some past years with the emergence of globalization, competitive atmosphere and
quality consciousness, has reached a new mark. With the steady improvement in technology &
application standards, a gradual rise was observed in consumer demands and to reach up to that
mark, manufacturers have to add something to their products to get market value for their
products. A product must be able to encompass something more with it & therefore this has
taken today’s market to a platform where it seems very difficult for a manufacturer to market his
product until he satisfy the consumer with something new which not only rewards him for his
novel concept but also lures him with considerable increase in profit . The role of the textile
finisher has become increasingly demanding, and now requires a careful balance between the
compatibility of different finishing products and treatments and the application processes used to
provide textiles with desirable properties.

Growing trends and escalating standards leave no stone unturned to boast the current scenario of
textile industry. Performance with beauty describes the potential of textile finishing. Anti
Microbial or flame retardant finishing of textiles is one such immaculate magnanimous entry into
any textile culture.

A new revolution is in the textile industry by providing Anti Microbial with Flame Retardant on
the same fabric. Dual action finishing of textiles is the process where we enhance the value of the
product by adding some incentives to it. The world market place is continuously changing and so
is demand of people changing .Every person desires for some change .i.e. something new &
unique. The successful effective implementation of change has to be done to in the market. We
by the medium of this project have made an earnest attempt to present you a detailed
comprehensive analysis done by combined application of anti microbial and flame retardant
finishes on cotton fabric and which has busted this industry with exuberant value added finishes
which provides double protection for fabric i.e. protection against bacteria and other microbes
and also at the same time an effective protection against the fire [1].

The anti microbial component has an ability to penetrate and destroy the bacteria like
Salmonella, Listeria, Campylobacter, Staphylococcus Aureus, Streptococcus and also many
other environmental bacteria. This component also protects the fabric against Mould, Fungi and
Yeasts. The fire retardant component helps to keep away the fire from the fabric [2].

Now firstly we will discuss Anti Microbial and then later Flame Retardant Finish.

6
Antimicrobial Finish

History

The use of antimicrobials dates back to ancient Egypt, where these were used in the treatment of
mummies [3]. The first antimicrobial textile material, in modern history, was developed by Lister
in 1867 [4]. Over the last few years there has been increased interest in antimicrobial finishes.
The main reasons for this increased interest include: the promotion of healthier and physically
active lifestyle; an increased awareness of the harmful effects of organisms on textiles as well as
on human hygiene and freshness [5], and the greater use of synthetic fibers and blends in items
such as shirts, hosiery, blouses and underwear, which tend to cause greater perspiration wetness
because of poor moisture transport properties as compared to natural fibers [6].

Other factors that are responsible for the current level of interest include the increasing use of
carpeting and architectural fabrics [7]. Consumers are becoming more conscious of carpet odors
created by bacteria, mold and mildew. Protection of fabrics, used in buildings, from fungi that
cause staining, odor and damage is critical in the outdoor environment.

What Are Microbes?

A microbe or microorganism is an organism that is so small that it is microscopic (invisible to

the naked eye) [8]. Microorganisms i.e. bacteria, fungi, mildew, mold and yeasts, are found
everywhere in nature, even in hostile environments. The human skin is usually crowded with
innumerable microorganisms. A suitable temperature, moisture, dust and receptive surface
provide perfect conditions for their growth [9]. In favorable conditions certain bacteria can grow
from a single germ to millions in a very short period of time. They can double every 20 to 30
minutes in a warm and moist microclimate that has plenty of food for them, e.g. perspiration and
other body secretions, skin particles, fats and leftovers from worn-out threads [10].

Effects of Microbes on Textiles And Human Beings

Although microbes can be useful in many ways, for example in brewing, baking and
biotechnology, they can also be harmful to both textiles and humans. Different substances added
to textiles, such as size, hand modifiers, antistats, thickeners, lubricants and dirt as well as
grease, sweat and dead skin from the human body provide a great source of nourishment for
microorganisms. Following are some of the possible effects of micro-organisms on textiles:

 Bad odour

 Discoloration, unsightliness or staining of the fabric

 A slick slimy handle

 Loss of functional properties like elasticity and tensile strength

7
  Decrease in the life of the textiles, especially cotton and wool

Natural fibres are particularly prone to microbial attack as they are readily digestible by bacteria
and fungi but the synthetic fibres are not completely immune either as they might contain some
additives that may be a nutrient for microbes [11, 12]. Wool is more likely to be attacked by
bacteria than cotton while cotton is more likely to be attacked than wool by fungi. Many
different finishes applied on textiles are excellent source of nutrients for microbes, making
textiles susceptible to microbial attack. Work in progress in textile manufacturing is also
susceptible to microbial attack, particularly if the goods are left for a long time in conditions
conducive for microbial growth.

Apart from their effects on textiles, microbes can be a source of many problems to human
beings, ranging from simple unpleasant odour to physical irritation, allergy, toxic responses,
infection and diseases. An unpleasant odour results when, among other things, human
perspiration is converted by bacteria into foul-smelling substances such as aldehydes, amines,
ammonia, sulphides, mercaptans, aromatics, lactones and fatty acids (acetic, propionic, butyric,
valerianic, caproic). The minute particles of house dust mite excrements adhering to dust
particles can cause dust allergies while mould fungi of the aspergillus type can produce lung
disease [13].

Mechanism of Antimicrobial Finishes

Normal home-washing of textiles, which is generally under mild conditions, does not completely
remove the microbes. In order to eliminate microbes, very severe laundering conditions, e.g., a
temperature of 95 °C and strong detergents followed by bleach, are essential. Any surviving
microbes can quickly multiply again at each further wearing. This can be avoided by the
application of antimicrobial finishes.

Antimicrobial is an agent that works against microbes. It can either inhibit their growth and
reduce the undesired by-products or kill them altogether. Agents which inhibit the growth of
microorganisms and do not kill them are known as biostats, i.e. bacteriostats, fungistats. Agents
which actually kill the microorganisms are known as biocides, i.e. bacteriocides, fungicides.
While biostats are subject to fewer regulations, biocides are more strictly controlled by
governmental regulations.

All antimicrobials do not work in the same manner. They primarily function in two different
ways. The conventional leaching types of antimicrobials work by leaching or moving from the
surface on which they are applied. They leave the textile and chemically enter or react with the
microorganism acting as a poison. Like an arrow shot from a bow or a bullet shot from a gun,
they are used up in the process of working, wasted in random misses, or complexed with other
chemicals in the environment for use or abuse. Leaching types of antimicrobials can be effective
against microbes on the fiber surface or in the surrounding environment. However, they may
have the following disadvantages:

8
  Poor durability, as the antimicrobial reservoir will be eventually depleted

 Can contact the skin and potentially affect the normal skin bacteria

 Can cross the skin barrier and have the potential to cause rashes and other skin irritations

 Allow for the adaptation of microorganisms

The second type of antimicrobials consists of molecules that are chemically bound to fiber
surfaces. The bound antimicrobials remain affixed to the substrate, killing microbes as they
contact the surface to which antimicrobials have been applied. They control only those microbes
that are present on the fiber surface and are not effective in the surrounding environment. They
can potentially be abraded away from the fiber surface or may become deactivated and lose long
term durability.

The actual mechanism of control of microorganisms by antimicrobials is extremely varied,

ranging from poisoning the cell from within, preventing cell reproduction, blocking of enzymes,
and reaction with cell membrane to the destruction of cell walls.

Textiles Normally Subjected To Antimicrobial Finishes

 Apparel/Sportswear/leisurewear/work wear: to get rid of the bad odor produced by the

bacterial decomposition of sweat and other body fluids.

 Undergarments (including underwear worn by astronauts): to control the growth of

bacteria which thrive on suitable body temperature and moisture conditions, leading to
skin diseases [14].

 Socks: to make them free from unpleasant odor by controlling the growth of microbes.

 Shoes: to avoid shoe odor and the stains on the shoelaces caused by bacterial growth,
especially in rainy season.

 Home Furnishings and Upholstery: to inhibit the growth of bacteria leading to

degradation and/or staining in carpets [15], shower curtains, mattress ticking, pillow
covers, pillow fills and upholstery.

 Industrial Fabrics Exposed to Weather: to protect fabrics used for awnings, tents,
tarpaulins and the like from rotting and mildew.

 Sized Fabrics: to protect microbial growth due to the presence of warp size.

 Wet Textiles: to prevent degradation of fabrics by microbial attack during prolong

storage between processing steps.

9
  Medical Textiles: to impart antimicrobial properties on wound dressings [16] and get
freedom from microbes/pathogens from textiles used in hospitals, nursing homes,
medical and research facilities, and veterinary clinics for protection against infectious
diseases.

 Textiles in Museums: to preserve textile monuments from microbial attack.

Benefits of Antimicrobial Finishes

Antimicrobial finishes add value to the product for both the producer and the consumer in the
following ways:

 Protection of the raw material from decay or degradation

 Control of staining caused by microbial growth

 Added freshness to the fabrics

 Elimination of smells created by microorganisms

 Increased life period of the fabric because of control of the growth of microbes

 Improvement in the handle for most of the fabrics

 No irritation of the skin and no physiologic impact to human health

Requirements for Effective Antimicrobial Finishes

Following are the major requirements for an effective antimicrobial finishing agent:

 Quick acting and effective in killing or inhibiting the growth of a broad spectrum of
microorganisms

 Non-selective and non-mutable to pathogens

 Fast to repeated laundering, dry-cleaning and exposure to light

 Safe and easy to apply

 Safe and comfortable to wear (no irritation of the skin/dermatologically tested)

10
  Minimal environmental impact

 Compatible with other finishing agents

 Low cost

There is no such thing as universal antimicrobial. The choice of a suitable antimicrobial depends
on whether it is meant to combat odour or staining, or inhibit the growth of fungi, mildew or
bacteria. Furthermore, the different ‘anatomy’ of the microorganism also plays a role in the
selection of a suitable antimicrobial.

Chemistry of Antimicrobial Finishes for Textiles

Antimicrobial chemicals are mainly of two types: those which work by controlled release
mechanism and those which remain bound to the textile substrate [17]. Examples of
antimicrobials for controlled release are: Copper naphthenate, copper-8-quinolinate and various
organo mercury compounds; tributyl tin oxide, dichlorophene and 3-iodopropynylbutyl
carbamate; Benzimidazol derivatives, salicylanilides and alkylolamide salts of undecylenic acid;
Formaldehyde; Triclosan (2,4,4’-trichloro-2’-hydroxydiphenyl ether); Quaternary ammonium
salts; Organo-silver compounds and silver zeolites. Examples of bound antimicrobials are:
Octadecylaminodimethyltri-methoxysilylpropylammonium chloride; Polyhexamethylene
biguanide (PHMB) and Methylol-5,5-dimethyldyantoin + hypochlorite.

Chitosan, manufactured from inexpensive natural waste product (crustacean shells such as crab
etc.), has been used with great success in Japanese domestic market for surgical dressings
because of its skin-healing properties and also has undergone successful trials in EU and UK
markets. It can be applied by microencapsulation or by reactive bonding to cellulose and by
crosslinking. When applied to cellulose by crosslinking, it gives antimicrobial as well as
moisture control properties. It offers many advantages including high absorbency properties,
moisture control, promotion of wound healing, non-allergenic, non-toxic and biodegradable
properties [18, 19].

Application of Antimicrobial Finishes on Textiles

Technologies that are utilized to help keep the active antimicrobial ingredients on textile
materials wash after wash can be classified into four categories: surface application, chemical
bonding, internal antimicrobial release, and micro-encapsulation [20].

11
Surface Application

This method has the following characteristics:

 It is applicable to all fibers.

 Washing durability depends normally on the affinity of antimicrobials.

 In the case that polymeric coating products are used together, washing durability depends
on the strength with which the polymers can bind with the textile surface.

 For certain fibres, such as PAN, ionic charge could be another factor to be considered.

Chemical Bonding

This method has the following characteristics:

 It is applicable only to those fibres that have a suitable reactive group, e.g. cellulose,
wool and polyamide.

 Washing durability depends normally on the strength of the chemical bond between the
antimicrobial agent and the fibre.

 It is theoretically the best way to achieve durable antimicrobial finish.

Internal Antimicrobial Release

This method has the following characteristics:

 Antimicrobials are incorporated into the fibres when they are spun.

 It is a viable option only for synthetic fibres.

 It does not work well on cotton.

Microencapsulation

This method has the following characteristics:

 It is a hybrid of “chemical bonding and controlled internal release”.

12
  In this method, instead of antimicrobials making the chemical bond with fibres, micro-
capsules that contain the antimicrobials are covalently fixed on the fibres.

 Effective antimicrobial effect depends on the particular capsule system to regulate the
release of antimicrobials in a sustained way [21].

Durability of Antimicrobial Textiles

Temporary antimicrobial properties in textiles are easy to achieve in finishing but readily lost in
laundering. Temporary antimicrobial textiles are useful only for disposable materials. Durable
antimicrobial function is quite challenging to achieve and can last more than 50 machine
washes.

Evaluation of Antimicrobial Finishes

The objective of evaluation is to determine the effectiveness of an antimicrobial treatment

against a variety of microorganisms in the shortest amount of time. Methods for evaluating
antimicrobial finishes can be divided into two types: quantitative and qualitative. In quantitative
methods, the number of bacteria, still living after an opportune contact time, is counted.
Quantitative evaluation can be further divided into two types according to the main test
conditions. For example in the static method AATCC 100, a small amount of liquid culture
medium is used to cover a specimen, while in the dynamic Shake Flask Test Method, the fibre
specimen is immersed in a larger amount of liquid culture.

In qualitative methods, the test specimen and an untreated control sample are pressed into
intimate contact with agar culture medium inoculated with the test bacterial solution. In case the
antibacterial activity is present, a clear zone of inhibition around the treated sample may be
observed and compared to the zone of bacterial growth around and over the untreated control
sample after the same contact time. The qualitative methods provide a formula to measure the
width of the inhibition zone. However it cannot be considered as a quantitative indication of the
antibacterial activity.

In both the quantitative and qualitative tests, it is essential to measure the bioactivity of a
reference control sample without antimicrobial properties but of nature similar to the one with
antibacterial properties. There may be three outcomes as a result of testing a textile for
antimicrobial properties:

(i) a significant increase in the initial population of bacteria

(ii) an inhibition of the growth of bacteria in a sample with antimicrobial treatment as

compared to the one without antimicrobial treatment

(iii) a reduction in the number of test bacteria

13
The first case indicates no antibacterial activity. The second case indicates biostatic activity
while the third case indicates biocidal activity. If only bacteriostatic activity (inhibition of
multiplication) is intended, a qualitative procedure which clearly shows antibacterial activity as
contrasted with lack of such activity by an untreated specimen may be acceptable. However, if
bactericidal activity is intended or implied, quantitative evaluation is necessary. Some of the
standard testing methods for the evaluation of antimicrobial textiles are given as follows:

 AATCC Test Method 147: Antibacterial activity of textile materials: parallel streak
method. This method is used for the detection of bacteriostatic activity on textile
materials. The method is useful for rough estimate of activity [22].

 AATCC Test Method 100: Antibacterial finishes on textile materials: Assessment of.
This is a quantitative method for the determination of degree of antibacterial activity [23].

 AATCC Test Method 30: Antifungal activity, assessment on textile materials: Mildew
and rot resistance of textile materials [24]. This test method is used to determine the
susceptibility of textile materials to mildew and rot and to evaluate the efficacy of
fungicides on textile materials.

 AATCC Test Method 174: Antimicrobial activity, assessment of carpets [25]. This
method provides procedures for qualitative antibacterial and antifungal assessment and
quantitative antibacterial assessment of carpet materials.

 BS EN ISO 20645: Determination of antibacterial activity. Agar diffusion plate test. This
method gives procedure for the determination of the effect of antibacterial treatments
applied to woven, knitted and other flat textiles. The method is applicable to testing
hygienic finishes of hydrophilic, air-permeable materials or antibacterial products
incorporated in the fibre. The method is not suitable for testing textiles treated with
antibacterial treatments that react with the agar.

 BS EN ISO 11721-1: Determination of resistance of cellulose-containing textiles to

micro-organisms - Soil burial test - Assessment of rot-retardant finishing. This method
gives procedure for the determination of the resistance of chemically-pretreated textiles
to the action of microorganisms present in soil in comparison with untreated textiles. The
method is applicable to flat textiles made of cellulose-containing yarns that will typically
come into contact with soil during use, e.g. tents, tarpaulins, webbings and tapes. This
method is intended to give comparative performance rather than provide absolute values.

 BA EN ISO 11721-2: Determination of the resistance of cellulose-containing textiles to

micro-organisms - Soil burial test - Identification of long-term resistance of a rot
retardant finish. This method gives procedure for identification of the long-term
resistance of a rot retardant finish against the attack of microorganisms in the soil. The
method allows making distinction between rot-retardant finishes with no long-term

 SN 195 920: Textile Fabrics - Determination of the antibacterial activity : Agar diffusion
resistance, with regular long-term resistance and with increases long-term resistance.

plate test.

14
  SN 195 921: Examination of the antimycotic effect of impregnated textiles by the agar
diffusion test.

 SN 195 924: Textile Fabrics - Determination of the antibacterial activity : Germ Count
Method.

 ASTM D2020-92: Mildew (fungal) resistance of paper and paperboard.

 ASTM D4300-98a: Ability of adhesive films to support or resist the growth of fungi.

 ASTM E1428-99: Evaluating the performance of antimicrobials in or on polymeric solid

against staining by Streptoverticillium reticulum (a pink stain organism).

 ASTM G21-96: Determining resistance of synthetic polymeric materials for fungi.

National Standard of Canada - Textile Test Method (Can 2-4.2-M91)

Method 28.1: Fungus damage test - pure culture

Method 28.2: Surface growing fungus test - pure culture

Method 28.4: Fungus damage test - pure culture - qualitative

Federal Test Method STD 1 91A-1978

Method 5750: Mildew resistance of textile materials: mixed culture method

Method 5760: Single culture method

Method 5830: Leaching resistance of cloth standard method

Problems With Anti Microbial Finishes

Some common problems related with the application of antimicrobial finishes are given as
follows:

 Stiff Hand And Fabric Strength Loss: This may be caused by the use of binders and
resins with controlled-release finishes.

 Color Change: This may be due to inappropriate choice of antimicrobial finishes.

 Selectivity: Some antimicrobial finishes are efficient against Gram-positive bacteria or
Gram-negative bacterial, while others against fungi. A formulation that is a mixture of
several substances will be more effective for good all-round protection against microbes.

15
  Toxicological And Environmental Problem: include skin irritation, sensitizing, allergy
or dermatitis on prolonged contact with skin, biodegradability and bioaccumulation.

 Handling: the higher the biocide activity, the higher the need for safe handling and
prevention from toxicity.

 Development of Resistant Microbes: an area of concern regarding the use of

antibacterial finishes is that their long term use may lead to the development of resistant
microbes which might have deadly consequences for humans.

Considerations for Antimicrobial Textile Product Development

Antimicrobial finishing should not be considered as a simple add-on finishing process. Some of
the important points that must be considered for the development of a textile product with
antimicrobial properties are given as follows [5, 26]:

 Identification and definition of the customer and the customer’s needs

 Selection of the most appropriate fabric

 Selection of the most appropriate antimicrobial on the basis of safety

 considerations, regulatory compliance, application technology and efficacy

 Selection of the most appropriate application technology

 Setting up of a manageable testing and quality control program

Different Antimicrobial Finishes/Agents

Several durable antimicrobial finishes/agents show some promise for selected end-uses. Below is
a brief description of some of these products.

 Polyhexamethylene biquanide hydrochloride (PHMB) has a broad spectrum of activity

against bacteria and fungi with a long history of safe use. Application may be by pad,
spray, foam, or exhaust methods. Upon drying, it becomes quite durable; however,
researchers have reported good and bad results.

 Metallic silver combined with zeolite and dispersed in the polymer before extrusion
spinning provides a polyester fiber that can be intimately blended with cotton to produce
a durable antimicrobial composite. The blend is reported to have excellent anti-bacterial
and anti-fungal properties. It has been reported in patents where these antimicrobial
agents have been fixed on cotton fabrics with a binder such as an acrylic or polyurethane
[27].

16
  Quaternary silicones like 3-trimethoxy-silylpropyldimethyloctadecyl ammonium chloride
have been used for a number of years as a durable odor preventive on socks. However, it
is reported to be less than 90% effective on bacteria and to have limited activity against
fungi.

A renewable antimicrobial agent is based on the reaction of monomethylol-5,5-

dimethylhydantoin (MDMH) with cotton and subsequent reaction with hypochlorite
bleach. The activity is derived from the slow release of chlorine that can be renewed
when subjected to hypochlorite bleach again. This application requires that the fabric be
white or dyed with pigments or vat dyes due to the reduction of most dyes by chlorine.

 Trichloro-orthophenylphenol (Triclosan) can be added to the spinning solution of acrylic

or acetate fibers for blending with cotton. Triclosan may also be exhausted or
thermofixed to cotton blends containing polyester to impart antimicrobial properties.
Some reports indicate good results and others show inferior performance.

 Chitosan made insoluble by cross linking is effective in neutralizing some odors.

Although it is environmentally friendly, the level of the finish required to be effective
imparts excessive stiffness to the fabric.

 Magnesium hydroperoxy acetate, another environmentally friendly compound, can be

fixed to cotton to impart some antimicrobial properties. Few industrial evaluations have
been reported [28].

Leaching Antimicrobial Finishes

Fields of Application

They can be applied to colored and white textiles. Their application is possible on all common
types of fibers. But the treatment of pure polyester requires pre-treatments in order to assess the
best application conditions. The names of some of the materials to which they can be applied are
given below:

Sportswear

Working Clothes

Lining Fabrics

Terry Fabrics

17
 Socks

Tights

Pullovers

Woolen Blankets

Acrylic Blankets

Non-Leaching Antimicrobial Finishes

Fields of Application

They can be applied to impart durable, broad-spectrum antimicrobial protection to substrates for
the following applications:

Air Filters/Materials

Aquarium filter material

Bed sheets

Blankets

Bed spreads

Buffer pads

Draperies

Carpets

Upholstery

Sleeping bags

Towels

Fire hose fabric

18
Humidifier belts

Mattresses

Men’s underwear & outerwear

Non-woven disposable diapers

Non-woven polyester

Polyurethane foam for packaging and cushioning

Roofing materials

Sand bags

Tents

Tarpaulins

Ropes

Athletic & casual shoes

Shoe insoles

Shower curtains

Socks

Seat covers

Umbrellas

Vacuum cleaner bags

Wiping clothes

Women’s hosiery

19
Chitosan (Antimicrobial Finish)

History

Chitin was described for the first time in 1811 by Braconnot, who was professor of Science of
Nancy, France. Chitosan was discovered by Rouget in 1859. He was found that chitin, which has
been boiled in a very concentrated potassium hydroxide solution, becomes soluble in diluted
solutions of iodine and acid, where as chitin was stained brown.

The production of chitin and chitosan is currently based on crab and shrimp shells discarded by
the canning industries in Oregon, Washington, Virginia, and Japan and by various finishing
fleets in the Antarctic.

Several countries possess large unexploited crustacean resources e.g. Norway, Mexico, and
Chile. The production of Chitosan from crustacean shells obtained, as a food industry waste is
economically feasible, especially if it includes the recovery of carotenoids. The shells contain
considerable quantities of astaxanthin, a carotenoid that has so far not been synthesized, and
which is marketed as fish additive in aquaculture, especially for Salmon.

Chitosan is form ed by the deacet yl ati on of chitin (pol y- N-acet yl glucose

amine), an abundant byproduct of the crab and shrimp processing industri es. . It
has a number of commercial and possible biomedical uses.

20
Chitin and Chitosan
The distinction bet ween chiti n and Chitosan is so mewhat blurred; some
definitions st ate t hat chitin that is m ore than 50 per cent de -acet yl at ed is
chitosan, whereas others define chitosan as sol uble i n 1 percent aceti c acid,
chitin being insoluble. Most commerci al l y avail abl e chitosan preparations are
more than 85 per cent de -acet yl ated.

Chitin and chitosan have the potential to reduce and to solve some problems for creating
“Greener environment”.

21
The following is a chronological order of the processes needed to produce Chitosan from
crustacean shells [29].

22
How Chitosan Formed? (Crustacean)

Shell—Size reduction—Protein Separation (NaOH)—Washing—Demineralization (HCl) –

Washing and Dewatering – Chitin -- Deacetylation (NaOH) – Washing and Dewatering –
Chitosan.

Chitin and Chitosan are natural resources refined from the waste products of the crabbing and
shrimp industry. Chitin is produced from the processing waste of shellfish, frill, clams, oysters,
squid, and fungi. They have a high percentage of Nitrogen (6.89%) compared to the synthetically
substituted cellulose, which has 1.25% nitrogen. Chitosan has amino groups and hence it exhibits
many properties, such as biodegradability, which are different from the cellulose. Chitin does not
melt; it is insoluble in water, dilute acids, cold alkalies, and organic solvents. However, the
solvents like formic acid, concentrated mineral acids, and tetrechloroacetic acid can dissolve
Chitin, but they are not convenient and lead to polymer degradation. On the other hand, Chitosan
is readily soluble in most aqueous solutions, like that of 5% formic acid and acetic acid because
of the basicity of the primary amine groups. Chitosan dissolves readily when electric repulsions
(corresponding to cationic charges)
The solubility of chitosan is also favoured by the process of hydration of various, mainly charged
sites. As a result, the ratio between NH3+ and NH2 groups, a parameter directly related to the
charge density of the polymer, is a very important factor in ascertaining the properties of
chitosan. The basic difference between Chitin and Chitosan is the degree of deacetylation
(DAC), which is the same as the relative amount of free amount amine. Chitosan is obtained
from chitin by treating the latter with strong caustic soda and heat, which removes the N-acetyl
groups.

As a natural renewable resource with a number of unique properties, chitosan is now attracting
more and more scientific and industrial interest from diversified fields such as chemistry,
biochemistry, medicine, pharmacology, biotechnology, and food and textile sciences. Properties
such as biodegradability, biocompatibility, non-toxicity, wound healing and antimicrobial
activity have generated much research work. Many unique products have been developed for
various applications such as surgical sutures, artificial skin, cosmetics and dietary foods.

23
Properties of Chitosan

Almost all properties of chitin and chitosan depend on two fundamental parameters; the degree
of acetylation and the molecular mass distribution (or average molecular weight), although they
do have some contrasting properties. The molecular weight of chitin and chitosan can be
determined by methods such as chromatography, light scattering and viscometry. Viscometry is
by far the most simple and rapid method for the determination of average molecular weight by
measuring an intrinsic viscosity for several concentrations of chitosan or chitin solutions.

Physical Properties of Chitosan

Solution properties of Chitosan in free Amine (-NH2) form soluble in acidic solutions.

 Insoluble at pH’s > 6.5

 Insoluble in H2SO4

 Limited solubility in H3PO4

 Insoluble in most organic solvents

 Soluble at pH’s < 6.5

 Forms viscous solutions

 Solutions shear thinning, forms gels with polyanions

 Will remain soluble in some alcohol-water mixtures [28]

Chemical Properties of Chitosan

Chitosan is a linear polyamine (poly-O-glucosamine) with reactive hydroxyl and amine group.

 Biocompatibility
Chitin and chitosan are natural biopolymers. They have no antigenic properties, and thus

24
 are perfectly compatible with living tissue. Their antithrombogenic and hemostatic
properties make them very suitable for use in all fields of biology.

 Cicatrizant
Chitosan forms films that are permeable to air. It facilitates cellular regeneration while
protecting tissue from microbe attack. In addition, chitosan has been found to have a
biostimulant effect on the regeneration of tissue.
Lysozome that kills various germs increases 1.5 to 2 times as fiber made from chitosan
comes in contact with the skin it also activates nitrogen, which regenerates the skin. This
property has allowed it to be used in making an
artificial skin for skin grafts on high degree burns and in surgical applications such as
chitin suture thread. It binds to mammalian gum tissue. It accelerates the formation of
osteoblasts responsible for the formation of bone.

 Anticholesterolemic Agent
Chitosan can trap lipids at their insolubilization pH in the digestive tract. Administered to
rats, chitosan considerably reduces the level of cholesterol in the blood.

 Chelation Agent
Chitin and its derivatives are remarkable chelation agents. Chitosan is used for a wide
rangeof applications: as a chromatography medium, or for trapping heavy metals, or for
water treatment. It chelates many transitional metal ions.

 Biodegradable
Chitin and chitosan are biodegradable biopolymers. Enzymes-chitinase and chitosanase-
break them down into oligopolymers that are then dealt with by the metabolism. It is
biodegradable to normal body constituents.

 Strengthening Immunity
Fibers made from chitosan strengthen the immunity of the human body to expel foreign
matters when disease germs or viruses enter the body.

25
  Antimicrobial Activity
It is also a fungi static and has spermicidal and antitumor properties. Generally chitosan
(D.A.=9.9%, concentration 0.15%) is proved to be free from mildew activity during four
cultivating days. The activity increases with increase in concentration of chitosan.

Electric Properties of Chitosan

Fibers made from chitosan can effectively generate static electricity due to its high molecular
weight. It has a unique resistance value similar to other natural high molecular matters such as
cellulose or rayon.

Deodorant Properties of Chitosan

Chitosan eliminates stink of sweat and other odors. It has humid retention properties due to the
amine radical & is also a central nervous system [30].

Application of Chitosan in Textile Wet Processing

Chitin and chitosan have higher affinity for dyes and metals and certain surfactants, which
contribute to water pollution. Using the shellfish waste thus has two-fold
advantage:

a) First to find a viable method to purify dye wastewaters.

b) To use natural resources, this could otherwise have been wasted.

After use for color removal the spent sorbent further finds use as a fibrous raw material for
papermaking.

Chitosan Use in Printing

The use of chitosan as a combined thickener and binder in pigment printing has been studied in
comparison with the commercial printing system. Printing pastes made from chitosan, acetic acid
and pigments at appropriate viscosity give stable pastes and satisfactory results on polyester and
polyester –cotton blends.

26
Chitosan Use in Dyeing

Chitosan can also be used in the dyebath, because due to the unimolecular structure it has an
extremely high affinity for many classes of dyes, including disperse, direct, reactive, acid, vat,
sulphur etc. Rate of diffusion of dyes in cellulose is similar to that in cellulose. Sorption of
chitosan is exothermic: hence an increase in temperature leads to an increase in dye sorption. At
lower pH chitosan free amines are protonated causing to attract anionic dyes.

Chitosan As Shrink-Proofing Agent

Chitosan is used as a shrink-proofing agent and also is used to increase the dye uptake of wool.
In its protonated form, it exhibits the behavior of a cationic polyelectrolyte, forming viscous
solutions and interacting with the oppositely charged molecules. Thus it is suitable for processing
of wool near its isoelectric point, offering minimum fiber damage and providing good quality.
However the main limitation is the uneven distribution on the fabric surface.A new ecological
method for shrink proofing of the wollen fabric is based on the enzymatic pretreatment and
chitosan deposition on the wollen fabric.

This method shows the enzymatic pretreatment has an essential influence on the shrink proofing
qualities and chitosan stabilizes the shrink proofing property. It also increases the kinetics of
dyeing and causes a decrease in hydrophobicity.

Chitosan Use in Finishing

Antimicrobial finishing is very important because cotton fabrics have poor resistance to
microorganisms and thus the possibility of harming the human body, chitosan is also known to
be an antimicrobial polysaccharide. The ability of chitosan to immobilize microorganisms
derives from its polycationic character. Its protonised amino groups block the protein sequences
of microorganisms, thus inhibiting further proliferation. Chitosan binds to the negatively charged
bacterial surface disrupting the cell membrane and altering its permeability. This allows
materials to leak out of the bacterial cells resulting in cell death. Chitosan can also bind to DNA
inside the cell inhibiting mRNA and hence protein synthesis.

27
Recent studies have revealed that chitosan is more effective in inhibiting the growth of bacteria
than chitosan oligomers. Also the antibacterial effect of chitosan oligomers are reported to be
dependent on its molecular weight.

Chitosan Use in Medical Field

Chitosan is expected to be one of the safest and most effective Antimicrobial agents for hospital
applications where many antibiotic substances are used. Chitosan is especially important .which
is resistant to most antibiotic substances. Hygienic yarns can also be made through the addition
of chitosan fibres. Chitosan fibers are blended with cotton fibers and a yarn is spun out of this
blend; 10% chitosan component is sufficient to achieve a hygienic effect. This effect should
endure 20 washes.(1)currently, there is also a hightened interest in protecting health care workers
from diseases that might be carried by patients. Especially for surgical gowns, there is an
increasing need to protect medical staff from infection by bloodborne and so surgical gown
materials should have not only antimicrobial properties but also blood barrier properties.
Chitosan and fluoropolymers seem to be the most suitable finishing agents for providing surgical
gown materials with barriers against microorganisms and blood. Because many medical products
including surgical gowns are used in close proximity to human skin, the hand and air
permeability of these materials are also very important. Recently, single-use gowns made from
non-woven have gained in popularity because non-woven fabrics block fluids so well and single-
use gowns are so reliable.

Dissolving of Chitosan

Dissolving in 1, 2, 3, 4-Butanetetracarboxylic Acid (BTCA)

Polycarboxylic acids that crosslink with cotton through an esterification reaction. BTCA
is the most effective of these plycarboxylic acids, but its cost is very high; citric acid is a
less effective crosslinking agent but is not as costly.

Dissolving in Citric Acid

However, cotton fabrics treated with citric acid alone exhibit appreciable yellowing,
although there have been some investigations undertaken to reduce this yellowing.

28
Dissolving in Acetic Acid

Generally, cellulose is treated with chitoan by dissolving the chitosan in dilute acetic acid
solution, but this method does not create any firm chemical bonds between chitosan and
cellulose and thus is not durable to repeated laundering.

Citric Acid Results

In citric acid The esterification reaction not only occurs between citric acid and cellulose but also
between citric acid and the hydroxy groups of chitosan, and free carboxylate groups can also
react with the amino groups of chitosan resulting in a salt linkage.

It is widely known that the Antimicrobial properties of cotton treated with chitosan is attributed
to amino groups of chitosan, which convert to ammonium salts in dilute acid solution; the salt
then binds to the negatively charged surface of the microorganism..

As a durable press and an Antimicrobial finishing agent for cotton fabric, citric acid and chitosan
show satisfactory results. there are slight improvements in tensile and tear strength using
chitosan as extender of the cross linking chain. A high Antimicrobial property level is obtained
by treatment with chitosan, and despite repeated launderings, the Antimicrobial property remains
at over 80%.

Effect of Molecular Weight on Activity of Chitosan

One of the most important characteristics of chitosan is its Antimicrobial activity at specific
molecular weights. Protonated amine groups in chitosan inhibit the growth of microorganisms by
holding negatively charged microorganism ions. Many studies have examined chitosan as an
Antimicrobial finish for textile materials, either for production of low molecular weight chitosan
followed by its application on textile fibers or for co-spinning or co-casting of low molecular
weight chitosan with cellulose molecules to make Antimicrobial fibers and films. However, these
methods had to produce chitosan with specific molecular weights, which could considerably
increase production costs. In addition, insolubility of chitosan in neutral or alkaline conditions
further limited its application.

29
A quaternary ammonium derivative of chitosan, N-2-hydroxy propyl-3-trimethylammonium
chitosan chloride (HTCC), is synthesized as an Antimicrobial finish for cotton using a reaction
of glycidyltrimethylammonium chloride (GTMAC) and chitosan. The use of crosslinking agents
or binders increase laundering durability of cotton treated with HTCC. A 5% nonionic binder
applied along with 0.1% or higher concentration of HTCC on cotton is quite effective in
increasing the laundering durability of the HTCC-treated cotton [28].

Flame Retardant Finish

Fabric Flammability

Fabric flammability is an important issue to consider, especially for drapery that will be used in a
public places such as a school, theatre or special event venue, since federal regulations require
that drapery fabrics used in such spaces be certified as fire retardant. Although all fabric will
burn, some are naturally more resistant to fire than others. Those that are more flammable can
have their fire resistance drastically improved by treatment with flame retardant chemicals.

Certain synthetic fibers are extremely flame resistant, including glass fibers and modacrylic.
Other synthetics, including certain polyesters, are slow to ignite and may even self-extinguish.
However, once synthetic fabrics ignite, they will melt rather than flame. The resulting substance
can lead to severe burns if it comes into contact with the skin.

Natural fibers typically do not melt. Wool and silk burn slowly, are difficult to ignite, and may
self-extinguish. With other untreated natural fabrics, such as cotton and linen, the fabric can
ignite quickly, resulting in a fast moving flame spread. Fabrics that include a combination of
natural and synthetic fibers, such as polyester-cotton blends, can be particularly troublesome, as
they combine the fast ignition and flame spread of the natural fiber with the melting aspect of the
synthetic fiber.

The ignition and burn factors of fabric are also affected by the weight and weave of the fabric.
Lightweight, loose weave fabrics will burn more quickly than heavier fabrics with a tight weave.
In addition, fabric flammability can also be affected by the fabric’s surface texture, with napped
fabrics (such as velvets and velours) igniting more easily than fabrics with a smooth surface.

Flame Retardancy of Fabrics

The good news is that the flammability of fabric can be drastically reduced through the use of
fire retardants. Many natural fibers, including cotton, can be topically treated with a chemical
that reduces the fabric’s flammability to the extent that it becomes nearly non-combustible.
During a fire, the chemical reacts with the gases and tars generated naturally by the fabric,
converting the gases and tars to carbon char, thus drastically slowing the fabric’s burning rate.

30
Some polyester fabrics are considered permanently flame retardant. This is because the fabrics
are manufactured utilizing fibers for which the flame retardant properties are built directly into
the molecular structure of the fibers. Fabrics manufactured utilizing Trevira™ and Avora™
polyester fibers are considered inherently or permanently fire retardant. Other synthetic fabrics
may be considered durably fire retardant, fire retardant, or non-fire retardant. “Durably fire
retardant” refers to a process in which polyesters are chemically treated during the
manufacturing process with a non-water soluble chemical. In other cases, synthetic fabrics may
be topically treated with chemicals after the manufacturing process (in the same manner as
natural fibers such as cotton), or may be untreated (or untreatable) and therefore considered non-
flame retardant.

When a fabric is designated as “inherently flame retardant,” “permanently flame retardant,” or

“durably flame retardant,” the flame retardancy will last for the life of the fabric. The drapery
can be laundered or dry-cleaned as recommended by the drapery manufacturer. In the case of
fabrics that are designated as “flame retardant,” that have been topically treated with chemicals,
the flame retardancy of the fabric will dissipate over time, particularly with repeated cleaning.
These fabrics must be dry-cleaned with a non-liquid cleaning agent. Typically, the flame
retardancy of topically treated fabric is certified for one year, though the actual length of time in
which the treatment remains effective will vary based on the number of times the drapery is dry-
cleaned and the environmental conditions in the location in which the drapery is used. It is
recommended that topically treated drapery be re-tested for flame retardancy on an annual basis,
and re-treated by a qualified professional as needed.

Categories of Flame Retardants

There are many categories in which fire retardants can be divided. The major categories among
them include:

 Tetrakis (hydroxymethyl) phosphonium salts that are made by passing phosphine gas
through a solution of formaldehyde and a mineral acid like hydrochloric acid. This
category is mostly used as flame retardants for textiles.

 Minerals like asbestos, compounds such as aluminum hydroxide, magnesium hydroxide,

antimony trioxide different hydrates, red phosphorus, and boron compounds, mostly
borates

 Synthetic materials, usually halocarbons which include organochlorines such as

polychlorinated biphenyls (PCBs), chlorendic acid derivates and chlorinated paraffins;
organobromines such as polybrominated diphenyl ether (PBDEs), organophosphates in
the form of halogenated phosphorus compounds and others [32]

31
Types of Flame Retardants

 Brominated flame retardants

 Chlorinated flame retardants

 Phosphorous-containing flame retardants {Phosphate ester such as Tri phenyl phosphate

 Nitrogen-containing flame retardants (i.e. Melamines)

 Inorganic flame retardants

Many of the flame retardants do not remain on the fabric, instead they slowly leak from the
products in the atmosphere. Brominated flame retardants are a subject of scrutiny. Evidence
shows that they are likely to exist long time in the environment, bio accumulate in the food chain
and finally in to our bodies. A survey of the newer flame retardants suggests a simple theory for
their constitution.

The molecule should be water-insoluble to achieve durability in laundering. A solvent-soluble

organic molecule will give better results. The ortho-phosphate group should be present in the
molecule to dehydrate catalytically the cellulose substrate. The molecule should contain
polymerizable groups to effect a permanency of finish. The molecule should contain halogen or
other groupings to reduce the flammability of the gases of decomposition.

When chemical free alternative materials or designs are not feasible, non halogenated flame
retardants can be used to meet fire safety standards. Numerous alternatives are available. It is
also confirmed that flame retardants based on Aluminum Trioxide, Ammonium Polyphosphates
and Red phosphorous are less problematic in the environment.

How do Flame Retardants Work?

Flame retardant chemicals that are applied to fabrics are intended to inhibit or suppress the
combustion process. These flame retardants interfere with combustion at different stages of the
process like during heating, decomposition, ignition or spreading of flame. For understanding
how flame retardants resist fire, first it should be known how a textile is heated up, catches fire
and contributes in spreading it.

As with any matter, a textile fabric exposed to a heat source experiences rise in temperature. If

32
the temperature of the fire source is high enough and the net rate of heat transfer to the fabric is
great, pyrolytic decomposition of the fiber substrate occurs. The products of this decomposition
include combustible gases, non combustible gases and carbonaceous char. The combustible
gases mix with the surrounding air and its oxygen. The mixture ignites, yielding a flame. It
happens when the composition of textile and the temperature, both are favorable. Part of the heat
generated within the flame is transferred to the fabric to sustain the burning process and part is
lost to the surroundings.

Now, if the textile is flame resistant then the flame retardant can act physically and/or chemically
by interfering at particular stages of burning. There are different mechanisms of flame retardants.

Mechanism of Flame Retardancy

Flame retardant systems for synthetic or natural polymers can act physically and/or chemically
by interfering at particular stages of burning.

By cooling, endothermic processes triggered by the flame retardants cool the substrate.

By forming a protective layer: The heat transfer is impeded, fewer pyrolysis gases are evolved,
and the oxygen is excluded.

By dilution. substances, which evolve inert gases on decomposition, dilute the fuel in the solid
and gaseous phases. The concentrations of combustible gases fall under the ignition limit.

Reaction in the gas phase: The free radical mechanism of combustion processes which takes
place in the gas phase could be interrupted by flame retardants.

Reaction in the solid phase: One mechanism is the accelerated breakdown of polymers.

Mechanisms of Flame Retardants

Fire retardants can act physically or chemically and sometimes both by physically and
chemically interfering at particular stages of burning. The different mechanisms are:

Endothermic Degradation
Certain compounds break down endothermically when they are subjected to high
temperatures. Magnesium and aluminium hydroxides are such examples. Various
hydrates also act similarly. The reaction takes off heat from the surroundings, thus
cooling the material.

33
Dilution of Fuel
Substances, which evolve inert gases on decomposition, dilute the fuel in the solid and
gaseous phases. Inert fillers, eg. talc or calcium carbonate, act as diluents, lowering the
combustible portion of the material, thus lowering the amount of heat per volume of
material that it can produce while burning. Thus the concentrations of combustible gases
fall under the ignition limit.

Thermal Shielding
A thermal insulation barrier is created between the burning and the yet-to-burn parts.
Intumescent additives are sometimes applied that turn the polymer into a carbonized
foam, resultantly separating the flame from the material and slowing down the heat
transfer to the unburned fuel.

Dilution of Gas Phase

Inert gases, mostly carbon dioxide and water, act as diluent of the combustible gases,
lowering their partial pressures and the partial pressure of oxygen, thus slowing the
reaction rate. These gases are produced by thermal degradation of some materials.

Gas Phase Radical Quenching

Chlorinated and brominated materials undergo thermal degradation and release hydrogen
chloride and hydrogen bromide. These react with the highly reactive H. and OH. radicals
in the flame, resulting in an inactive molecule and a Cl. or Br. radical. The halogen
radical has much lower energy than H. or OH. and thus has much lower potential to
propagate the radical oxidation reactions of combustion. Antimony compounds tend to
act in synergy with halogenated flame retardants. The HCl and HBr released during
burning are highly corrosive, which has reliability implications for objects subjected to
the released smoke.

Application of Flame Retardants on Textiles

Flame Retardants on fabric can be applied through conventional padding, padding with multiple
dips and nips. If followed by 30 to 60 seconds, it gives good results. The pH of the pad bath is
optimally kept at approximately 5.0. The amount of flame retardant required depends primarily
on the fabric type, application conditions, and test criteria required to be met with. Screening
experiments should be conducted to determine the minimum application level for a fabric.

One of the most common processes for applying Flame Retardants on cotton fabrics is the

34
"Precondensate"/NH3 process. One of several phosphoniums "precondensates" is applied after
which the fabric is cured with ammonia. Then it is oxidized with hydrogen peroxide.
Precondensate is the Tetrakis-hydroxymethyl phosphonium salt pre-reacted with urea or another
nitrogenous material. The amount of anhydrous sodium acetate is approximately 4% of the
amount of precondensate used. Some precondensates are formulated along with the sodium
acetate. Softeners are also added along with precondensates. A critical factor in the successful
application of precondensate/NH3 flame retardant is the control of fabric moisture before
ammoniation. Generally, moisture levels between 10% and 20% give good results [27].

An Ideal Flame Retardant for Cotton Should Posses the Following Properties:

Fast to washing/dry cleaning/light should be Ok

Low add on means High effectiveness.

Neutral or Alkaline Ok.

Fast to washing/dry cleaning/light should be Ok.

Low add on means High effectiveness.

Neutral or Alkaline Ok.

Contains glow proofing elements. Ok.

Non-toxic in the fiber and treatment bath.

Compatible with other finishes. Ok.

Low cost.

Minimum effect on fabric handle, strength and abrasion resistance Ok.

Good flame retardant effect.

No effect on shade / fastness of dyes.

Minimum smoke /toxic gas emitted.

35
Pyrovatex® CP New (Flame Retardant Finish)

History

PYROVATEX® CP New was introduced in 1960 as a durable flame retardant product for
cellulose fibers. Continuous improvements have reflected changes in market requirements and
environmental awareness, yet one thing has remained constant since its introduction:

Properties

 PYROVATEX® CP New offers the maximum combination of overall flame and heat
protection and unsurpassed comfort available in treated garments.

 PYROVATEX® CP New has been used to treat more than 100 million linear yards of
fabrics. Garments produced from these fabrics provide life-saving protection to people
around the world.

 Pyrovatex® CP New is manufactured by the Swiss based company Ciba (now known as
Swisstex). Pyrovatex® CP New provides maximum protection against heat and flame
combined with superior comfort at a very affordable price.

It has been laboratory tested using live subjects with particularly sensitive skin. Testing
has been conducted by San Francisco Medical Center University of California, Canton
Hospital Zurich, Dermatology University, Food and Drug Research Lab.
Inc.Conshocken, Pa USA and more. Testing showed that none of the tested individuals
had any negative skin reactions after contact with the skin for prolonged periods of time.
Pyrovatex® fabric is gentle and non-irritating to even the most sensitive skin [32].

Swisstex Chemicals
Old name of Swisstex Chemicals was Ciba. Ciba Specialty Chemicals Inc. is one of the world’s
leading organizations dedicated to producing high value effects for its customers’ products.
Active in a variety of industries including the textile market, Ciba develops, manufactures and
markets a complete line of leading textile chemicals in more than 117 countries – adding value to
virtually every step of the textile manufacturing process. Our innovative products enhance the
performance, look and feel of fabrics; create comfort; promote care and provide protection. Ciba
Specialty Chemicals Inc. has also been evaluating the ecological value of its products for quite
some time. This brochure highlights our ecological commitment.

36
Cotton Fiber

Cotton is a natural vegetable fibre produced in the cotton plant in many countries of the world
even in Bangladesh also. Some important properties of cotton fibres are discussed briefly below:

Properties of Cotton Fibres

Length of Cotton Fiber

Physically the individual cotton fibres consist of a single long tubular cell. Its length is about
1200-1500 times than its breadth. Length of cotton fibre varies from 16mm to 52 mm depending
upon the type of cotton.
Indian cotton- 16-25 mm
American cotton- 20-30 mm
Sea Island- 38-52 mm
Egyptian cotton- 30-38 mm

Fineness of Cotton Fiber

Longer the fibre, finer the fibre in case of cotton fibre. It is expressed in term of decitex and it
varies from 1.1 to2.3 decitex.
Indian= 2.2-2.3dtex
American= 2.1-2.2 dtex
Egyptian= 1.2-1.8 dtex
Sea Island= 1.0-1.1 dtex
Fineness may be more in case of immature fibre. So it is necessary to express maturity with
fineness.

Strength And Extension of Cotton Fiber

Cotton fibre is fairly among natural fibres in relation to tenacity which is 3-3.5g/dtex. Its tensile
strength is between wool and silk fibre but disadvantage is low extension at break which is 5-7%.

Elastic Properties of Cotton

Recovery from deformation of cotton fibre, yarn or fabric from applied load is very low. By

37
applying heat it can’t be achieved. This property can be achieved by -1.Chemical treatment to
improve crease recovery, but the problem is the materials become harsher due to chemical
treatment 2. blending or mixing of cotton with elastic fibre, e.g. polyester, blend ratio depends on
the end use of the fabric. The initial modulus is fairly high=0
5 g/dtex (wool=0.25 g/dtex)

Cross Section
Cross-section of cotton fibre is somewhat ribbon like. The cell wall is rather thin and the lumen
occupies about two-third of the entire breadth and shows up very prominent in polarized light.
Fibre cross-section becomes round when mercerized.

Appearance

Cotton fibre is fairly short, fine and creamy white color. Color of the fibre depends on soil of
growth. By adding chemicals in the soil, color of the cotton fibre may be varied.

Crimp

Cotton fibre is more or less twisted on its longitudinal axis which cab not be seen from out side
is called convolution. The twist in the fibre does not to be continuous in one direction i.e. if at
first right direction, then left direction. This property of cotton fibre helps in spinning.

Why Cotton is Used for Antimicrobial & Flame Retardant Activity Instead of Polyester?
As the cotton fiber is hydrophilic so, when a flame retarded and antimicrobial agent is applied, it is
absorbed by cotton, not by Polyester.

38
 Chapter # 2

Experimental Work

The Antimicrobial finishes can be applied to the textile substrates by the following techniques:

 Exhaust Method

 Pad – Dry – Cure Method

 Coating Method

 Spray Method

 Foam Method

Various Methods For Improving The Durability Of The Finish Include:

 Insolubilisation of the active substances in/on the fiber.

 Treating the fiber with resin, condensates or cross-linking agents.

 Micro encapsulation of the antimicrobial agents with the fiber matrix.

 Coating the fiber surface.

 Chemical modification of the fiber by covalent bond formation.

 Use of graft polymers, homo polymers and/or co polymerization on to the fiber.

The application of antimicrobial finishes depends on its type. i.e. leaching or non-leaching
antimicrobial finish. Hence we will discuss the application of both finishes with the help of
commercial examples.

Application of Leaching Antimicrobial Finishes

These finishes can be applied with help of continuous, exhaust methods and Pad -- Dry -- Cure.
Hence we will only discuss Pad-dry-cure method of application.

39
Mode of Application
We have 9 different recipes with different amounts of auxiliaries. In every recipe , we changed
amounts of Chitosan , Knittex CHN and Pyrovatex CP New. Amounts of rest of
chemicals/auxilaries in which Acetic Acid, Phosphoric Acid, Turpex ACN New and Invadine
PBN included, are kept constant.

Run Order Chitosan Knittex CHN Pyrovatex CP

1 0.5 50 400
2 0.5 80 200
3 1 80 200
4 0.5 80 400
5 0.5 50 200
6 1 80 400
7 1 50 400
8 1 50 200

9 0.75 65 300

 Invadine PBN= 5 ml/l

 Turpex ACN New = 45 g/l

 Acetic acid = 2 ml/l

 Phosphoric Acid = 20g/l

Apparatus (Laboratory Preparation)

Beakers, Stirrer, pH Meter, Eye Cleaner, Measuring Balance, Scissors etc.

40
Chemicals
Chitosan, Crosslinking agent(CHN), Acetic Acid, Pyrovatex CP New, Wetting Agent (PBN),
Softner Turpex CAN New and Water etc.

Pretreatment
Before application the sample must be acidified. It must be free from active chlorine and residues
of production additives such as sizes, printing thickeners etc because they can have negative
influence on the effectiveness and durability of finish.

pH of Bath
The pH of bath must be in between 5-6. Higher pH values may damage the absorption capacity
of substrate. The absorption properties can be improved by treating the substrate with any type of
wetting agent. e.g. “Invadine PBN”

We can regulate the pH with the help of acetic acid.

Application Way

 Prepare solution according to recipe calculation.

 Take sample of bleached cotton fabric.

41
 Remember! Sample of fabric should be only bleached ; neither mercerized nor OBA
(Optical Brightening Agent) applied.

 Set the pick up of padder of padding machine at 70%

 Set the temperature of curing machine for drying at 120°C for 1-2 minutes

 After drying, again set the temperature of curing machine at 150 °C for 5 minutes or 170
°C for 1minute for curing.

Procedure
The fabric is dipped in a solution and padded on a padding machine. Adequate liquor pick-up is
essential 70-90 %, depending on weight and construction of fabric and can be achieved by a
combination of absorbent fabric and long contact of the fabric with the liquor (padding speed).

Drying
Drying on curing machine should be carried out with maximum overfeed. The recommended
drying temperature is 120 °C for 1-2 minutes.

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. If the residual moisture on the goods is too
high, they may end up with a harsh handle as a result of migration.

Curing

 In the curing oven, 5 min at 150 °C must be guaranteed.

 In the case of curing on stenter, 30 to 60 sec at 170 °C are sufficient.

42
  It is advisable to check the curing effect at regular intervals.

 Drying and curing should be carried out at maximum rate of air replacement. This largely
prevents soiling of the machinery.

 If the goods are to be batched up after curing, it is advisable to cool them below 40 °C,
for example by passing the fabric over a cooling device

 By this method we can prepare samples according to our requirement.

Precautionary Measures

 Wear goggles or face shield and rubber gloves when handling the concentrated material

 “Chitosan and Pyrovatex” must be stored at room temperatures. i.e. up to 30oC.

 On contact with skin it can cause a little rash or irritation so avoid contact with skin.

43
Advantages

 Lasting hygienic freshness and greater wear comfort

 Prevents microbially caused odors

 Protects functional characteristics (e.g. elastomer fibers)

 Protects against discoloration and felting caused by micro-organisms

 Safe hygiene

 Good wash fastness

Application of Non-Leaching Antimicrobial Finishes

These finishes can be applied by brushing, dipping, padding, soaking, spraying, fogging or by
using foaming

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 Chapter # 3

Testing of Anti Microbial & Flame Retardancy

Verification Tests of Antimicrobial Finish

After the application of antimicrobial finishes on textiles we check whether our finish has been
applied to the substrate according to the requirement of customer or not. For this purpose there
are many verification tests.

In this chapter we will discuss two major verification tests of antimicrobial finishes. i.e.

 Verification Test for application of finish on substrate

 Verification Test for checking the type of finish applied on the substrate. i.e. leaching or
non-leaching

Verification Test for the Application of Finish

There are two types of test for verification of antimicrobial finsh:

(i) Quantitative Test

(ii) Qualitative Test

Qualitative Test helps us to determine the exact numerical value of how much effective
antimicrobial is.

Qualitative Test helps us to verify that whether antimicrobial finish is applied properly on the
substrate or not. The test that we commonly use on industrial scale is known as “BPB (Bromo
Phenol Blue)” Test.

In Interloop Private Limited, there is only facility of BPB (Bromo Phenol Blue)” Test to verify
antimicrobial finish. So, we did verification of antimicrobial finish of our nine samples via. BPB
(Bromo Phenol Blue)” Test.

BPB (Bromo Phenol Blue)

This is a qualitative method for detecting the presence of antimicrobial finishes on light
and dark colored substrates. We will discuss this test for both types of substrates.
Actually BPB is a sodium salt of bromo-phenol blue.

45
Test for Dark Substrates
Field of Detection
It is basically not designed to detect the presence of “Antimicrobial Finish” but we can also use it
to detect the Chitosan .

Test Method
Standards According to the Company

 Prepare 0.001 % solution of BPB

 Take a sample of 2 × 2 inch2

Apparatus

Beakers, Stirrer, Petridishes, Eye cleaner, Measuring Balance, Measuring Cylinders, Scissors,
Glass jars etc.

Chemicals

BPB (Bromo-phenol blue), Distilled Water etc

Pretreatment of Sample

Before application the sample must be acidified. It must be free from active chlorine and residues
of production additives such as sizes, printing thickeners etc.

Application of BPB to the Sample

 First of all take some fabric and make a sample of 2 2 inch2 from them by cutting them
into pieces with the help of scissor.

 Now prepare the BPB solution according to the type of substrate (light or dark) and
standards given. Mostly we prepare 500ml or 1000ml of solution in glass jars. The color
of the solution is purple.

 Now place the dark treated samples into the glass jar for 2 minutes. Stirerr this solution
constantly. Now remove the sample from the solution, place them in petridishes and
observe the color of the solution of BPB.

 The solution may have two possible colors according to the antimicrobial treatment given
to the sample. i.e.

46
For well-treated sample the solution will have very light or virtually no purple color

For untreated or poorly treated sample the solution will have a dark purple color

47
Test for Light Substrate
Field of Detection

It is basically not designed to detect the presence of “Antimicrobial Finish” but we can also use it
to detect the Chitosan

Test Method

Standards According to the Company:

 Prepare 0.025 % solution of BPB

 Take a sample of 2 2 inch2

Apparatus

Beakers, Stirrer, Petridishes, Eye cleaner, Measuring Balance, Measuring Cylinders, Scissors,
Glass Jars etc.

Chemicals

BPB (Bromophenol blue), Distilled Water etc

Pretreatment of Sample

Before application the sample must be acidified. It must be free from active chlorine and residues
of production additives such as sizes, printing thickeners etc.

Application of BPB to the Sample

First of all take some fabric and make a sample of 2 × 2 inch2 from them by cutting them into
pieces with the help of scissor.

Now prepare the BPB solution according to the type of substrate (light or dark) and standards
given. Mostly we prepare 500ml or 1000ml of solution in glass jars. The color of the solution is
purple.

48
Now place the light treated samples into the glass jar for 2 minutes. Rinse the solution
constantly, then after 2 minutes remove the samples and rinse them in hot water in a separate jar.
After rinsing place these samples into the petridishes and then compare them with the “BPB
Color Test Scale”.

The “BPB Color Test Scale” is as follows:

Conclusion
With the help of BPB (Bromo Phenol Blue) Test, we concluded that how much effective is
Chitosan on our samples.

49
Quantitative Test

There are some also quantitative tests by which we can get exact numerical value of
effectiveness of antimicrobial finish. Quantitative Tests are given below:

 AATCC Test Method 100

AATCC Test Method 100 is the testing of assessment of antibacterial finishes on textile
material.

 AATCC Test Method 147

AATCC Test Method 147 is testing of antibacterial activity assessment on textile
material.

REMEMBER! This method is not suitable for materials which tend to encapsulate and
prevent the diffusion of the antibacterial agent-neutralizing substances.

Future of Antimicrobial Finishes

In Pakistan and in almost all parts of the world these antimicrobial finishes are mostly used in
knitted fabrics. i.e. socks or some undergarments.

But with the advancement and passing of time people are getting more conscious about their
health and in coming time it is believed that these finishes will be applied to almost all type of
textiles used in wearing to assure maximum satisfaction for the customer that the fabric which
he/she is buying for him/herself will also protect him/her from harmful microorganisms, because
these finishes are expensive so mostly we are using them in sensitive substrates where the
growth of microbes is easy like in socks, baby diapers etc.
But researches are being done in order to prepare cheap antimicrobial finishes and soon they will
be introduced in almost all types of textile materials.

Verification Tests of Flame Retardancy on Cotton Fabric Samples

NFPA 701 Test

Fabrics used in most public places (including schools, churches, auditoriums, theatres, and
more.) is required by law in many states and cities to be certified as flame retardant, according to
standards developed by the National Fire Protection Association (NFPA). NFPA has various

50
standards depending on how the fabric will be used. In the case of draperies, curtains, and similar
hanging textiles, the standard that applies is NFPA 701: Standard Methods of Fire Tests for
Flame Propagation of Textiles and Films. This test measures the flammability of a fabric when it
is exposed to specific sources of ignition.

NFPA 701 (Small Scale) testing measures the ignition resistance of a fabric after it is exposed to
a flame for 12 seconds. The flame, char length, and flaming residue are recorded. The fabric will
pass the test if all samples meet the following criteria:

1. An after flame of less than 2.0 seconds

2. A char length of less than 6.5”
3. The specimen does not continue to flame after reaching the floor of the test chamber

Fabric certified as flame retardant is certified to have been tested and passed the NFPA 701 test
[33].

We did this flame retardancy testing of our samples in Al-Rehmat Textile Mills.

16 CFR 1610 Test

Purpose
Test is carried out for rating for flammability of textiles and textile products for clothing use

Standard establishes three classes of flammability for classifying textiles and warns against the
use of textiles that have burning characteristics unsuitable for clothing.

Class 1:

 Normal Flammability: Fabric meets minimum requirements of the standard and has no
un-usual burning.

 Plain Surface Fabric: Average burn time 3 seconds or above

 Raised Surface Fabric: Average burn time is 7 seconds or above

Class 2:

 Intermediate Flammability: Fabric meets minimum requirements with flammability

characteristics between normal and rapid and intense burning

 Plain Surface Fabric: No standard ; should not be sold.

 Raised Surface Fabric: Average burn time is 4 to 7 seconds with 2 or more base burns

51
The class of fabric is still technically acceptable to sell in US. However , CPSC has been asking
retailers to say away from Class 2 fabrics mainly because some of Class 2 fabrics may turn into
Class3 when more garments are treated.

Class 3:

Rapid and intense burning. Fabric dangerously flammable and un-suitable for clothing

 Plain Surface Fabric: Average burn time is less than 3.5 seconds.
 Raised Surface Fabric: Average burn time is less than 4 seconds with 2 or more base
burns

Testing Procedure
 First of all, Fabric in dry cleaned/washed state is cut into specimens (2” × 6”) which are
dried and cooled.
 Specimens are placed at 45˚ angle and impinged with a flame (5/8” length) for 1 second.
 Burn times as well as burning characteristics are recorded [34].

Conclusion
In this way, we will conclude that how much effective is flame retardancy of fabric by observing
different parameters like tear strength, char length etc.

52
 Chapter # 4

Samples & Conclusions

In this chapter, antimicrobial activity and flame retardancy of the treated fabric is investigated
against different concentration of Chtosan, Pyrovatex® CP New and Knittex CHN.

First of all, we will talk about the results of effectiveness of antimicrobial activity.

Sample # 1

53
Sample # 2

Sample # 3

54
Sample # 4

Sample # 5

55
Sample # 6

Sample # 7

56
Sample # 8

Sample # 9

57
Conclusion of Testing Results of Antimicrobial Activity

It is concluded from testing results of antimicrobial activity that sample like 1, 2, 4 and 5
have 0.05grams/100ml amount of Chitosan in their recipes. Amount was less and when
we compare their results with given table then we concluded that “It comes in the
category of “”Under Treated”.

Similarly when we compare Sample # 9 with Standard BPB Color Test Scale then we
concluded that it comes in the category of “Slightly Under Treated”. In this recipe,
amount of Chitosan was 0.075grams/100ml.

When we again compare Sample # 3, 6, 7 and 8 with Standard BPB Color Test Scale then
we concluded that they come in the category of “Good Treated”. In these recipes, amount
of Chitosan was 0.1grams/100ml.

58
Now we will talk about the results of effectiveness of flame retardant finish.

Sample # 1

59
Sample # 2

Sample # 3

60
Sample # 4

Sample # 5

61
Sample # 6

Sample # 7

62
Sample # 8

Sample # 9

63
Conclusion

It is concluded that amount of Pyrovatex® CP New has a direct impact on results.

Sample 2, 3, 5 and 8 have 20grams/100ml amount of Pyrovatex® CP New in their
respective recipes. Due to less amount of Pyrovatex® CP New, burned portion is more
comparatively others, which have greater amount of Pyrovatex® CP New in their
solutions.

Sample 9 has 30grams/100ml amount of Pyrovatex® CP New in its recipe. It has slightly
better result as compared to sample 2, 3, 5 and 8.

Sample 1, 4, 6 and 7 have 40grams/100ml amount of Pyrovatex® CP New in their

recipes. Due to proper amount of Pyrovatex® CP New in their solutions, we succeed to
achieve best result.

 We can also observe by analyzing burning portion, char length and tensile strength.

64
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66