Wollo University

Kombolcha Institute of Technology

School of Textile Leather and Fashion Design

Module: Textile Pretreatment and Finishing

By

Textile ❖ Seid Shiferaw (MSc.)

Pretreatment ❖ Prof. Vishnu Appa Dorugade (PhD)

Finishing ❖ Fenta Mehabie (Msc.)

Technology ❖ Badasa Abebe (MSc.)

Target group: 5th year Textile Engineering Students

Kombolcha, Ethiopia, February 15, 2023

Part I: Textile Pretreatments .............................................................................. 1
1.1 Need for preparation/pretreatment. .....................................................................................1
1.2 Chemical structure of cellulose...........................................................................................2
1.4 Wool: a protein fibre ..........................................................................................................4
1.4.1 Impurities in wool ........................................................................................................4
1.5 Silk ....................................................................................................................................5
1.7 Process sequence in pretreatment processing ......................................................................5
Chapter Two ........................................................................................................ 7
SINGEING ........................................................................................................... 7
2.1 Singeing .............................................................................................................................7
2.2 Types of singeing ...............................................................................................................8
2.2.1 Plate singeing machine .................................................................................................8
2.2.2 Rotary cylinder machine ..............................................................................................9
2.2.3 Gas Singeing ................................................................................................................9
2.3 Singeing Parameters...................................................................................................... 10
2.4 Fabric singeing................................................................................................................. 10
2.5 Problems in Gas Singing .................................................................................................. 11
2.6 Yarn singeing ................................................................................................................... 12
2.7 Assessment of singeing efficiency .................................................................................... 12
Chapter Three .....................................................................................................14
DE-SIZING .........................................................................................................14
3.2 Hydrolytic Desizing ......................................................................................................... 15
Acid desizing: ..................................................................................................................... 15
3.3 Enzymatic desizing: ......................................................................................................... 15
3.3.1 Enzyme Sources for Desizing:.................................................................................... 16
3.3.2 High temperature enzymatic desizing ......................................................................... 18
3.4 Oxidative Desizing........................................................................................................... 18
3.5 Assessment of desizing efficiency .................................................................................... 20
3.5.1 Reagent preparation ................................................................................................... 20
3.5.2Method of testing ........................................................................................................ 21
Chapter Four.......................................................................................................23
SCOURING .........................................................................................................23
4.1 Basic surfactant concepts ................................................................................................. 23

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 4.1.1 Why surface tension of a solution goes down in presence of a surfactant? .................. 24
4.1.2 Surfactant Aggregation in Solution ............................................................................ 24
4.2 Scouring Process .............................................................................................................. 25
4.3 Machinery for Scouring.................................................................................................... 30
4.4 Assessment of scouring efficiency.................................................................................... 33
Chapter Five ........................................................................................................37
MERCERIZATION ...........................................................................................37
5.1 Structural Modification .................................................................................................... 38
5.1.1 Effect of NaOH Concentration ................................................................................... 38
5.1.2 Effect of temperature.................................................................................................. 38
5.1.3 Enhancement in luster ................................................................................................ 39
5.2 Mechanical properties ...................................................................................................... 40
5.2.1 Effect of tension ......................................................................................................... 40
5.2.2 Effect of Alkali concentration .................................................................................... 40
5.3 Dyeing Properties............................................................................................................. 41
5.4 Hot mercerization............................................................................................................. 41
5.5 Mercerization of blends .................................................................................................... 42
5.5.2 Problems faced in mercerization of cotton/viscose blends .......................................... 42
5.6 Machines for Mercerization: ............................................................................................ 43
5.6.1 Yarn mercerization..................................................................................................... 43
5.6.2 Fabric mercerizing machines: ..................................................................................... 44
5.7 Determination of degree of mercerization (Barium activity number): ............................... 45
Chapter Six..........................................................................................................48
BLEACHING ......................................................................................................48
6.1 Introduction to Bleaching .............................................................................48
6.2 Bleaching with sodium Hypochlorite (NaOCl): ................................................................ 50
6.2.1 Bleaching of cellulosic fibres with NaOCl: Influence of process parameters .................. 50
6.3 Bleaching with NaClO2 (sodium chlorite) ........................................................................ 54
6.3.1 Effect of Temperature: ............................................................................................... 56
6.3.2 Antichlor Treatment ................................................................................................... 56
6.4 Bleaching with hydrogen peroxide (H2O2)........................................................................ 57
6.4.1 Auxiliaries Used In H2O2 Bleaching........................................................................... 57
6.4.2 Effect of Process parameters ...................................................................................... 59

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 6.5 Assessment of bleaching efficiency .................................................................................. 60
6.6 Optical whitening agents .................................................................................................. 61
6.6.1 Mechanism of OBA action ......................................................................................... 62
6.6.2 OBAs for cellulosic substrates.................................................................................... 63
Chapter Seven .....................................................................................................67
7.1 Combined Desizing and scouring ..................................................................................... 67
7.2 Combined scouring and bleaching .................................................................................... 68
7.3 Combined desizing, scouring and bleaching ..................................................................... 69
Chapter Eight ......................................................................................................73
PRETREATMENT OF OTHER TEXTILE FIBERS ......................................73
8.1 Preparation of Protein Fibres ............................................................................................ 73
8.1.1 Preparation of Wool ................................................................................................... 73
8.1.2 Impurities in raw wool ............................................................................................... 73
8.1.3 Wool scouring ............................................................................................................ 74
8.1.4 Carbonization of wool ................................................................................................ 74
8.1.5 Wool Bleaching ......................................................................................................... 77
8.2 Pretreatment of Silk ......................................................................................................... 79
8.2.1 Extraction with water ................................................................................................. 80
8.2.2 Boil-off in soap .......................................................................................................... 80
8.2.3 Degumming with Alkali Buffer .................................................................................. 80
8.2.4 Degumming with Organic Acids ................................................................................ 82
8.2.5 Degumming with Enzymes ........................................................................................ 82
8.2.6 Degumming with Aliphatic Amines ........................................................................... 83
8.2.7 Assessment of degumming ......................................................................................... 83
8.2.8 Bleaching of silk ........................................................................................................ 84
8.3 Preparation of manmade and synthetic fibres and Blends ................................................. 84
8.3.1 Scouring of Polyester: ................................................................................................ 85
8.3.2 Bleaching of polyester:............................................................................................... 85
8.3.4 Scouring of Nylon: ..................................................................................................... 86
8.3.5 Scouring of acrylic (PAN) .......................................................................................... 87
8.3.6 Scouring of Viscose: .................................................................................................. 87
8.3.7 Pretreatment of Blends ............................................................................................... 88
Chapter Nine .......................................................................................................92

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 ASSESSMENT OF VARIOUS PRETREATMENT PROCESSES ........................................ 92
9.1 Desizing........................................................................................................................ 92
9.2 Scouring ....................................................................................................................... 93
9.3. Mercerisation ............................................................................................................... 98
9.3.1 Barium Activity Number (BAN) ................................................................................ 98
9.4 Heat Setting ..................................................................................................................... 98
9.4.1 Effect of tension on Properties ................................................................................... 99
9.4.2 Recommended setting temperatures ........................................................................... 99
9.4.3 Effect of heat setting on fibre properties ................................................................... 100
CHAPTER ONE ...............................................................................................104
MECHANICAL AND CHEMICAL FINISHES .............................................104
1.1 Introduction to Finishing ................................................................................................ 104
1.2 Classification of finishing ......................................................................................... 104
1.2.1 According to the nature of Finish ............................................................................. 104
1.2.2 Classification according to degree of permanence .................................................... 105
1.2.3 Classification according to performance ................................................................... 105
1.3 Mechanical Finishing ..................................................................................................... 105
1.3.1 Calendaring.............................................................................................................. 105
1.3.2 Compacting.............................................................................................................. 106
1.3.3 Embossing ............................................................................................................... 106
1.3.4 Sueding .................................................................................................................... 106
1.3.5 Raising or Napping .................................................................................................. 107
1.3.6 Sanforizer ................................................................................................................ 107
1.3.7 Stentering................................................................................................................. 107
1.4 Chemical Finishing ........................................................................................................ 108
1.4.1 Methods of Application ............................................................................................ 108
CHAPTER TWO ..............................................................................................114
DURABLE-PRESS FINISHES ........................................................................114
2.1 Theory of Wrinkling ...................................................................................................... 114
2.2 Mechanisms of easy-care and durable press finishing ..................................................... 114
2.3 Examples of textiles with easy-care and durable press finishes ....................................... 115
2.4 Chemistry of easy-care and durable press finishes .......................................................... 116
2.4.1 Formaldehyde-containing products .......................................................................... 116

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 2.4.2 Formaldehyde considerations ................................................................................... 120
2.4.3 non-formaldehyde containing products. .................................................................... 121
2.5 Application methods ...................................................................................................... 123
2.6 Compatibility with other finishes.................................................................................... 124
2.7 Formaldehyde testing ..................................................................................................... 124
CHAPTER THREE ..........................................................................................127
REPELLENT FINISHES .................................................................................127
3.1 Introduction ................................................................................................................... 127
3.2 Theory of wetting ........................................................................................................... 128
3.3 High-energy versus low-energy surfaces ........................................................................ 130
3.3.1 Critical surface tension ............................................................................................. 130
3.4 Mechanism of repellency ............................................................................................... 131
3.5 Water proofing and water repellency .............................................................................. 132
3.5.1 water repellency ....................................................................................................... 132
3.5.2 Water proofing ......................................................................................................... 133
3.5.3 Undesirable Effects of water repellency ................................................................... 134
3.6 Stain and soil retardancy ................................................................................................ 134
3.7 Repellent Chemistry ....................................................................................................... 136
3.7.1 Paraffin repellents .................................................................................................... 136
3.7.2 Stearic acid–melamine repellents ............................................................................. 137
3.7.3 Silicone water repellents .......................................................................................... 137
3.7.4 Fluorocarbon-based repellents .................................................................................. 138
3.8 Test methods .................................................................................................................. 140
CHAPTER FOUR.............................................................................................143
RETARDANT FINISH.....................................................................................143
4.1 Flame Retardant finishes ................................................................................................ 143
4.2.1 Thermal properties of textile materials ..................................................................... 143
4.1.2 Combustion Cycle for Fibers.................................................................................... 144
4.1.3 Flammability of textile fibers ................................................................................... 145
4.1.4 Limiting oxygen index ............................................................................................. 147
4.1.5 Flame Retardants ..................................................................................................... 148
4.1.5 Mechanism of flame retardancy ............................................................................... 148
4.1.6 Flame-retardant chemistry ........................................................................................ 150

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 4.1.7 Flame retardants for cellulose ................................................................................... 150
4.1.8 Flame-retarding fibre blends .................................................................................... 152
4.1.9 Evaluation of flame retardants .................................................................................. 152
4.1.10 Requirements of Flame-retardant Textiles .............................................................. 153
4.1.11 Applications of flame retardant textiles .................................................................. 153
4.2 UV protective finishes .................................................................................................... 153
4.2.1 The definition and effects of UV Radiation .............................................................. 154
4.2.2 Mechanism of UV protection ................................................................................... 155
4.2.3 Protection factor ....................................................................................................... 156
4.2.4 Methods of ultraviolet protection ............................................................................. 156
4.2.5 Chemistry and mechanisms of UV protection finishes .............................................. 156
4.2.6 Application methods ................................................................................................ 157
CHAPTER FIVE ..............................................................................................160
ANTI FINISHES ...............................................................................................160
5.1 Antimicrobial finishes .................................................................................................... 160
5.1.1 Microbes or microorganisms .................................................................................... 160
5.1.2 Antimicrobial ........................................................................................................... 161
5.1.3 Growth of microorganism ........................................................................................ 161
5.1.4 Effects of microbial growth on textiles and human health ......................................... 161
5.1.5 Types of antimicrobial finishing agent ..................................................................... 162
5.1.6 Properties of an effective antimicrobial finish .......................................................... 162
5.1.7 Mechanisms of antimicrobial finishes ...................................................................... 163
5.2 Insect resist, mite protection ........................................................................................... 164
5.2.1 Insect resist .............................................................................................................. 164
5.2.1.1 Mechanisms of insect resist finishes ...................................................................... 164
5.2.1.2 Application Area ................................................................................................... 165
5.2.1.3 Application Methods ............................................................................................. 165
5.2.2 Finishes for protection from dust mites..................................................................... 165
5.3 Antistatic finishes........................................................................................................... 166
5.3.1 The concept of antistatic finishes.............................................................................. 166
5.3.2 Effects of static charge on textiles ............................................................................ 166
5.3.3 Mechanisms of antistatic finishes ............................................................................. 167
5.3.4 Chemistry of antistatic finishes ................................................................................ 167

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 5.3.5 Conductive fibres ..................................................................................................... 168
CHAPTER SIX .................................................................................................172
HAND MODIFICATION OF TEXTILES ......................................................172
6.1 Soft Finishes .................................................................................................................. 172
6.1.1 Reasons for using softener........................................................................................ 173
6.1.2 Classification of textile softeners according to their ionogenity ................................ 173
6.1.3 Softening Mechanism............................................................................................... 174
6.1.4 Requrements of softners ........................................................................................... 174
6.1.7 Silicon Softeners ...................................................................................................... 177
6.2 Hand building finishes ................................................................................................... 180
6.2.1 Hand building classification ..................................................................................... 180
6.2.3 Hand builder chemistry ............................................................................................ 181
6.3.2 Bio-denim Washing ................................................................................................. 185
6.3.3 Enzymatic Ageing .................................................................................................... 187
6.3.4 Bio-Carbonizing....................................................................................................... 188
CHAPTER SEVEN ...........................................................................................192
OTHER CHEMICAL FINISHES ....................................................................192
7.1 Anti-pilling finishes ....................................................................................................... 192
7.1.2 Pilling mechanism .................................................................................................... 192
7.1.2 Mechanisms and chemistry of anti-pilling finishes ................................................... 193
7.2 Non-Slip finishes ........................................................................................................... 194
7.2.1 Mechanisms of non-slip finishes .............................................................................. 194
7.2.2 Chemistry of non-slip finishes .................................................................................. 194
7.2.3 Application methods and combinability ................................................................... 194
REFERENCES .................................................................................................196

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 Part I: Textile Pretreatments
Chapter One
INDTRODUCTION

1.1 Need for preparation/pretreatment.

The basic objective of pretreatment is removal of added and natural impurities present in textile
fibres to facilitate further processing. This prepares the textile substrate for downstream
processes like dyeing, printing, finishing, etc.

The impurities present depends on the fibre type (generally high in natural fibres). In general,
synthetic fibres have added impurities like additives or chemicals which are added to facilitate
certain processes like weaving (sizing) or prevention of static (lubrication/antistatic treatment
during melt spinning).

Pretreatment stage

✓ Is non- value –added stage of the coloration process

✓ Makes excessive use of chemicals, auxiliaries and utilities
✓ Is characterized by high carry-over of preparation residues in the effluent water which
has a major impact on the effluent treatment of the discharged water.
✓ Effluent load varies from fibre to fibre.

This makes it imperative to understand the science of impurity removal and functions of various
chemicals and auxiliaries used in pretreatment of textiles.

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Major Textile fibres
Natural Synthetic/Man made
Cotton Polyester
Wool Nylon
Silk Acrylic
Viscose

The composition of cotton is given in Table 1.1 below:

Table.Composition of cotton

Constituent Composition of a fibre

Typical (%) Low (%) High (%)

Cellulose 94.0 88.0 96.0

Protein 1.3 1.1 1.9

Pectic matter 0.9 0.7 1.2

Wax 0.6 0.4 1.0

Mineral matter 1.2 0.7 1.6

Coloring Matter 0.8 0.5 1.0

Total sugars 0.3 - -

Most of the impurities in cotton are concentrated in the primary cell wall.

1.2 Chemical structure of cellulose

Cotton is one of the purest natural sources of cellulose. In natural cellulose, the crystal form
of cellulose, known as Cellulose, I is different from that of regenerated cellulose which is
known as cellulose II. Cellulose II is thermodynamically more stable than cellulose I and
hence any attempt to change the cellulose, whether by mercerization or regeneration may
result in conversion of cellulose I to cellulose II (partially or completely). Chemically,
cellulose is 1, 4-β-D-glucan or a condensation polymer of β-D-glucopyranose. The glucose
units are linked at 1-4 position, resulting in formation of 1, 4-glycosidic bonds. In the
cellulose polymer, there is a reversal of every alternate unit, and hence the monomer of
cellulose is actually cellobiose (consisting of two glucopyranose units) and not glucose
(single unit). In that sense cellulose is different from starch, which has a single unit of

2
 glucose as repeat unit. The reversal helps cellulose polymer to form linear chains whereas
starch polymer chains form helical conformations. The degree of polymerization may lie in
the range of 1000-2000.

The chemical structure of cellulose is depicted in figure 1.2 below. (note the reversal at every
alternate unit)

Figure. Chemical structure of cellulose with four residues

1.3 Impurities in cotton

Proteins

Proteins present in cotton are mostly concentrated in cuticle and lumen. They are vegetable
proteins. Proteins can be called polymers of amino acids. Amino acids are organic molecules
having both the acidic (carboxylic) and basic (amine) groups present on the same unit. They
impart yellowish color to cotton.

Pectins

Pectins are derivatives of pectic acid and are found in the cover of citrus fruits. These are
polymers of high molecular weight polysaccharide that acts as a cementing material in the
cell walls of all plant tissues. It is a polymer of α-Galacturonic acid with a variable number of
methyl ester groups

Wax

The wax present in the primary cell wall of cotton protects the fibre from environmental
agencies, is responsible for the smooth handle and is a source of hydrophobicity. In the
presence of wax, cotton has poor wettability. The wax consists of long chains of fatty
alcohols, fatty acids,

3
Mineral Matter

Mineral matter (Ash) consists mainly of alkaline earth compounds and potassium and
phosphate ions. The mineral matter may be water soluble or may be removed by treatment
with dilute mineral acids (demineralization/souring). Composition of mineral matter on a
fibre depends on soil composition. The quantity and composition of water-soluble mineral
matters vary according to the nature of soil on which cotton is cultivated.

Coloring Matter

The natural yellowish or brownish color of cotton is due to the presence of proteins and some
flavone pigments. The structure of these pigments is given in Figure 1.7

1.4 Wool: a protein fibre

1.4.1 Impurities in wool

Wool is a protein fibre. On the basis of fineness and fibre length, wool is classified as fine,
medium or coarse. With increasing fineness, the impurity content of wool also increases. The
level of impurities in different wool types is given in table 1.3.

Table. Impurity (in %) level in different wool types

Type Fat and Sand and Vegetable wool

suint dirt matter
Fine 20-25 5-40 0.5-2 20-50

Medium 15-30 5-20 1.5 40-60

Coarse 5-15 5-10 0.2 60-80

As is clear from the above Table, finer wool tend to have a higher proportion of impurities as
compared to coarser wool.

Type of impurities:

Wool wax (Fat) – It is easily saponifiable and emulsifiable hydrophobic impurity.

It consists of Esters, Diesters and Hydroxy esters of high molecular weight Lanolin alcohol
and acids

Suint - It is the perspiration of sheep and is generally water soluble.

4
Sand and dirt - Particulate type of impurity which sheep picks up during its movement.

Vegetable matter - Parts of dried leaves and sticky seeds of certain plants. These are
primarily cellulosic in nature.

1.5 Silk

Silk is a minor fibre in terms of volume produced (~1% of world fibre production) but is a
high value fibre. Composition of a typical silk fibre is given in Table 1.4.

Table. Composition of typical silk fibre

Component %
Fibroin 70-80
Sericin 20-30
Waxy matter 0.4-0.8
Inorganic matter 1.2-1.6
Pigment 0.7

Silk is composed of two proteins namely fibroin and sericin, while the former forms the
actual silk fibre, the latter is largely an impurity which is removed during degumming. Since
both fibroin and sericin are proteins, some of the approaches for removal of sericin may
result in some damage to silk (fibroin) also.

1.6 Added/acquired impurities.

• Mainly sizing matter (protective coating for warp yarns)

• Machine oils, lubricants, grease, etc

• Coning oil (In knitting)

The size material, applied on the warp yarns for facilitating weaving process, may be natural,
synthetic or a modified/substituted natural product or even a blend of all these. Hence the size
removal process becomes specific to a size depending on its chemistry.

In many cases the oils and lubricants are specially formulated to be self emulsifiable and
hence are easy to remove.

1.7 Process sequence in pretreatment processing

The general process sequence followed in pretreatment processing for cotton is:

5
Singeing …..> De-sizing ………> Scouring ……..> Bleaching ………> OBA
Treatment …….> Mercerisation

EXERCISE 1

Part I: Discuss the following in detail

1. What is the importance of pretreatments of textiles in wet processing?

2. What are the different impurities present in raw cotton?
3. Give the general sequence of textile pretreatments in wet processing.
4. What are the different impurities present in silk?
5. Which is the main component of wool fibre?

Part II: Fill the blanks with the appropriate choice given below
1. ……… is one of the pre-treatment processes of cotton wet processing
a. Spinning b. Sizing c. Scouring d. Carding
2. What happens in pre-treatment?
a. Fabric weight increase b. Fabric weight decreases
c. Fabric weight remains unchanged d. Fabric length increases

3. …….. is the hydrophobic impurity present in raw cotton

a. Protein b. Wax c. Minerals d. None

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 Chapter Two

SINGEING

2.1 Singeing

The main purpose of singeing is to remove floating fibers from both sides of the fabric to get
the clean appearance of the fabric.

The protruding fibres;

1. Create a fuzz which might obscure sharpness of a print or a coloured strip on the
garment
2. Can attract soil
3. May aggravate pilling

Many cotton materials are valued for their smooth appearance e.g. lustrous sateen and satin
weaves. Hence, in general, it is desirable to remove these surface fibres. One of the most
common methods to do this is just burn off these fibres. This is known as Singeing. Although
now a days it is also done using enzymes for cellulosic fibre fabrics. In the figure below, it is
easy to see the difference between the fabric surfaces with and without pills.

Fabric surface with pills clean surface

(Before Singeing) (After Singeing)

Figure. Fabric surface with and without pills

Objective of singeing - To burn off the protruding or raised fibers from a yarn or fabric
surface.

Advantages-
1) Improved end use and wearing properties.
2) Clean surface.
3) Reduced fogginess.

7
4) Reduced pilling.
5) Reduced soiling.
Singeing usually involves passing/exposing one or both sides of a fabric over a gas flame to
burn off the protruding fibers. And the temperature of the flame is quite high, hence the
fabric is passed over the flame at a high speed such that loose protruding fibres are burnt off
but the fabric itself remains undamaged.

Heat or the temperature is therefore a key parameter in singeing.

Other methods of singeing include infra-red singeing and heat singeing for thermoplastic
fibers.

Singeing of yarns is called “gassing”.

Cellulosic fibers such as cotton are easily singed because the protruding fibers burn to a light
trace ash which is easily removed.

Thermoplastic fibres are harder to singe because they melt and form hard residues on the
fabric surface.

2.2 Types of singeing

2.2.1 Plate singeing machine

Plate singeing machine consists of 1-2 inch thick copper plates which are heated from below
by burning heavy petroleum oil. The plates are heated to a bright red color and the fabric
passes over the plates at speeds up to 200 yards per minute. A special traversing arrangement
is provided to prevent local cooling which may occur due to constant passage of cloth over it.
The singed cloth is then run through water to extinguish the sparks if any.

8
2.2.2 Rotary cylinder machine

The problem of local cooling in plate singeing is overcome here. The disadvantage of plate
and roller singeing is the fibres present in the interstices of fabric are not burnt out. Cloth
passes over a hollow cylinder. It rotates slowly in a direction opposite to that of fabric

Figure. Rotary cylinder singeing machine

2.2.3 Gas Singeing

This is popular method of singeing in industry. In gas singeing, a suitable mixture of gas and
air under pressure is used as the heat source. This mixture is fed into a slot burner where it
undergoes combustion. Coal gas, petrol gas or butane gas may be used as the fuel.

The width of the burner can be adjusted to suit different fabric widths. The flame height
and consequently the heat intensity can be varied for different fabrics by altering the
pressure of the mixture or the ratio of gas and air in mixture.

Upon combustion the temperature of the flame may reach 1300oC.

It is important to preheat the cloth to reduce its moisture content before singeing, as a dry
cloth performs better than a cold fabric. The heat energy may convert the moisture in fabric
to steam which can hinder singeing.

Immediately after singeing, the cloth may be quenched in an aqueous bath to prevent a
potential fire. Today, gas singeing is the most prevalent singeing system in the textile
industry.

9
 Figure Typical gas singeing arrangement

2.3 Singeing Parameters

In gas singeing, the protruding fibres are generally burned off in a gas flame. The gas is
passed through a slot burner which is longer than the fabric width. A series of nozzles are
present on the burner. When the burner is started, it creates a uniform flame along its entire
length. Since the type of fibre in a fabric and its construction have significant influence on
the burning behavior of fibres, singeing parameters needs to be adjusted very carefully. In
fact, every time the fibre type or fabric construction changes, singeing parameters need to be
changed and may require some fine tuning as well.

Following are the parameters which need to be considered during singeing a fabric:

Fabric Speed
Burner Angle
Flame Intensity
Flame Colour
Burner Position
Flame Distance from Fabric Surface

2.4 Fabric singeing

Given below is the image (Figure 2.6) of a typical gas burner used for singing of textile
fabrics.

Figure. A gas burner used for singing of textile materials

In the sequence of two figures below, one can see the appearance of fabrics before and after
singeing. The clean fabric surface after singeing is clearly noticeable.

10
 Figure. Appearance of fabric after singeing

Since the loose fibres are present on both the surfaces of fabrics, one needs to expose both the
surfaces to the action of flame. In the schematic below, one can see the arrangement of
burners.

Figure. Principle of gas singeing machine

Singeing is more effective if the loose fibres embedded in the fabric structure can be loosened
and brought on fabric surface. To achieve this, many manufacturers today pass the fabric to
be singed through beating and brushing devices. The combined action of beating and
brushing loosens the fibres and results in more effective singeing subsequently.

2.5 Problems in Gas Singing

The singeing of fabrics is carried out in open width form. If for any reason, singeing is non
uniform, it may create problems in downstream processes like dyeing. Non uniformity may
arise due to uneven flame, which may result from blockage of some nozzles. Any crease
formed may run along the warp and result in non-uniform treatment. Some of the sizes may
be particularly sensitive to high flame temperature. And if the machine were to stop
suddenly, there should be some mechanism to put off the flame with the least delay as it may
result in localized heating.

The following problems may arise

1) Uneven singeing - can lead to dyeing Streak

2) Thermal Damage – due to high flame temperature

11
3) Stop Offs – whenever the machine stops, excessive localized heating may result in
Heat Bars
4) Creasing – Dyeing Streaks
5) Size Hardening – Difficulty in size removal
6) Sublimation of dye from dyed polyester fabric during singeing

2.6 Yarn singeing

Textile yarns are singed for applications like sewing thread, where the resistance caused by
protruding fibres during high speed sewing needs to be lowered. The high friction may lead
to a lot of frictional heat generation, leading to damage to fabric and frequent yarn breakage.
For yarn singeing, individual yarns are passed over gas flame to burn of the loose protruding
fibres.

Given below is the image of a singed yarn (right) and yarn before singeing (left).

Figure. A hairy and a singed yarn

The yarn singeing machines typically comprise of a let off and take up system, where the
yarn package to be singed is placed at the bottom of the machine. It is then threaded upwards
through guide rollers in a take up package placed at the top of the machine. The singeing
takes place at a single burner placed in the middle of the machine. When the operation starts,
a pneumatic arm places the yarn in the centre of the burner which generally has a circular
shape. A mixture of a flammable gas and air is supplied to each burner.

2.7 Assessment of singeing efficiency

Singeing efficiency is evaluated by different techniques as follows;

Visual observation or feel of fabric.
Dyeing test
Pilling testing

12
EXCERSIZE 2

Part II: Discuss the following questions in detail

1. What is singeing of textiles?

2. Describe the importance of singeing?

3. What are the different types of singeing methods?

4. Which is the most popular singeing method in textile industry?

5. How singeing efficiency can be measured?

6. Give the advantages of gas singeing method.

7. Where the yarn singeing is preferred?

8. What are the different parameters to be controlled during gas singeing?

9. What are the problems in singeing, if the process is not controlled properly?

10. Why quenching is done after singeing?

Part II: Fill the blanks with the appropriate choice given below
1. …………. is the process of removing protruding fibres from the yarn.
a. Scoring b. Singeing c. Pilling d. Oxidising
2. Removal of free fiber ends from fabric surface by burning method is __________.
a. Cleaning b. Finishing c. Singeing d. Shearing
3. Singeing done in fabrics for —————
a. Cleaning of fabrics b. Thinning of fabrics c. Removing hairy fibers
from fabrics d. Setting of dimension in fabrics
4. …….. singeing of cotton removes protruding fibres from both the sides of fabric.
a. Gas b. Plate c. Roller d. None of these
5. ……. …. is one of the parameters controlled in gas singeing.
a. Number of gas burners b. Type of gas c. Angle of gas burner
d. Number of nozzles

13
 Chapter Three

DE-SIZING

Desizing is the process of removal of size material applied on warp threads during weaving
(sizing) in order to facilitate the downstream chemical processes.

Removal of impurities

In general, the impurities from textile substrates can be removed by following processes:

Solubilization

Emulsification or

chemical breakdown by hydrolysis/oxidation.

In case the size is not soluble, it is removed by either hydrolysis or oxidation. Hydrolysis or
oxidation results in lowering of molecular weight of starch, which results in improved
solubility of degraded starch. Following parameters play an important part in determining the
efficiency of any desizing.

The important process control parameters in desizing are.

Temperature
pH
Time
Circulation
M:L ratio
Concentration of desizing agent

3.1 Mechanism of desizing

Starch consists of both amylose and branched amylopectin which is poly-α-glucopyranose.

The glucose units in both are linked at 1-4 positions. In case of amylopectin, certain linkages
also occur at 1-6 positions (~4%). When the 1-4 linkage is attacked and broken by hydrolysis,
the desizing is called hydrolytic desizing. Initial starch degradation product is insoluble
dextrin, which on further hydrolysis is converted to soluble dextrin and finally glucose.

14
3.2 Hydrolytic Desizing

Rot steeping:

• Steeping in water followed by batching for 16-24 hours, when starch swells
• Swollen starch is attacked by enzymes secreted by microorganisms in environment.
• Hydrolyzed starch is removed by normal washing.
• Low capital investment
• Slow process, incomplete size removal and low reproducibility are the disadvantages
of this process.
• Rot steeping has become obsolete because of poor process control and slowness of the
process.
Acid desizing:

The 1-4 linkage can be broken by acid hydrolysis also. mineral acids, like sulphuric acid or
hydrochloric acid is used.

• H2SO4/HCl- (5-10 g/l) is needed at 40oC for 3-4 hours.

• Above 40oC & 10 g/l acid concentration, degradation of cotton cellulose itself may
occur.
• The fabric is padded with acid solution and stored in pits or batched for 6-8 hours.
• Action of acid will result in gradual degradation of starch. But not all starch is
degraded to the extent where it all becomes water soluble.
• Desizing should always be followed by thorough cold wash to remove residual acid and
hot water washing to remove maximum amount of starch.

Precaution- Local drying during storage should be avoided. Local drying may result in
high concentrations of acid at localized places which can cause cellulose degradation.

3.3 Enzymatic desizing:

Enzymatic desizing is popular in industry and it is carried out using enzymes like, amylase.

Enzymes are:

• Organic biocatalyst,
• Physically---- colloidal in nature
• High molecular weight proteins (3-D)
• Highly specific in action and work under specific conditions of temperature and pH.

15
• Lose activity gradually with time.
• Generally, act under mild conditions
• Have to be cultivated and nurtured like crops (from fungi)
• Genetic engineering allows enzymes to be designed for specific processes
3.3.1 Enzyme Sources for Desizing:

Vegetable, bacterial, Animal

(Diastase, Rapidase, Amylase etc.)

Developments:

1900 --- Malt Diastafor, by Diamalt Co. of Munich, Germany for

commercial Desizing (Malt extract -
Vegetable)

1912 --- Enzymes from slaughterhouse waste

(Pancreatic - Animal)

1919 --- From bacterial sources (Bacterial -

Bacteria)

Malt Amylase has two components:

α & β- Amylase (Ratio 1:5 to 1:6)

α- Amylase attacks the chain at random

β -Amylase attacks the chain end & produces maltose

Figure. Schematic of amylase

Since enzymes act optimally at specific conditions of temperature and pH, it is

important to maintain narrow range of conditions for best results. Figure below show
effect of pH and temperature on enzyme activity.

16
 Figure. Effect pH and temperature on enzyme stability

Out of the three types of amylases, bacterial amylases are the most stable. This can be

confirmed from the figure below which shows decay in their activity with time at 60 oC

Figure. Thermal stability of various amylases

Sodium and Potassium chloride (0.2-1%) improve the activity of pancreatic enzyme. Ca++
improves the thermal stability of malt amylase. However, sequestering agents and heavy
metal ions like copper, iron, etc. inhibit their activity.

The optimum process conditions for various enzymes vary. The Table given below compares
the best process conditions for these enzymes.

Table. Optimum process conditions for enzymes from different sources

Process Concentration Time Temperature pH

(g/l) (hr.) (OC)
Rot Steeping - 10-16 30-40 ~7
H2SO4 5-10 3-4 40 <1
Malt Diastase 3-20 2-3 50-60 4.5-5.5
Pancreative 1-3 2-3 50-60 6.8-7.5
Diastase

Bacterial 0.5-1 2-3 60-70 6.5-7.5

Diastase

Since grey cotton has poor absorbency, surfactants can be used to improve the wetting of
fabric and dispersion of hydrophobic impurities. In general, anionic surfactants inhibit
enzyme action. Non-ionic surfactants are generally preferred.

Although traditionally enzymes are used under mild process conditions, genetic
engineering has allowed development of robust enzymes which can be used at higher
temperatures to increase the rate of desizing.

17
3.3.2 High temperature enzymatic desizing

Novozymes, an enzyme producing major, introduced an alkaline amylase with a broad

activity spectrum, capable of application over the pH range 5-10 and from 20-85°C. This
has enabled combined desizing and bioscouring to achieve commercial acceptance in a
number of textile industry. They have also developed enzymes for use in high temperature.
The details are given below:

Aquazym® PS (Novozymes)

Heat-stable alpha-amylase used in high-temperature continuous desizing processes (Pad

Steam).

Aquazym® SD (Novozymes)

It is a flexible amylase that works well at broader pH and temperature ranges than
conventional amylases

Table. Optimum process conditions for high temperature stable amylase enzymes

Enzyme product Temp. (°C) pH Continuous Pad-roll Jet, jig, winch

Aquazym® PS 85-115 5.5-6.5 +++ NR +/-

Aquazym® SD 20-85 5.5-6.5 +++ NR +/-

3.4 Oxidative Desizing

In oxidative desizing, the size is removed by oxidative degradation. It is particularly

useful when the size is based either on a synthetic polymer like PVA (poly vinyl alcohol)
or is a mixture of synthetic and natural polymers. Hydrolytic desizing is successful in
case of natural starch but is does not remove sizes based on synthetic polymers.

Following oxidative agents are used in oxidative desizing:

Hydrogen peroxide (H2O2)

Sodium bromite (NaBrO2)
Sodium and potassium persulphate (Na2S2O8, K2S2O8)
Sodium chlorite (NaClO2)
Peroxy monosulphuric acid (H2SO5)

18
 It can be seen that H2O2 action proceeds by attacking the hydroxyl group in PVA, which
it oxidizes to carbonyl group. Chain scission happens near groups involved in oxidation.
This continues and chain scission proceeds leading to small fragments of PVA chain
which have higher water solubility.

The mechanism of starch oxidation is given in Figure below.

(a) Oxidation of starch – ring opening (b) Oxidation of starch- chain

scission

Figure. Oxidative degradation of starch, mechanism

One can see in the figures above that in (a) oxidation does not lead to chain breakage or loss
in degree of polymerization (DP). This means solubility of the starch does not increase.

In general, the first stage of oxidative desizing of starch results in formation of aldehyde and
carboxylic groups from hydroxyl groups present in glucose. This makes the bridging–O–
linkage susceptible to alkaline scission. Hence an alkaline loss following treatment with
oxidizing agents results in efficient removal of starch.

With sodium chlorite, the desizing is carried out under alkaline conditions. Sodium bromite is
a powerful oxidant for starch. It breaks glucose ring by breaking C2-C3 link and produces a
di- aldehyde. This di-aldehyde dissolves in alkaline solution hence desizing is followed by an
alkaline wash. It acts best at pH 10. It works at room temperature for short duration and is
highly efficient. However, 50% of the bromite reacts with impurities and increases the AOX
problem of the effluent. With persulphates, desizing is carried out in alkaline medium. Since

19
peroxy compounds are sensitive to presence of heavy metal ions, a sequestering agent is
usually employed.

Hydrogen peroxide may be used in a similar way. Conditions are generally kept mild (pH-6-
8) and washing is done in alkaline conditions. Some recipes for desizing with peroxy
compounds are given below.

Table. Typical recipe for oxidative desizing

Parameters Value
Potassium persulphate or H2O2 (% owf) 0.5
Mg sulphate % owf 0.005
Caustic soda % owf 2
Sodium Silicate % owf 1
EDTA (sequestering agent) % owf 0.2
Temperature oC 100
Time min. 60
M L R (material to liquor ratio) 1:40

3.5 Assessment of desizing efficiency

Industrially, the assessment of desizing process efficiency is done by rating the process
on a TEGEWA violet scale. TEGEWA agent is basically a diluted solution of iodine in
water and alcohol. When this solution is applied on a desized fabric, the iodine in
solution reacts with residual starch in the fabric and forms starch iodide. This is blue in
color and the intensity of color indicates amount of residual starch on fabric.

The lesser the intensity of color, the higher the starch removal and higher the TEGEWA
rating of the fabric.

3.5.1 Reagent preparation

Put potassium iodide [10 g of KI (100%)] in 100 ml of water; then add 0.6358 g of iodine
(100%); stir well until iodine is completely dissolved in the KI solution. After this, add 800
ml of ethanol. Then by adding water the volume should be raised to 1000 ml.

20
3.5.2Method of testing

Put one or two drops of the above solution on a fabric. Rub it gently and then assess the
colour change as per the Tegewa scale. Before testing, the fabric should be cold and there
should not be any residual alkalinity in it.

Assessment

No Colour Change = No starch is present

Pale blue to bluish violet = Presence of starch size or a blend of starch+ synthetic size

Brown = Presence of modified starch or a blend of starch/PVA size

Figure. TEGEWA violet scale (1-9 from left to right)

Complete removal of starch will not result in any color formation (rating – 9) and poor starch
removal can give intense blue color (rating – 1).

EXCERSIZE 3

Part II: Discuss the following questions in detail

1. Give the importance of desizing?

2. What are the different types of desizing methods?
3. Which is the most safer desizing method?
4. What are the disadvantages of acid desizing method?
5. How it could be possible to remove sizing materials from fabric during desizing
process with water only? Justify the answer with appropriate reasons.
6. How desizing efficiency is measured?
7. Give the advantages of enzymatic desizing method.
8. What is Tegawa scale? Where it is used?
9. What are the different parameters to be controlled during enzymatic
desizing?
10. What are the disadvantages of enzymatic desizing?
11. What are enzymes?

21
 12. How starch size is removed in desizing?
Fill the blanks with the appropriate choice given below
1. Desizing is ……….. process
a. Dyeing b. after-treatment c. pre-treatment d. printing
2. The process of removing the starch from the fabric is called ——————-
a. Bleaching b. Mercerizing c. Desizing d. none
3. The substance removed during degumming is ——————-.
a. Sericin b. Fibroin c. Natural coloring matters d. Wool wax
4. ………. desizing process removes size without using any chemical compounds
a. Enzymatic b. Acid c. Rot steeping d. oxidative
5. pH of ………. is maintained during enzymatic desizing.
a. 3-4 b. 10-12 c. 6-7 d. Neutral
6. ………. Acid is used in acid desizing process to remove size.
a. Acetic acid b. Sulphuric acid c. Formic acid d. Nitric acid

22
 Chapter Four

SCOURING

4.1 Basic surfactant concepts

Surfactants are organic molecules which have amphiphilic nature. They have a hydrophobic
portion (generally a long fatty chain) and a hydrophilic head (an anion or action and
sometimes an ethylene oxide chain). Due to its dual nature a surfactant tries to occupy space
in the boundary of a hydrophilic and hydrophobic medium.

Given below is one schematic of surfactant molecules. One can see that hydrophobic tail is
compatible with a hydrophobic medium while the head is compatible with a hydrophobic
medium. So when put in the mixture of two immiscible liquids, such as oil & water, the
surfactant tries to concentrate at the interface i.e., the boundary of the two.

Figure. Schematic of various surfactant molecules

In the figure above, the left hand side shows hydrophilic heads of surfactant molecules
(nonionic, anionic, cationic and zwitter ionic) while the right hand side is a hydrophobic tail
(hydrocarbon).

Example- Desized cotton fabric is hydrophobic & repels water. If one tries to scour it with a
caustic solution, the wetting is not good. Unless the scouring liquor wets the fabric properly,
scouring will not be efficient. However if a wetting agent is added to the scouring liquor, it is
able to wet the fabric. There is interaction between the alkali & the impurities & scouring is
efficient.

23
4.1.1 Why surface tension of a solution goes down in presence of a
surfactant?

Consider water in a container. A water molecule in the bulk is pulled by molecules from all
direction & hence the resultant pulls on it may be negligible (Figure). However, the
molecules on the surface are pulled only by molecules below them. Hence water molecules at
the surface experience a net pull from molecules directly below them. This causes the surface
to act like a tense surface & lies at the root of surface tension phenomenon. Now when a
surfactant is added to the water, the surfactant molecule invariably goes to the air water
interface replacing the water molecules. This reduces the net pull on top layer of the water
molecules & hence surface tension of water goes down.

The reduction in surface tension is directly proportional to surfactant concentration in water.

Surface tension keeps decreasing with increasing surfactant concentration till the surface
saturates. Above the saturation point, surfactant molecules start aggregating (i.e. micelle
formation). The surfactant concentration at which it forms micelles is known as Critical
Micelle Concentration (CMC). Above CMC surface tension becomes constant as there is no
further increase in concentration of surfactant at the interface.

4.1.2 Surfactant Aggregation in Solution

As has already been discussed, the surfactant has a tendency to concentrate at the interface. If
surfactant is dissolved in water, its molecule tends to come to air water interface in such a
way that hydrophobic fatty chain is oriented outwards in the air (1), while the hydrophilic
head remains submerged in water. As more surfactant is added in water, it keeps moving to
the surface

HLB Value Concept (For surfactants and oils/fats/waxes etc.)

24
HLB stands for hydrophilic lipophilic balance. It indicates relative fraction of hydrophilic and
hydrophobic components in a surfactant. The nature of surfactants with different HLB values
are shown in following Table:

Table. Use of surfactant with different HLB values

HLB value of surfactant Applications

Less than 3 Surface films
3-6 Water -in-oil emulsifier
7-9 Wetting agent
8-15 Oil-in-water emulsifier
13-15 detergents
15-18 solubilizers

Contact angle (θ) - It is the angle between solid surface and the tangent to the liquid surface
drawn at point of contact of liquid with solid. It is denoted by θ. It is different at interfaces of
different pairs of liquids and solids. The value of θ determines whether a liquid will spread on
the surface of a solid or it will form droplets on it. As shown in Figure (Figure 3.8b), addition
of wetting agent in water (liquid) decreases angle of contact. The decrease in contact angle
reduces surface tension of liquid results in improving wetting properties.

4.2 Scouring Process

Scouring is an important pretreatment stage, especially for natural fibres which tend to have a
significance presence of natural impurities. In case of cotton, although the relative amount of
impurities is quite low, it still makes the fibre non absorbent. In case of wool, the amount
may be so high as to interfere with basic yarn manufacturing operations and hence the
scouring may have to be done at fibre stage itself. In case of silk, presence of natural
impurities tends to mask its natural luster for which it is valued.

The objective

To reduce the amount of impurities sufficiently to obtain level results in dyeing and
finishing operations by bringing the substrate to a highly absorbent state.

Hence the emphasis is on removal of hydrophobic impurities.

25
 Impurities in cotton

Table. Naturally occurring impurities in cotton

Waxes 0.4-1%
Nitrogenous Matter (Proteins) 1-2.8%
Pectic Matter 0.4-1%
Minerals 1-1.8%
Motes (seed coat fragments) --
Natural Coloring Matter Variable
Added Lubricants/Knitting oils,
grease stains

It is the wax present in the outermost layer of cotton fibres which turns it nonabsorbent in its
natural state. Although the amount of wax present on a fibre is low (0.4- 1%), it is not easy
to remove.

There are basically three scouring systems for cotton:

1. Conventional system

Most widely used system. It consists of an alkali and a combination of surfactants.

Alkali Surfactant Emulsifiers

NaOH Wetting Agents Non-ionic surfactants

Both wetting agents and emulsifiers are surfactants but they perform different roles as per
their HLB values. This system removes almost all the impurities except motes. It is a high
temperature, high alkalinity, and chemical and energy intensive process.

2. Solvent based
Two types of solvents may be used
Chlorine Based Tetrachloroethylene, Trichloroethylene

Hydrocarbon Benzene, White Spirit

Solvent based systems rely on their solvating power to remove wax by dissolving it. This
system removes only hydrophobic impurities and not others. It is a low temperature, low
energy process. It is not eco-friendly and hence, its use is limited.

26
3. Enzyme based: There have been attempts to remove impurities from cotton by use of
enzymes. It uses mild temperature and pH.

Conventional system

The agents used are:

Alkali – Mainly sodium hydroxide (NaOH), sometimes mix of NaOH and Na2CO3 (washing
soda)

Wetting agent - To reduce the surface tension of scouring liquor so as to wet out the goods
quickly and uniformly, generally anionic surfactants are used

Emulsifier – To emulsify non safonifiable wax. Generally, nonionic surfactants are used.

In this system, the combination of alkali and surfactants acts on various impurities in the
following manner:

1. Saponifiable oils are converted to soaps by the action of alkali.

2. Proteins – Hydrolyzed to soluble degradation products by alkali.
3. Simple amino compound – hydrolyzed to ammonia by alkali.
4. Pectose & pectins are converted into soluble salts of pectic/ metapectic acid by alkali.
5. Mineral Matter – either dissolves in water or removed by souring or sequestering
agents.
6. Unsaponifiable oils & waxes – Emulsified by emulsifying agent.
7. Modern mineral oil formulations usually contain self-emulsified system which can be
removed easily with water.
8. Motes - Cellulose of low crystallinity swell in alkali & became sodium cellulosate
which is water soluble. Residual motes are destroyed in bleaching.

While alkali removes majority of the impurities like, pectins and proteins, the fibre does
not become absorbent until the wax is removed significantly. Hence removal of waxes is
important for providing absorbency to fabric.

Saponification

• Wax, fats, oils & lubricants are present mostly as esters in the form of triglycerides.
• The triglycerides form glycerin and soap when reacted with NaOH (alkali).

27
 Reaction:

Triglyeride + Alkali ----> Glycerine + Soap (sodium salt of fatty acid)

Hence fat/oil forms glycerol (miscible in water) and soap (RCOONa). Soap is soluble in
water and acts as a surfactant to reduce the surface tension of scouring liquor. However, since
the amount of saponifiable matter present in cotton may be very low (< 0.5%) one has do
make additions of wetting agents in the liquor.

Conventional scouring based on caustic soda process

Old processes were designed for almost complete removal of wax by prolonged boiling of
cotton in alkaline solution at 130oC.

Chemicals used-

NaOH – 4% (owf) for normal fabric. 5-6% (owf) for heavier fabric.

Wetting Agent – 1 – 3 g/l.

Emulsifying agent – non-ionic surfactant (1-3 g/l)

Solvent systems

Developed in 1970s in Europe to deal with scarcity of water.

Given up towards the end of 70s. (Not all processes could be done with solvents.)
Examples:
Perchloro ethylene – (B.P. – 121oC, Non-flammable)
Trichloro ethylene – (B.P. – 87oC, Non-flammable)
The economy of the process depends on the recovery of solvent.
Use of neat solvent to remove the wax was not attractive due to very low amount of wax
present in the fabric.
Hence solvent assisted scouring was developed.

28
Advantages of solvent scouring

✓ Good solvents for cotton wax are available

✓ Removal of wax at room temperature

✓ Due to low specific heat and much lower heat of evaporation than water, removal of
solvent from fabric was economically much more favorable.

✓ Chlorinated solvents are non-flammable

The system had following components:

Solvent (PERC)

Wetting agent

Emulsifier

These all mixed to form a transparent mixture if they all have same HLB values.

HLB Value – 13- 13.5 for all the components.

Of the above mixture, 4% concentration for scouring was sufficient. Moreover, the recipe
was pH independent hence it could be combined with either desizing or bleaching..5
Enzymatic scouring

The term enzyme is derived from the Greek word enzymes, which means ‘in the cell or
ferments’. The molecular weight of these ferments is very high and is the order of 10 4-105.
From the chemical standpoint, an enzyme is defined as a protein complex composed of about
200 to 250 amino acids. Enzymes are very large, complex, protein molecules consisting of
inter-twined chains of amino acids formed within the cell of all living creatures-plants, fungi,
bacteria and other single cell organisms.

They are also known as biocatalysts as they are responsible for most life-generating
reactions. They promote hydrolysis of impurities to form low molecular weight, soluble
fragment of impurities. They can greatly enhance the rates of biological reactions even at
comparatively milder conditions. Being catalysts, they are actually not consumed in the
reaction but gradually lose their activity. The most important characteristic of the enzymes is
their specificity. They act upon a very specific substrate, under narrow range of conditions of
temperature, pH and agitation. Fluctuations from these conditions can cause the enzymes to
change their shape and lose the activity.

29
The nomenclature of the enzymes is based on the substrate on which they act. Hence Lipase
splits fats into glycerols and fatty acids, Catalase breaks down hydrogen peroxide, amylase
breaks down starch into simple sugar, proteases break down proteins, cellulases breaks down
cellulose & pectinases breaks down pectin.

There are several important factors which determine the effectiveness of enzymes for
scouring. These are the structure of cotton fibre, distribution of impurities in the fibre, type of
enzyme used, combination of components or a specific component, activity of the enzyme,
presence and type of surfactant and agitation. In view of this, the nature of the distribution of
natural impurities on the outermost layer of the cotton fibre assumes importance.

Till date the exact nature of the distribution of the impurities in the primary cell wall is not
known. But a general idea exists according to which waxes and other impurities exist in a
dispersed form in the matrix of pectin and protein matter, pectin acting as biological glue
binding the non-cellulosic matter in the primary cell wall.

Pectinases penetrate the cotton cuticle through cracks or micro pores and make contact with
the pectic substances in the cuticular layer of impurities.

Pectic substances are hydrolyzed with the aid of pectinases which result in the complete or
partial removal of the cuticle or the breakdown of the continuity of the cuticle

As a result of the hydrolysis of the pectin, the link between the cuticle and the cellulose body
breaks, leaving fibre in an absorbent form

4.3 Machinery for Scouring

Conventionally the following machines have been used for scouring.

(a) Kier (batch system)

i) Open kier - In this method, the heat sensitive textile material is scouring at boiling or low
temperature.

ii) Pressure kier

Kier is closed vessel in which the desized fabric is loaded and heated at high temperatures for
prolonged time. It results in very good removal of oils, fats, wax and other impurities and
fabric becomes highly absorbent.

30
 Figure. Pressure Kier

Table. Optimum conditions for scouring in a kier

31
(b) J-BOX (continuous system)

This machine is called J-Box machine because the scouring vessel looks like the English
letter ‘J’. It is a continuous system in which the fabric is fed from one end and the scoured
fabric from the out end comes out. The capacity is such that sufficient residence time is
allowed inside the machine for degradation and removal of impurities. The J-box is rarely
used in the industry now. De-sizing, scoring, and bleaching can be performed at once in this
system. The Continuous Souring process can be separated into four parts of J-Box:
Saturation, Pre-heater, J-Box and Washing unit.
Inside temperature – 100oC
Saturation of fabric with recipe before treatment in the J-Box.
Time 40 – 60 min.

Figure. J Box
Vapor loc System (continuous)

This is again a continuous system, but it is possible to maintain pressure inside the system.

This allows shorter treatment times at higher processing speeds.

Saturation of fabric with NaOH and wetting agent

Pressure inside the chamber – 30 lb/in2
Temperature – 134oC
Time – 90 – 120 sec.
(c) Bio scouring

It is a simple, repeat able and safe process. The removal of pectin components from cotton
adequately improves the water absorbencies of the fibers and facilitates the penetration of the
dye and other ingredients into the fiber. Natural qualities of the cotton fiber are preserved.
These are just a few submissions of Biotechnology; however, much such potential are yet to
be explored. Enzymes are not only beneficial from ecological point of view but they are also

32
saving lot of change by reducing water and energy consumption which ultimately reduce the
cost of production.

4.4 Assessment of scouring efficiency

During Scouring, the physical behavior of cotton undergoes some changes mainly due to the
loss of organic natural impurities which are mainly concentrated in the cuticle of cotton fibre.
However, the main desirable attribute of scoured cotton is significant increase in water
absorbency compared to raw cotton. Hence assessment of cotton scouring efficiency mainly
focuses on measurement of its absorbency. Some of the changes that take place on scouring
are listed below:

Main changes:
Loss in weight (5-10%)
Significant increase in absorbency (1-3 seconds)
Improvement is TEGEWA rating
Slight increase in average DP (due to removal of low mol. wt. components)
Shrinkage
Assessment of scouring efficiency
1. Practical tests of absorbency
2. Measurements of
(a) Weight loss
(b) Protein content
(c) Residual wax content
(d) Methylene blue absorption (removal of pectic substances)

Practical tests of absorbency

AATCC Test Method 79, Absorbency of Textiles

In this test water drops are allowed to fall by gravity from a burette placed at a certain height
(9.5 cm) from the fabric surface. The fabric is placed flat in an embroidery hoop without any
creases. The time required for the drops to be absorbed completely is noted as wetting time
(Figure 3).

AATCC/ASTM Test Method TS-018

It is a similar test except that the fabric is supported over a beaker and a water drop is
allowed to fall from a height of 1 cm (Figure 3.15).

33
 Figure. Setup for a) AATCC Test Method 79 and b) AATCC/ASTM Test Method TS-018

Degradation of Cotton during Scouring

Although cotton is stable in dilute alkalies at high temperatures in absence of air, presence of
air may cause serious degradation. The degradation may be assessed by determining one or
more of the following:

1. Copper number
2. Carboxyl group content.
3. Cuprammonium fluidity
4. Tensile strength of the cotton material before and after scouring.

1. Copper number

In the process of scouring, some the hydroxyl groups may be oxidized to carbonyl groups.
These carboxyl groups have a reducing nature and are capable of reducing an alkaline
solution of copper sulphate. Reduction of copper sulphate results in formation of insoluble
cuprous oxide which is deposited on the cellulose material. The amount of cuprous oxide
formed is directly related to the amount of reducing groups and is expressed as Copper
Number. Copper Number is defined as grams of cupric copper reduced to cuprous oxide by
100 g of cellulose under standard conditions of boiling in alkaline medium and is calculated
by the following formula
63.5 × 𝑉 × 𝑁
C𝑜𝑝𝑝𝑒𝑟 𝑁𝑢𝑚𝑏𝑒𝑟 =
W
Where V is the ml of ceric solution consumed after deducting blank reading, N is the
normality of ceric sulphate solution and W is the weight of the bone dry cellulose sample
(0.25 g for normal samples and 0.1 g for highly degraded samples having copper number
greater than 4). The method details are given in Annexure 1.
The copper number of pure cellulose ~ 0.05

34
For raw cotton ~ 0.9 due to the presence of impurities
Well-scoured and bleached cotton material > 0.3
For regenerated fibre it should be > 1.2.

2. Cuprammonium fluidity

Degraded cotton has lower degree of polymerization due to chain scission. For a given
concentration, the viscosity of the solution of a polymer in a solvent is directly related to its
degree of polymerization. The fluidity is inversely related to viscosity. Hence a degraded
polymer with lower viscosity will exhibit higher fluidity. In case of cotton, the fluidity is
measured by dissolving it in cuprammonium hydroxide solution. An increase in the fluidity
value indicates degradation.

Unbleached cotton shows a fluidity of about two. A fluidity value of five or less for bleached
cotton is acceptable commercially. A fluidity value of ten or higher, in loss in tensile strength.
Unbleached viscose has a fluidity of about ten.

Physical testing

Tensile strength, bursting strength and abrasion resistance, Tear strength can also be
measured

The results are influenced by both fabric structure and chemical damage.

Tear strength is also influenced by residual natural lubricants.

Staining tests

Carboxyl groups in oxidized cellulose resist staining with C.I. Direct Blue 1 or give increased
uptake of C.I. Basic Blue 9.

Harrison test

The oxycellulose test sample is immersed in a boiling alkaline silver nitrate solution.

Brown to black deposits of silver are produced on the substrate where there are reducing
aldehyde groups. (From Karmakar book).

EXCERSIZE 4

Part I: Discuss the following questions in detail

1. Give the importance of scouring?

2. What are the objectives of scouring process

35
 3. What are the different types of scouring machines?

4. What are the different chemicals/auxiliaries used in scouring bath?

5. What are the disadvantages of kier boiling method of scouring?

6. How scouring efficiency is measured?

7. Give the advantages of continuous scouring method.

8. What do you mean by saponification?

9. What is the role of detergent in scouring of cotton?

10. How wax is removed in scouring of cotton?

11. What are the major changes occurred in scouring of cotton?

12. What is bio-scouring?

13. What is the roe of sodium hydroxide in scouring of cotton?

14. Discuss the problems in scouring of cotton.

15. Give the different parameters to be controlled in scouring of cotton.

16. Elaborate and clarify scouring parameters then comment appropriate figures for
each parameter to cotton scouring.
17. Differentiate between fiber impurity and added impurity.

Part II: Fill the blanks with the appropriate choice given below

1. Why scouring is done for cotton fabrics?

a. For removing starch of fabrics b. For setting dimension of fabrics

c. For increasing strengths of fabrics d. For removing hydrophobic impurities

2. During scouring ………. used to reduce surface tension of water.

a. sodium hydroxide b. sequestering agent c. soap d. wetting agent

3. In scouring the role of emulsifying agent is to

a. remove oils b. remove pectins c. remove dirt d. remove wax

4. In scouring, the safonification reaction removes …….. from cotton fabric.

a. oils b. pectins c. dirt d. wax

5. The ……….. of cotton is improved in scouring.

a. crease recovery b. whiteness c. strength d. Absorbency

36
 Chapter Five

MERCERIZATION

The discovery of mercerization happened accidently when John Mercer was trying to filter a
concentrated caustic lye (NaOH) solution through a cotton fabric. He observed that the fabric
had shrunk after filtering and had become stretchable. Given below is a brief history of
mercerization:

1844 - John Mercer observed the effect.

1850 – Filed a patent for treatment of cotton with conc. NaOH solution with
improvement in strength & and dyeability.
1890 – Horace Lowe; found if shrinkage is controlled, the fabric becomes lustrous.
Tension Mercerization (Lowe) & and Slack Mercerization (Mercer)
Mercerization is carried out for the following purpose.
a) Improving lustre (silky look, in tension mercerization only).
b) Improving tensile strength.
c) Improved dimensional stability.
d) Improving color yield (savings in dyestuff).
e) Improving Elasticity or Stretch of cotton material (in slack mercerization only).
Mercerization is a process of impregnating the textile material with a concentrated solution of
(cold or hot) NaOH, keeping it in contact with the solution for a given time with or without
tension, and subsequently rinsing it.

The effect of mercerization is related to the size of the sodium hydroxide hydrates (NaOH.
xH2O). The concentration of NaOH solution determines the value of x or the size of the
hydrate. A dilute solution has larger sized hydrates, which can cause swelling in cotton fibre
by entering the amorphous phase of the fibre. At higher concentrations, the hydrate volume is
smaller. Such hydrates cause lower swelling but have the ability to penetrate the crystalline
phase and change the crystal structure. Such changes are capable of inducing important
structural modifications in fibre structure.

37
5.1 Structural Modification

5.1.1 Effect of NaOH Concentration

It has been discussed that mercerization leads to conversion of cellulose I to cellulose II.
Native cellulose is Cellulose I and regenerated cellulose (example – viscose) is cellulose II.
However, during mercerization, conversion of cellulose I to cellulose II is only partial. Hence
mercerized cotton is a combination of both crystalline forms. The extent of conversion is
dependent on various process parameters like concentration of NaOH, time of treatment,
temperature and tension employed in the process.

In the figure given below, the effect of NaOH concentration on crystallinity of cotton is given
(time 60 sec, temp 20oC, tension- to maintain length change=0%)

Figure. Effect of alkali concentration of crystallinity of cotton [3]

From the figure it can be inferred that the formation of cellulose II is favoured at higher alkali
concentrations. The overall crystallinity of cotton also goes down on mercerization.

5.1.2 Effect of temperature

Temperature seems to have a similar effect on conversion of cellulose I to cellulose II.

Overall crystallinity also goes down.:

38
5.1.3 Enhancement in luster

Cotton owes its non-lustrous appearance to its non-uniform twisted, convoluted, bean shaped
fire cross section. As there is continuous change in the fibre cross section along its length, it
has poor specular reflection which is responsible for high low lustre. On mercerization, the
fibre swells gradually and the false twist and the convolutions gradually disappear. The cross
section becomes almost circular and the fibre acquires the shape of a regular uniform
cylinder. This process of gradual change in the fibre cross section is depicted in figure below:

Figure. Gradual changes in cross section of cotton fibre on mercerization [3]

In the above Figure, stage 1-5 show swelling of cross section of fibre. It is easy to see
conversion of a bean shaped flat cross section to almost round shape and gradual
disappearance of lumen. Stage 6 and 7 are associated with removal of NaOH from fibre on
washing and drying. The values shown in the figure are relative where 1 corresponds to the
larger of the cross sectional dimension of untreated dry cotton fibre. Upon treatment with
NaOH solution of mercerization strength, it swells and increases in cross sectional dimension
by around 30% (1.3). Removal of

NaOH on washing and subsequent drying results in shrinkage and the diameter of the
mercerized fibre with almost circular cross section is around 0.8. It is important to note that
on loss of sodium hydroxide during washing and subsequent drying, the fibre shrinks in cross
sectional area, but maintains its rounder shape. Overall, there is very little gain in fibre
volume due to mercerization, and hence the density of the fibre remains unaffected.

The rounder, more uniform (convolution-free) and regular cross section results in more
specular reflection which results in higher lustre. However, it must be noted that the process
of removal of convolutions and other surface irregularities (wrinkles and creases) is greatly
aided by tension. Hence tension mercerization always results in more lustrous product as
compared to a slack mercerized one.

The presence of protruding fibre ends on the yarn surface suppresses lustre. Hence cotton
yarns meant to provide high lustre must also be singed in order to maximize lustre.

39
5.2 Mechanical properties

Mercerization has been found to increase the tensile strength of cotton fibres even though a
drop in overall crystallinity is recorded. The main reason for this phenomenon to occur is
swelling of fibres. The presence of many convolutions and false twists in the fibres cause
weak spots to be present. These weak spots act as zones of stress concentrations due to lower
cross sectional area on application of a tensile stress. Swelling, which is an integral part of
mercerization process, removes convolutions and false twists and the fibres acquire a more
uniform cross section along its length. With weak spots gone, the fibres exhibit enhanced
tensile strength as compared to a non-mercerized fibre.

Increase in tensile strength can be summarized as:

Removal of convolutions results in removal of weak spots at the point of reversal

Fibres have more uniform, circular and smoother cross section after mercerization

The fibrils are arranged parallel along the fibre axis

Fibre alignment along fibre axis is better in case of tension mercerization as compared
to slack mercerization

5.2.1 Effect of tension

Mercerization has a significant effect on mechanical properties of cotton. The enhancement in

both tenacity and modulus is higher at higher tension. It is easy to visualize this since it
results in better alignment of molecular chains in fibre axis direction (higher orientation).
However, in case of elongation, it is reverse. With increasing tension, the elongation at break
decreases monotonically. It is to be expected as increasing orientation would lead to lower
elongation. At negative tension though (shrinkage occurring) the breaking elongation is
higher than that of unmercerized cotton.

Hence it can be concluded that if improving the tenacity of cotton yarn is the main objective,
mercerization should be carried out under tension.

5.2.2 Effect of Alkali concentration

The effect of alkali concentration on tenacity, breaking elongation and Young’s modulus of
cotton mercerized with NaOH solution of variable concentration at 20oC for 60 sec at
constant length are plotted in the figure given below. The alkali concentration is varied from
100 to 300 g/l. Again, the elongation and modulus are indicated on secondary vertical axis.

40
5.3 Dyeing Properties

Since mercerization results in change in physical structure of cotton, as manifest in change in

crystal structure, crystallinity and lustre, it affects the dyeing behavior of cotton. The
important changes that cause this are:
Mercerization decreases the crystallinity (increases amorphous content)
Modifies the texture
Overall effect – greater moisture absorption, greater reactivity towards chemical reagents and
dye molecules
Mercerized cotton has higher
Dye absorption ( dye pickup)
Rate of dyeing
Visual colour yield as compared to unmercerized cotton
Improvement is more marked in slack mercerization (lower tension)
Increase in colour yield can allow for a saving of 15-50% in dyestuffs. Indeed many times,
this is one of the reasons for subjecting cotton goods to mercerization.
The effect of mercerization on dye absorption and apparent color yield is shown in the figure
below. The concentration of sodium hydroxide is varied from 150 to 350 g/l.

5.4 Hot mercerization

Although mercerization is an exothermic process and is more efficient at lower temperatures

(typically a temperature range of 15 to 20oC is used), it has following drawbacks:

At lower temperatures, NaOH solution of mercerizing strength has high viscosity and
surface tension.

When a yarn/fabric is mercerized, swelling of fibres at yarn surface due to

mercerization causes compaction of yarn structure.

This results in poor penetration of NaOH solution in the core of yarn

The treatment becomes non-uniform

The basic problem of poor penetration leading to non uniform mercerization can be tackled
by carrying out mercerization with hot (60 to 100oC) NaOH solution of mercerizing strength.
This is known as hot mercerization.

However, since mercerization won’t take place at high temperature, the temperature of the
treated fabric has to be brought down.

41
Therefore, hot mercerization becomes a two stage process, in which the first stage is
treatment of cotton fabric with hot NaOH solution of mercerization strength and the second
stage is the reduction in temperature of the treated fabric to bring about the mercerization.

As the temperature of the fabric is brought down, swelling may start and the fabric may
shrink and hence the dimensions may need to be maintained during cooling stage by desired
applied tension.

Advantages:
Hot NaOH solution has low viscosity and higher penetration power
Swelling of cotton fibres in hot NaOH solution is low, hence more uniform
treatment
Faster process, leading to: higher productivity and compact unit
Period of contact between material and NaOH can be reduced by upto 50%
The fabric can be stretched to greater degree as the fabric becomes more
plastic
More uniform coloration
Better dye uptake (less colour yield)
Can permit elimination of scouring process.

However, under conditions prevailing in hot mercerization, degradation of cellulose at high

temperatures in presence of air can take place.

More uniform treatment, faster process, hence process time can be reduced.
More productivity or more compact unit
Higher stretching is possible; this will result in higher mechanical strength/lustre
Higher stretch is possible if stretching proceeds while cooling.
Uniform dyeability

5.5 Mercerization of blends

Sometimes blends of cotton and viscose need to be mercerized to bring dyeuptake and lustre
of cotton at par with that of viscose

5.5.2 Problems faced in mercerization of cotton/viscose blends

Solubility of viscose in alkaline solutions causes weight and strength loss

Dissolution occurs at 80-130 g/l concentration of NaOH
(Viscose becomes highly swollen)

42
This problem can be solved by using a modifying sequence of mercerization as described
below:

Hot impregnation (saturation with hot mercerization liquor to minimize swelling

of viscose)

Addition of electrolyte in the mercerizing liquor

Use of KOH or admixture of NaOH and KOH (KOH induces less swelling)

HOT water rinse (at 90oC); viscose solubility is less at higher temperature

Addition of electrolyte (NaCl) in rinsing bath (electrolyte suppresses swelling of

viscose)

5.6 Machines for Mercerization:

5.6.1 Yarn mercerization

Yarns are mostly mercerized in hank form. Yarn mercerizing machines generally consist of
two rollers, on which the hank can be mounted. A device can be used to apply tension (to
stretch) on the hanks. After the hanks are mounted, the rollers can be lowered into a tray
which consists of caustic soda solutions of mercerizing strength. The hanks are allowed to
saturate with alkali, the tension is generally applied later. After sufficient time is allowed for
mercerization (1-2 min) the hanks are squeezed and rinsed. The tension is released once the
residual alkali concentration drops below 60 g/l. For optimum gain in tensile strength and
lusture, a tension causing stretch of 0.5-3% is applied, higher tension results in lower tensile
strength.

Figure. Hank Mercerizing Machine

43
5.6.2 Fabric mercerizing machines:

Fabric mercerizing machines are generally continuous operation machines with the ability to
apply controlled lengthwise tension. There are mainly two types of fabric mercerising
machines:

1. Chain Mercerizing Machine

2. Chainless Mercerizing Machine

1. Chain mercerizing machine

In these machines fabric is saturated with alkali solution and padded. The saturated fabric
passes over a set of rollers (airing rollers) which allows the swelling or mercerization to take
place. Fabric is again saturated and squeezed and passed into a stenter where length and
width wise tension is applied. Width wise tension is applied using stenter clips on chain

Figure. Pad Chain mercerized

This is followed by sprinkling of fabric with water to remove alkali. The tension is
maintained till the alkali concentration drops below 60 g/l. After this, fabric can be rinsed and
neutralized in open width washing machine (Tension may be relaxed).

The tension applied by means of clips in weft direction can be higher which can impart
higher lustre to the fabric. However the tension in width wise direction can cause the fabric to
expand in a non-uniform way, as shown in the figure below. Also there is a risk of fabric
getting torn near the edges where it is held by clips.

44
Chainless Mercerising Process

This method of mercerization running fabric through a number of rollers without the use of a
clip stenter is also called roller mercerization. The machine used has a number of stainless
rollers, or stainless and rubber rollers, of a relatively-large diameter tiered zigzag in close
contact to each other inside a long trough, with the lower tier designed to submerge in
alkaline solution for mercerization.

Chainless mercerizing machine tackles above problem by using bowed rollers (Figure 5.13)
to apply width wise tension. The clips of chain mercerization machine are replaced by an
expander unit consisting of bowed rollers. The stretch or tension applied in weft direction is
determined by warp wise tension in the fabric which in turn is controlled by oscillating
rollers. Other features are more or less similar to chain mercerization units (Figure 5.14).

Figure. Chainless mercerizer

This chinless mercerising machine is popular in industry.

Steps involved in mercerization machine:

Apply 200 to 220 g/l of caustic at the pad mangle at 100% wet pickup. Pass fabric over
timing cylinders. The number of cylinders must correspond to the range speed and provide
at least one minute dwell time. Clip fabric onto stenter chains and stretch weft wise.
Run fabric under spray washers to remove caustic. Release tension and continue washing
in open-width wash boxes, to further reduce the caustic. Neutralize with acetic acid and
dry the fabric.

Assessment of mercerised fabric

5.7 Determination of degree of mercerization (Barium activity number):

Although there are many methods to do this, one quantitative test based on the ability of
mercerized cotton to absorb barium hydroxide is widely used. Mercerized cotton can absorb

45
more Barium hydroxide than un-mercerized cotton and this is the basis for this test. The test
method is described below:

Mercerized and un-mercerized cotton samples (2 gm each) are treated with 30 ml of N/4
Barium hydroxide for two hours in conical flasks at room temperature. Preferential
absorption of barium hydroxide by cotton samples reduces the strength of Barium Hydroxide
solutions. The amount of Barium hydroxide absorbed can be determined by taking 10 ml of
Ba(OH)2 solution from each of the flasks and titrating it with N/10 HCl, phenolphthalein
being used as an indicator. Fresh Ba(OH)2 is also titrated (blank titration) to accurately assess
the actual Ba(OH)2 in solution.

The Barium Activity Number is given as:

BAN = (B-M) / (B-C)*100

Where B = Volume of HCl (ml) required for blank titration

M = Volume of HCl (ml) required with mercerized cotton

C= Volume of HCl (ml) required with un-mercerized cotton

For completely mercerized cotton the value of BAN is around 155 and for semi mercerized
cotton it varies in between 115 and 130.

Mercerisation efficiency is also determined by the measuring lustre, deconvolution count,

swelling index, benzopurpurine test, sodium hydroxide spotting test, dyeing test, etc.

EXCERSIZE 5

Part I: Discuss the following questions in detail

1. What do you mean by mercerization of cotton?

2. What are the different types of mercerization machines?
3. What are the different chemicals/auxiliaries used in mercerisation?
4. What are the advantages of mercerization of cotton?
5. How mercerization efficiency is measured?
6. What are the major changes occurred in mercerization of cotton?
7. What is yarn mercerization?
8. Give the different parameters to be controlled in mercerization of cotton.
9. What is barium activity?
10. Give the advantages of hot mercerization.
11. Mention the different parameters maintained in hot mercerization of cotton.

46
 Part II: Fill the blanks with the appropriate choice given below
1. Caustic soda is used in ………..process.
a. Whitening b. Mercerization c. Cleaning d. None of these
2. Mercerization is carried out with NaOH of
a. 10–15% Conc. b. 18–25% Conc. c. 5 –10% Conc. D. 25-35% Conc.
3. The ……….. of cotton is improved in mercerisation.
a. strength b. whiteness c. wetting d. absorbency
4. The mercerization is carried out ………..temperature.
a. 50oC b. 90oC c. room temperature d. 100oC
5. The mercerization is carried out using ………...
Alkai b. Acid c. Buffer d. Reducing agent

47
 Chapter Six

BLEACHING
6.1 Introduction to Bleaching
After desizing and scouring most of the textile fabrics especially the natural ones, retain slight
coloration. The source of the colour may be:
• Flavone pigment in case of cotton
• Soil and dirt acquired from atmosphere
• Contact with plant parts and seeds etc.
• Colour acquired during mechanical processing e.g., grease, oil etc.

The objective of bleaching is to destroy this natural or acquired color to bring the textiles in a
white state.

This may be necessary when:

• The fabric has to be supplied in white colour
• It needs to be dyed in pastel shades
• It needs to be printed

If the fabric is to be dyed in dark shades, then bleaching becomes an optional process.

In case of cotton, the motes or the seed coat fragments are visible on woven or knitted fabrics
after scouring. These appear as specks of brown or black colors on fabric surface. The color
of these motes is also destroyed by bleaching.

Dyeing an unbleached fabric in pastel shades might mask the brightness of applied color.
Many times, these bleached fabrics are given treatment with Optical brightening agents to
confer extra whiteness. Bleaching also removes residual impurities left by other pretreatment
processes like desizing, scouring etc. In that sense, the absorbency of a cotton fabric may
increase after bleaching.

Although reductive bleaching has been used in past to bleach wool and silk, today almost all
textile material is bleached by oxidative bleaching agents.

Bleaching agents can be classified as:

Oxidative bleaching agents and reductive bleaching agents

Oxidative bleaching agents can be further divided into

48
Peroxy compounds and Chlorine based compounds

Examples of Peroxy compounds Examples compounds of Chlorine based

Hydrogen peroxide Bleaching powder

Sodium perborate Sodium hypochlorite

Potassium permanganate Lithium hypochlorite

Peracetic acid Sodium chlorite

Examples of reductive bleaching agents

Sulphur dioxide
Sodium hydrosulphite
Sulphoxylates
Acidic sodium sulphite
Sodium bisulphites
Thioureadioxide

The main bleaching agents are

• Sodium hypochlorite (NaOCl)

• Sodium chlorite (NaClO2)
• Hydrogen peroxide (H2O2)

The use of oxidative bleaching dates back to the end of eighteenth century, when solid
bleaching powder (based on chlorine) was used for bleaching of cellulosic textiles. The
discovery of peroxide bleaching in 1925 has gradually resulted in replacement of other
bleaching processes with peroxide/peroxygen based bleaches. Out of the main bleaching
agents mentioned above, H2O2 has virtually replaced chlorine-based bleaching. It must be
mentioned here that hypochlorite and chlorite-based bleaching is still prevalent in some
developing countries to some extent. However, these have been withdrawn in most of the
developed countries due to the possibility of formation of AOX (adsorbable organic
halides) which are potential carcinogens.

49
6.2 Bleaching with sodium Hypochlorite (NaOCl):

NaOCl is sodium salt of Hypochlorus acid (HOCl). It can be prepared by passing chlorine gas
in a solution of NaOH or by electrolysis of NaCl solution (aqueous).

2NaOH + Cl2 → NaOCl + NaCl + H2O

Sodium hypochlorite is a strong oxidising agent, with a redox potential of 1400-1550 mV.
Cl2 acts as an oxidising agent in presence of water (moisture) only. Dry chlorine gas does not
have oxidising power.

Cl2 + H2O HOCl

HCl +HOCl HCl + [O]

Formation of HOCl is important as it provides the nascent oxygen molecule responsible for
oxidation (bleaching). NaOCl solution in water undergoes the following reaction:

NaOCl + H2O NaOH + HOCl

HOCl is a weak acid. Aqueous NaOH solution has a pH of 11-11.5 due to the presence of
strong NaOH.

Bleaching occurs due to the following reaction:

HOCl HCl + [O]

In acidic medium, the consumption of hypochlorite is very fast and can lead to cellulose
degradation by oxidation. The reaction is given below:

NaOCl + HCl ---> NaCl + HOCl

HOCl + HCl ---> H2O + Cl2

6.2.1 Bleaching of cellulosic fibres with NaOCl: Influence of process

parameters

The conditions like concentration, pH, time, etc. influence bleaching process in a major way.
Generally, cotton is bleached with NaOCl solution containing 1-3 g/l available chlorine at
room temperature in the pH range 9.5-11.

Available Chlorine or active chlorine is a unit of concentration used for hypochlorite-based

bleaches. One gram of 100% active chlorine bleach has the same bleaching power as one
gram of chlorine. It is based on the assumption that hypochlorite ions can liberate equivalent

50
amount of iodine by oxidation from a potassium iodide solution. The amount of iodine
liberated is measured indirectly by titration. Since the same amount of iodine can also be
liberated by equivalent amount of Cl2 gas, the term available chorine has become popular. In
that sense, available chlorine is a measure of active oxidizing matter in the bleach solution. It
is important to determine active or available chlorine in a bleach solution since the bleach
may also contain some fraction of chloride ions (a byproduct of bleach decomposition) which
has no bleaching power. Only hypochlorite ions have bleaching (and oxidizing power to
liberate I2 and cause bleaching).

Liquid bleaches sold for domestic use are typically 3–10% active chlorine, and should be
diluted to 1–2% active chlorine before use. Commercial domestic bleaching powder is
typically about 40% active chlorine.

Active chlorine values are usually determined by adding an excess of potassium iodide to a
sample of bleach solution and titrating the iodine liberated with standard sodium thiosulphate
solution.
ClO− + 2I− + 2 H+ → I2 +H2O + Cl−
(Hypochlorite ion) (Potassium iodide) (Acidic solution) (Iodine)
(Pot/sod. salt)
Similarly
Cl2 + 2I− → I2 + 2Cl −
And (determination of liberated I2 by titration)

2S2O32− + I2 → S4O62− + 2I−

From the above equations it can be seen that 2 moles of thiosulphate are equivalent to 70.9
grams (1 mole) of active chlorine or 51.5 g of hypochlorite ions. In other words a 51.5 g/l
solution of OCl− (or 75 g/l NaOCl) is equivalent to 70.9 g/l solution of available chlorine.

6.2.1.1 Effect of pH
The concentration of different chemical species in bleach bath depends on pH. The Figure 4.1
below, relative change in different types of chemical entities with pH change is shown.

Figure. Effect of pH on relative fraction of different chemical entities in hypochlorite bleach

bath

51
This plot can be divided in three distinct zones:

In acidic region (upto pH-5) the sodium hypochlorite hydrolyzes to form free hypochlorous
(HOCl) acid. At lower pH values hypochlorous acid decomposes and the chlorine gas is
liberated which has no bleaching action. The fraction of free hypochlorous (HOCl) acid
increases as the pH increases and at pH 5, almost all the hypochite exists as free
hypochlorous acid.

At pH-7-7.5, both hypochlorous acid and hypochrorite ions are present in almost same
concentrations.

In the pH range 9-11.5, most of the hypochlorite is present in the form of OCl− ions and not
as free acid. From the figure above it is clear that consumption of available chlorine is quite
low and oxidation of colored impurities is rather slow. This has less adverse impact on cotton
fibre itself and hence is known as the practical leaching range for natural cotton fibres.

It can be easily seen that rate of oxidation at around pH 7 is the highest. This means cotton
can degrade as the rate of consumption of available chlorine is quite high. Hence pH-7 is an
unsafe zone for bleaching.

The degradation occurring to cotton is measured in terms of cuprammonium fluidity. In the

figure below, one can see the degradation of cotton with increasing pH. It is easy to see that
the maximum degradation is occurring near pH-7 region, the same region where the rate of
consumption of available chlorine was the highest. If compared with above figure it looks
almost reverse of that. Hence on can surmise that bleaching with hypochlorite in the neutral
pH range (6-8) is dangerous for cellulosic fibres

Figure. Cupra-ammonium fluidity of cotton with change in pH

Therefore, the best conditions for bleaching are:

pH 6-7 (bleaching time 1 min.)

However, it is very difficult to control such short time. (can lead to cotton degradation)

So practical bleaching conditions are:

52
 At pH 9 Time to bleach - 45 min

At pH 11.5 Time approximately 4 hrs.

Temperature Room temperature

Concentration
2-3 g/l available chlorine

Commercial solutions of NaOCl are available as 40% (~ 400 g/l) solutions.

Bleaching with sodium hypochlorite

The advantages of using Sodium hypochlorite as a bleaching agent are:

1. It is economical

2. Risk of catalytic damage is low. (this is a problem with H2O2 bleaching)

3. Since it is a room temperature process, the energy costs are low

However, use of NaOCl is associated with certain disadvantages due to which its use is on
the wane. These are:

1. Fibre damage can take place if temperature and pH are not controlled.
2. It results in formation of AOX, which has led to it being banned in developed
countries for textile bleaching.
3. Bleached material can turn yellow on storage
4. Can degrade many dyes and FBAs ( simultaneous dying and bleaching or bleaching
and FBA treatment is not possible )
5. It cannot be used for bleaching of synthetic or protein fibres.
6. It does not produce a very satisfactory white.

The residual hypochlorite needs to be removed from the fibres after bleaching, as it may
damage the fibres due to lowering of pH on storage (by absorption of CO2 gas from the
atmosphere).

The residual hypochlorite, also termed as residual chlorine is removed by treatment with a
reducing agent. This is done by treating the bleached and rinsed fabric with 2-2.5% of a
reducing agent for 15 min at 40oC. Sodium Sulphite, bisulphite, hydrosulphite, thiosulphate
etc. may be used. The treatment is also known as antichlor treatment.

53
6.3 Bleaching with NaClO2 (sodium chlorite)

• Sodium chlorite is another Chlorine containing oxidising bleaching agent. It remains

stable at high pH and has to be activated with acids or acid liberating agents to bring
down the pH when bleaching takes place.

• The bleaching species in Sodium chlorite is ClO2 gas which is liberated at pH below
6. The equations below show the decomposition of chlorite into ClO2 gas and other
components.

• These acid generators (activators) include Sodium Chloroacetate, Triethanol Amine,

Ammonium Persulphate etc.

• Acids like formic acetic, phosphoric acids may be used to bring the pH down. Other
alternatives are esters like ethyl lactate or diethyl tartarate which hydrolyse to give
lactic and tartaric acid respectively.
Reactions:

4 ClO2– + 2 H+ 3 ClO2 + Cl- + 2OH-

5 ClO2– + 2 H+ 4 ClO2 + Cl- + 2OH-

ClO2 is a toxic corrosive gas.

NaClO2 + HCl NaCl + HClO2 pH 2.5

5HClO2 4 ClO2 + HCl +2H2O At lower pH

54
NaClO2 is stabilized at higher pH.

As can be seen in the Figure above, with reducing pH chlorite ions start forming chlorous
acid (HClO2). This is a weak acid and remains un-dissociated at strong acidic conditions.
However, below pH 6, it starts forming ClO2 which is a corrosive and toxic gas and is
supposed to be responsible for bleaching. Formation of excessive ClO2 gas may result in
wastage of the bleaching agent and may also damage the substrate.

At pH 1-2, the rate of bleaching and the evolution of ClO2 gas is very rapid. Hence a balance
is struck between the liberation, the evolution of ClO2 and the rate of bleaching by adjusting
the pH in the range of 3.5-4. This is done with acetic or formic acid and buffered with
Sodium dihydrogen phosphate.

Use of NaClO2 also results in formation of AOX but it is about only 1/10th of that generated
by hypochlorite.

Salient features of NaClO2:

Redox potential – 1040-1200 mV

Bleaching temperature – 70-90⁰ C

Suitable pH for bleaching – 3-4.5(4+- 0.2)

Problem of Corrosion with NaClO2 Bleaching:

The ClO2 gas released during bleaching has the tendency to corrode most of the equipment
used in the construction of bleaching equipment. The following approached are used to
minimize the corrosion of bleaching equipment:

1. Use of corrosion resistant materials like Stainless Steel with 2.5% Molybdenum.
Titanium can be used as the material of construction but it is very costly. The other
option is to have normal stainless steel vessels lined with Ti, glass or ceramics. Glass
fiber reinforced plastic can also be used as a choice for corrosion resistant material of
construction.

2. Use of ClO2 scavenging chemicals. These chemicals scavenge and bind the liberated
ClO2 and suppress the corrosion of construction materials. These are (NH4)H2PO4,
sodium and ammonium nitrate, nitric acid, melamine, urea etc.

3. Use of chlorite stable surfactants. The foam of the surfactant can trap the ClO2 gas
formed and prevent it from coming in contact with the walls of the equipment.

55
6.3.1 Effect of Temperature:

NaClO2 is a fibre gentle bleaching agent. It does not affect cellulose adversely even if
bleached at high temperature (100o C) for several hours.

At boil, the bleaching time is a few hours (1-4).

However, bleaching at ambient temperature may require overnight batching.

The rate of bleaching rate double for every 10oC rise in the process.

Advantages and disadvantages of sodium chlorite bleaching

1. It can be used for both cotton and synthetic fibres. Since it works in acidic conditions,
it is better suited to bleach synthetic fibres which are susceptible to alkaline pH.

2. Since it is used in acidic conditions, hardness of water does not impair the process
(low ash content).

3. Leaves material soft. Hence it can be preferred for knitted fabrics.

4. It can give good white colour with excellent mote removal even without kier
boiling.

5. It causes very little or no cellulose degradation.

6. It is insensitive to the presence of metal ions.

Disadvantages

1. More expensive than NaOCl or H2O2.

2. It cannot be used to bleach silk and wool (pink coloration).

3. ClO2 can corrode the metals used in construction of processing vessels.

4. ClO2 is also a toxic gas, so care should be taken in handling the bleaching process.

5. Since in works at acidic pH, wax removal is not very satisfactory.

6.3.2 Antichlor Treatment

Antichlor treatment is given with Sodium thiosulphate or Oxalic acid 85-95oC for goods to
be dyed subsequently.

For white goods, an FBA or softening treatment maybe given at pH 6-7.

56
6.4 Bleaching with hydrogen peroxide (H2O2)

H2O2 is gradually replacing other oxidative bleaching processes. The reasons for its dominance
are:

1. Since it’s by products are only water and oxygen, it is an eco friendly agent.

2. It is a versatile and universal bleaching agent. It can be used at almost any temperature, in
batch or continuous processes for almost all the fibres.

H2O2 is supplied as concentrated transparent solutions in dark bottles. It is quite stable in acidic
pH and can decompose in presence of alkalis or UV light.

Mechanism
H2O2 H+ + HO2–

HO2– HO– + [O]

Perhydroxyl ion (HOO–) is the bleaching agent. Its redox potential is 810- 840 mV.

For bleaching to take place, the stabilized H2O2 needs to be activated with alkalis. In alkaline
medium H2O2 decomposes as per the following reaction:

H2O2 + OH– OOH– + H2O

The perhydroxy ions formed in the reaction are the actual bleaching agents which decompose to
provide nascent Oxygen (O) which oxidizes organic compounds including colouring matter.

Above pH 10.8, the formation of HO2– ions is so rapid that it decomposes to liberate O2 gas
which has no bleaching power. The high rate of formation can also degrade cotton. Hence pH in
H2O2 bleaching is maintained between 10.5-10.8.

6.4.1 Auxiliaries Used In H2O2 Bleaching

• Activator
• Stabilizer
• Sequestering agents

57
6.4.1.1 Activators

Commercially available H2O2 is stabilized at acidic pH. For it to act as an oxidizing beaching
agent, the pH of H2O2 solution must be increased to basic range with the help of an alkali. The
most commonly used alkali used in raising the pH of the bleach bath is sodium hydroxide
(NaOH).

6.4.1.2 Stabilizers:

The stabilizers are added to regulate the perhydroxyl ions to prevent rapid decomposition of
bleach bath and fibre damage. These may act by:

1. Buffering action
2. Sequestering of heavy transition metal ions
3. Complexing with perhydroxy ions The most popular stabilizer used in H2O2 bleaching is
Sodium Silicate. It is easily available, economical and effective. The preferred ratio of
Na2O and SiO2 in silicates is 1:1. The silicate is supposed to provide stabilization by
formation of a complex with perhydroxyl ions which are released slowly at elevated
temperature. The silicate also provides a buffering action and its solution is colloidal in
nature.

The stabilizing action of silicates is improved by Ca or Mg ions and hence water of hardness
between 2-5o is recommended.

It is difficult to maintain the colloidal form of silicates in the industrial processes, deposition of
silicates on goods as well as equipment interior walls takes place. The deposition produces a
harsh feel on the goods.

Deposition on the equipment surface makes it abrasive. A thorough rinsing of goods can be
helpful in removal of harshness on the fabric.

6.4.1.3 Sequestering Agents

It has been shown earlier that in the presence of alkalis, H2O2 undergoes heterolytic fission
resulting in formation of perhydroxyl ion. However, presence of transition metals or UV light
causes H2O2 to undergo homolytic fission to two hydroxyl radicals (OH•). The metal actions can

58
have a catalytic effect on the decomposition of H2O2. The rate of decomposition may be so high
that cellulose is attacked and oxycellulose formed. The oxycellulose thus formed results in poor
mechanical properties. In extreme case, holes may form on the substrate due to severe localized
action.

To minimize the harmful effects of metal cations, sequestering agents are often used. These are
compounds which sequester the metal cations, rendering them harmless. Some examples are:

• Poly phosphonates
• Poly hydroxyl carboxylic acids
• Amino poly carboxylic acids
• Phosphonic acids
• Poly acrylic acids
The sequestering agents prevent the metal ions from catalytically decomposing peroxide
solutions by chelating them. The complexes formed may be complicated 3 dimensional
structures involving water of solvation molecules. Generally these metal ions are held by five
membered rings and one sequestering agent molecule may interact with one metal ion. A
simplified representation of 3-D structure of the complex is shown below:

6.4.2 Effect of Process parameters

6.4.2.1 Effect of pH:

In acidic pH, H2O2 is stable, hence very little bleaching takes place. Since NaOH is a strong
alkali, it is difficult to plot variation of bleaching efficiency as a function of time. However,
concentration of alkali does have an effect on whiteness which is shown in the figure below.

Figure. Change in reflectance of bleached cotton fabric with increasing NaOH concentration in
bleach bath [4]

59
6.4.2.2 Effect of temperature:

In practice, the bleaching of cotton is carried out at or around boil (90-100oC). However, rapid
bleaching is possible in pressurized equipment at 120oC. Bleaching at low temperature (~80oC)
will result in concomitant increase in process time.

Advantages of Peroxide bleaching

1. It is a universal bleaching agent. It can be used for bleaching of natural, synthetic and
blended fibres.
2. It is possible to combine scouring and bleaching.
3. No antichlor treatment is required.
4. It is noncorrosive and does not produce unpleasant odour.
5. No AOX problem, no harmful by-products.
6. Residual size and wax removal continuous through bleaching; results in improved
absorbing and TEGEWA rating.
Disadvantages
1. Use of silicates as stabilizers has a risk of silica stain formation on goods and silica
deposits forming on plant machinery
2. Catalytic damage to cotton can occur in presence of transition metal cations (hard water).
3. Not very effective for synthetic fibres.

6.5 Assessment of bleaching efficiency

Since the main objective of bleaching is to transform textile goods into high, uniform whiteness,
the most important assessment of textile goods is assessment of whiteness Index. This is done
by:
1. Comparing the sample against a standard which can be magnesium oxide or barium
sulphate. The standard has 100% reflectance at all wavelengths. For bleached samples the
reflectance at 460 nm (blue region) is measured. Unbleached cotton shows a reflectance
of 55% which increases to 83-85% on bleaching.
Other whiteness calibrations take into account the reflectance at short as well as long
wavelengths (for blueness and redness respectively).
W(Harisson)= 100-(R670 –R430) and W(Stephensen)= R430 (R670- R430)
The term R430 refers to the yellowness which reduces whiteness.

60
2. Calorimetric methods

One of the most popular whiteness indices is Hunter lab Whiteness index (W Hunter)).
This system uses the Hunter L, a, b values for evaluation of whiteness index which is
given by
W= L-3b
This formula gave importance to blueness/yellowness but neglected redness/greenness.
Good, bleached fabric should have a WI > 75.
However, in case of Stansby, importance was given to all three parameters. Thus
W(Stansby)= L-3b+3a
In Europe, Burger Index once used most widely is W(Burger)= 0.333Y+1.060Z-1.277X
6.6 Optical whitening agents
Most of the textile materials, especially the natural ones, appear slightly yellowish or off white
even after they have been bleached. They are not bright white. The reason lies in slight
absorbance by these substrates in blue region of visible light which leaves these materials
appearing as slightly yellowish. Across cultures, bright white has been regarded as signifying
purity and hence there have been efforts to achieve brighter whites. Attempts have been made to
tint white goods with blue pigments since bluish whites are preferred over whites with yellowish
or greenish tinge.
To make whites brighter, one needs to increase the reflectance of the bleached goods further.
This is possible with certain additives which absorb UV component of solar radiation and emit in
visible range (preferably in blue violet region). Thus, the overall reflectance of the goods
becomes higher than that of bleached goods with a blue tinge to it, making it appear much
brighter.

The first recorded evidence of OBA application happened in 1929 when Paul Krais applied
aqueous extract of aesculetin-6-glucoside (a naturally occurring OBA) on linen.

61
 Aesculetin-6-glucoside

These agents have been known as Fluorescent Brightening Agents (FBA) or Optical Whiteners
(OWA). They are distinct from blueing agents in that while blueing agents suppress overall
reflectance, the OBAs actually enhance it.

Figure. Reflectance spectra of a typical textile fabric. A) Bleached white fabric B) Bleached
white fabric with addition of a bluing agent C) Bleached white with addition of an Optical
whitening agent

In the figure above, it can be seen that even after bleaching, a white fabric tends to reflect less in
blue (lower wavelength region), making it appear slightly yellowish/off white (curve A). After
addition of a bluing agent, the fabric his higher reflectance in blue region as compared to higher
wavelength regions (curve B). Although, addition of a bluing agent reduces the overall
reflectance and thus making it less bright, the bluish tinge it acquires makes up for the loss of
brightness. But when an optical whitening agent is used, not only does the reflectance in blue
region increase, the overall brightness also increases (Curve C). Hence the fabric appears whiter
and also brighter. This increase in overall reflectance is accompanied by an absorption in UV
region of solar spectrum.

6.6.1 Mechanism of OBA action

OBAs are designed to absorb light between 340 to 380 nm (UV spectrum) & emit it in the range
425 to 450 nm (visible spectrum). Effective OBAs must absorb strongly in UV region and emit a

62
large part of the absorb energy in the visible region. OBA molecules have an extended
conjugated bond system as it is capable of strong fluoresce.

6.6.2 OBAs for cellulosic substrates

Brighteners for cotton are anionic in nature and are applied in a way similar to the application of
direct dyes. A range of products varying in substantively from high to low is available. Low
substantively OBAs are suitable for application by continuous method while the high
substantively ones are applied by exhaust method. OBAs can be applied during bleaching or in a
separate step after bleaching.

Since fading of OBAs on cellulosic substrates is faster due to poor light fastness, they need to be
fortified frequently. This is generally done by formulating them in washing soaps and detergents.

The most common OBAs for cellulosic fibres are based on triazine derivatives of
diaminostilbene disulphonic acid (DAST) with following chemical structure.

Where M is alkali metal like Na or K, or ammonium cation

R1 is an aromatic amine residue /its derivatives

E.g. or

R2 is generally aliphatic amine derivatives

E.g. N(CH2CH2OH)2or -NH-CH2CH2 OH

The following product (vic triazol)

63
Has a light fastness of 5 on cotton, which is very high for OBAs on cotton. It is stable to chlorite.

Hypochlorite bleaching and can be applied along with resin finish. However, it is expensive.

Nylon –

OBA generally used for Nylon are anionic in nature like acid dyes. These are generally applied
from an acidic bath (pH – (4-5).

Polyester-

The OBAs for polyester are dispersing type. They can be applied by exhaust & pad-thermosol
(continuous process) or by addition directly in the melt (mass brightening) like as in mass
coloration. Following OBAs are useful for polyester.

These can be applied by exhaust at 125-130oC and by thermosol operation at 160-220oC.

64
Can be applied by thermo sol process above 190oC. The light fastness of OBAs on PET is
generally higher at 5-6.

Acrylic fibre-

OBAS for acrylic fibres are generally applied from acidic baths by exhaustion around boil.

Derivative of 1,3-diphenylpyrozoline (figure below) can produce very high whiteness of violet
tinge, the OBA is unstable to chlorine bleach and can produce light fastness of 4.

The following product is stable to chlorite and can be applied during bleaching itself. It can also
give a light fastness of around 4.

EXCERSIZE 6

Part I: Discuss the following questions in detail

1. What is the need of bleaching of textiles?

2. What are the different types of bleaching agents used for cotton bleaching?
3. What are the different chemicals/auxiliaries used in bleaching of cotton with
hydrogen peroxide?
4. What are the advantages of hydrogen peroxide bleaching?
5. What are the disadvantages of sodium hypochlorite bleaching?
6. How bleaching efficiency is measured?
7. Give the different parameters to be controlled in hydrogen peroxide bleaching
of cotton.

65
 8. Which is the active species in peroxide bleaching?
9. Give the role of following in peroxide bleaching
a. Stabilizer
b. Activator
c. Sequestering agent
10. Mention the correct temperature and pH maintained in peroxide, sodium
hypochlorite and sodium chlorite bleaching.
11. What will happen if the rate of formation of per hydroxyl ion in peroxide bleaching is
below and above optimum level respectively?
12. What do you mean by whiteness index?
13. What is optical bleaching?
14. Describe the mechanism of optical bleaching.

Part II: Fill the blanks with the appropriate choice given below
1. The pH of peroxide bleaching is ……
a. 12-13 b. 9-10 c. 4-5 d. 6-7
2. ……….. is an universal bleaching agent.
Bleaching powder b. Hydrogen peroxide c. Copper sulphate d. Hydrogen chloride
3. All bleaching processes—————–the strength of fiber:
a. Increase b. Decrease c. No change d. None of these
4. The pH of sodium hypochlorite bleaching is ……
b. 13-14 b. 10-11 c. 4-5 d. 6-7
5. Bleaching of cotton is carried out using ……
a. Alkali and acid b. oxidizing and reducing agent c. soaping agent
d. sequestering agent
6. Bleaching of cotton is never done after ……
a. Scouring b. mercerisation c. dyeing d. desizing

66
 Chapter Seven

COMBINED PRE-TREATMENT PROCESSES

As has been discussed so far, the pre-treatment processes are designed to remove the specific
type of impurity from a fibre. For example, the specific processes to deal with removal of sizes,
natural impurities and colouring components are known as desizing, scouring & bleaching
respectively. All these processes employ specific chemicals and process conditions like
temperature, pH, and time to optionally remove the specific impurity. Most of the time these
processes many not be compatible with each other and hence have to be carried separately in
specific sequence.

Now a day, industry has become increasingly aware about the optimal use of resources like
water, energy and on the other hand the fallout of pollution caused by industrial textile processes.
All these pre-treatment processes consume large amount of water and energy. Combining any of
the two or all processes can result in huge savings in terms of water, energy and reduced effluent
load. In the subsequent sections, such combined pre-treatment processes will be discussed.

7.1 Combined Desizing and scouring

Traditionally Desizing is carried out with acid or enzymes (starch based sizes) which are carried
out in acidic medium. This type of Desizing cannot be combined with alkaline scouring where
higher pH is used. Now a possibility of combining dDesizing with scoring arises if dDesizing
can be carried out in alkaline conditions. This is possible if oxidative Desizing is carried out.

Following recipe can be used (Pad –steam)

Potassium per sulphate 3 g/l

Sodium hydroxide 70 g/l

Wetting agent 1 g/l

Nonionic detergent 10 g/l

67
The fabric is padded and steamed for 12 min. The fabric is washed in an open soaper. The
temperature in first compartment is at boil with gradually reducing temperature in subsequent
compartments.

7.2 Combined scouring and bleaching

Now a days, most of the textile industries are using this technique of combined scouring and
bleaching. The options available for cotton scouring are alkaline scouring with sodium
hydroxide, enzymatic scouring or solvent/emulsion scouring. The approaches to combine
scouring and bleaching are based on hydrogen peroxide as it is carried out under alkaline
conditions. Other per oxygen compounds like potassium per sulphate (PPS) have been used in
H2O2 based single stage scouring and bleaching. An example is the following recipe:

NaOH - 5%
H2O2 - 1%
Temp. - 70oC
PPS - 0.5%
Contavan GAL (stabilizer) - 0.4 g/l
Time - 2hrs
M:L ratio - 1:30
Attempts have also made to combine bio-scouring with per acetic acid bleaching. For example-
TAED (tetraacetylethylenediamine) - 2 g/l
Sodium perborate - 0.15 ml/l
Pectinase - 2 g/l
Egyptol (non ionic surfactant) - 5 g/l

The treatment time - 90 min

Temperature - 60oC

Washing is done with boiling water followed by cold water rinse and drying.

Although this recipe can be used for one stage desizing, scouring & bleaching, best whiteness is
obtained when the fabric is desized prior to the treatment. It was also found that peracetic acid
does not suppress the activity of enzymes.

68
The following recipe is followed in industry for combined scouring and bleaching

Detergent: 1 g/l (Stock Solution - 1%)

NaOH: 3 g/l (Stock Solution - 2%)
H2O2: 4 g/l (Stock Solution - 3%)
Peroxide stabilizer : 1 g/l (Stock Solution - 1%)
Sequestering agent: 1g/l (Stock Solution - 1%)
Temperature: 100oC
Time: 1 Hour

7.3 Combined desizing, scouring and bleaching

The attempts to combine all three sequences are again based on alkaline scoring and bleaching.

A process for combining all three preparatory processes (Desizing, scouring & bleaching) was
carried out by Gulrajani et.al.

They optimized a recipe which is given below:

Scouring agent - 4%
Hydrogen per oxide - 1-2%
Temperature - 95oC
Time - 180 min
Sodium silicate - 2%
Wetting agent - 0.1 % (sodium octyl sulphosuccinate )
pH - 10.5 (soda ash)
The scouring agent has the following compositions:
Pine oil - 5 parts

Emulsifier - 4 parts

Perchloro ethylene - 1 part

The fabric is padded twice in to 80% pickup and stored in a J-box type container.

After treatment, samples are washed with cold water and dried.

69
New concepts

In the last decades there have been some developments which have focused on the mechanical
aspect of the process to improve the impurity removal. These processes have developed systems
which intensify the interaction between the liquor and the fabric.

Some of these processes are:

1. Ben bleach concept
2. ROCO yet bleaching system
3. Kuster’s flexinip process
4. Dip sat vario process

All these ranges have a common function, i.e. maximum increase of application when
impregnating the material with the bleaching liquor before steaming. They all prevent creasing
and chafing in the steamer and make alkaline scour boiling. A shorter production cycle means
higher final quality.

The specific novelty of Booster system (Benninger AG) is the inclusion of a special low liquor
trough following the classical saturator for maximum application impregnation.
Ben bleach system consists of four modules:
Ben-Injecta – for Desizing
Ben –Impacta – Impregnation
Ben-Reacta – For steaming
Ben extracta – washing
Desizing is done in a separate module (Ben Injecta) for size removal.

Ben Injecta: In Ben bleach system, the steam at high temperature (100°C) is allowed to impinge
on the fabric in a narrow casing. Due to high turbulence caused in the casing, penetration of the
fabric by the steam is thorough. This ensures intensive interaction between the steam and the
size. This results in dissolution of size material very quickly and efficiently without any pre-
swelling. Ninety percent removal of sizes, greases and waxes is claimed.

Ben Impacta: Ben Impacta, better and faster impregnation of fabric with controlled liquor pick-
up is ensured by having High liquor exchange through turbulent flow.

70
Ben-Reacta: In ben-Reacta, a combination steamer (fabric in tension in open width and in
plaited form) allow a steaming time from 1 to 60 min. Air-free conditions and control of steam
quality ensure constant conditions in steamer.

Ben- Extracta: In Ben-Extracta, energy and water are conserved using counter current flow of
wash liquor and liquor segregation. It is clear from the figure below that space requirement is
also lower.

Bleaching Drying
Raco-Yet (Ramisch Kleinewefers, Germany is a machine for single step desizing-scouring-
bleachng process with a process time od about 1-3 min. The unit consists of inlet, applicator,
reaction storage unit, post-scouring machine and automated chemical metering station. Raco-Yet
utilises a mixing nozzles, in which steam, chemicals and water are mixed and ejected as heated
aerosol, which is applied to the fabric structure and the capillaries of the fabric.

Flexinip applicator (Kuster, Germany) is based on the concept of add-on, meaning application of
liquor without any exchange of substances. No interaction occurs between liquor and textile
materials during application so that the changes in concentration in wet-on-wet processes or
tailing effect in case substantive products do not occur. It consists of a V shaped trough. The
fabric is drawn down through this trough, wet or dry and leaves the bottom slot with an evenly
applied pressure on both sides. Application is truly additive-there is no recycling of mixed or
depleted liquor. Immersion time is only 0.15 seconds at 100 m/min. An extremely fast turnover
of the trough liquor prevents concentration variation and cooling or heating of the liquor by the
fabric.

The bleaching liquor application is identical from fist to the last meter of the fabric. 10% saving
in chemical cost is reported in one step bleaching. The desized, still hot (90oC) fabric with a
moisture content of about 70% passes downward into a 10 litre capacity trough in which the
bleaching bath is renewed in a matter of second. Emerging at the bottom, the fabric passes
71
between two flexible squeezing rollers that adjust the total pick-up to 150%. In case of
mercerization and causticisation, add-on application results in a constant concentration of caustic
soda and auxiliaries.

Dip-sat Varic (Goller, Germany) system generates a high degree of humidity on the fabric
leading to very efficient swelling of fats, waxes and cotton seeds in single step bleaching. This
system can be incorporated into any existing range and is based on a free liquor add-on, i.e.
impregnation without squeezing the fabric. The substrate absorbs maximum of liquor and the
excess liquor runs back to the first trough. An automatic system controls the concentration of
chemicals. The desized fabric passes in this manner through the Dip-Sat system with a capacity
of 10 litres and a moisture content of 60% and then runs horizontally into a steamer with a
maximum application of approximately 140%.

EXCERSIZE 6

Part I: Discuss the following questions in detail

1. What are advantages of combined pretreatments?

2. How does one can carry out combined scouring and bleaching?

3. What are different modules of Ben bleach system?

4. Discuss the combined desizing and scouring?

5. What are the machines where combined pretreatments can be carried out?

6. Differentiate batch and continuous type of pretreatment processing.

Part II: Fill the blanks with the appropriate choice given below
1. Combined pretreatments are to save …………
a. Energy b. water c. both a and b d. none
2. In industry, the most practiced combined process is …………
a. scouring and bleaching b. desizing and bleaching c. mercerization and
bleaching d. desizing and mercerization

72
 Chapter Eight

PRETREATMENT OF OTHER TEXTILE FIBERS

8.1 Preparation of Protein Fibres

8.1.1 Preparation of Wool

Carbonization
Scouring
Bleaching
Preparation of Silk
Silk degumming
Silk bleaching

Preparation of Wool

Wool is perceived to be a clean, green, natural fibre. However, raw or ‘greasy’ wool is
contaminated with natural impurities, the type and level depending on the breed of sheep, and the
conditions under which the wool is grown. These impurities, which may be up to 40% (or more)
by weight, must be washed off before the wool can be used as a textile fibre.

8.1.2 Impurities in raw wool

Wool fleeces usefully contain less than 50% of clean fibre, being heavily contaminated by wool
wax, skin flaxes, suint, sand, dirt & vegetable matter. Raw wool contains 30 to 60 % of wool
grease compared with 0.5% of oil & wax in cotton. Following are the impurities present in wool
fibres

Wool Wax: Whether it exists as pure wax or a mixture with other contaminants. The wool wax is
partially degraded during its exposure on the sheep. The wool wax recovered during scouring
process & usually called wool grease.

Suint: It is water soluble and its solutions are alkaline because it contains a high percentage of
dissociable potassium salts of organic acids.

73
Inorganic Dirt: Sand grains, clay particles are present which are removed by detergency
mechanisms.

Organic Dirt: Organic dirt originates in fecal matter, in dead cells & possibly in organic soil
components. In traditional scouring small quantities of residual organic dirt are removed by
extensive rinsing.

Vegetable Matter: Vegetable matter is not removed to a significant extent in the scouring
process. It is mainly removed in carbonization process.
8.1.3 Wool scouring

The type and level of impurities in wool fibres discussed in chapter 1. The amount of impurities
especially the wool grease may be so high that it may hinder the processing of wool. The transfer
of wool grease from fibres to metallic machine parts may lead to

Dirt/oil accumulation on processing equipment

Poor drafting performance

Therefore, wool is generally scoured at fibre stage. Due to the presence of scales on wool fibre
surface, it has a tendency to felt/shrink. Scouring involves treatment with aqueous scouring
liquors containing mainly surfactants. Efficacy of scouring can be increased by mechanical
agitation or stirring action. However, this may also lead to fibre entanglement.

Hence the scouring process design should address:

• Effective contaminant removal from wool fibres

• Minimal fibre entanglement

8.1.4 Carbonization of wool

Objective: To remove cellulosic impurities from wool by treatment with acid/acid producing
salts.

The most commonly employed method for removal of vegetable matter from wool is treatment
with mineral acids, especially sulphuric acid. The treatment is based on the premise that the
stability of wool to hot mineral acids is higher than that of cellulose. The treatment with mineral

74
acids turns the cellulose into brittle carbonaceous mass which can be removed by crushing it into
a powder.

Sequences-

Acidification Drying/Baking Crushing Dusting Neutralization.

Processing Stages:

Treatment with (5-7% w/v) sulphuric acid & acid stable wetting agent.

Hydro extraction

Drying at 60-70oC to low regain

Baking at 110oC in dry heat for 2 min. (wool is relatively stable to acidic conditions. The
vegetable matter turns brown/black, becomes brittle)

Crushing to break the degraded vegetable matter to small fragments by passing through
heavy fluted rollers

Dusted & Neutralized with sodium bicarbonate.

Bleaching with acidic hydrogen peroxide to minimize yellowing caused by carbonization

Wool scouring- salient features

Generally done at raw wool stage.

Residual grease/wax is kept around 0.5-0.75%.

Older machines – Long bowls with flat bottoms.

Older machines – 4-5 long bowls (35-40 m.)

Modern machines – Hopper bottomed bowls.

Modern machines – At least six bowls (16-28 m.)

Wool fibres are scoured with detergent by emulsification or by solvent scouring method.

Wool scoring may be carried out in a series of bowls where the wool fibre mass is transported
from one bowl to another with gentle stirring.

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Nonionic surfactants are primarily used for contaminant removal. Sodium carbonate may be used
as builder sometimes to facilitate contaminant removal when immersion time is short. As wool
gets cleaned progressively, the composition of treatment bowls keeps changing.

The most important auxiliary used for wool scouring is a detergent. Alkyl phenol ethoxylates
have been used as highly effective detergents but are being phased out due to environmental
concerns. Due to the Eco-friendly nature, fatty alcohol ethoxylates are nowadays being preferred
over Alkyl phenol ethoxylates.

Wool scouring machines

Wool scouring machines may be classified into the following main types:

Swing rake machine

Harrow machine

Paddle machine

These machines have a mechanism to continuously agitate wool in a rectangular bowl or shallow
tank in such a way that it is transported to the next bowl. Before being transported to the next
stage, the wool mass is squeezed to minimize upstream contamination (Figure 8.1).

A feeding conveyor transfers the raw wool to the scouring trough. The wool is agitated and at the
same time moved forward by the action of a unit situated just above the bowl. An output
conveyor transfers the wool to the other bowl with an intermediate pad unit squeezing the wool
between the two bowls.

In case of swing rake type machine, the rakes move individually by a cam and crank
arrangement. The rakes come down, press the wool, move it forward and rise vertically up in the
process getting detached from the wool mass. They then move back, come down again and the
cycle continues.

For a gentler treatment, harrow type machine is used where all the prongs move together. This is
more suitable for finer wool, which can undergo damage and felting in a more vigorous swing
rake machine.

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The bowls have perforated false bottoms to allow the contaminants to escape and settle at the
bottom from where they can be collected.

Figure. Different types of wool scouring machines

8.1.5 Wool Bleaching

Wool bleaching is generally carried out by oxidation, reduction or combined oxidation/reduction

process.

8.1.5.1 Oxidative bleaching-

Wool is invariably bleached with hydrogen peroxide. The chlorine based oxidative bleaching
agents are not suitable for wool.

Under higher alkalinity, particularly in the presence of an oxidizing agent, wool get damaged.
So, the bleaching solution must be buffered to a maximum of pH 9.5. Phosphate buffers are
commonly used for this purpose. Sodium silicate also acts a buffer & stabiliser.

The alkali used for activating should be mild. The stabilizers used are phosphates, tetra sodium
pyrophosphate or sodium tri polyphosphate. Since wool can be damaged under alkaline
condition, an alternative is to bleach in acidic conditions using a per acid activator.

In normal bleaching the wool is conventionally steeped in a both containing 10-20 g/l H2O2 (35
% w/w) together with wetting agent. Bath is fitted with good circulation. The goods are usually
entered at cold, the temp raised to 40-50oC. & treatment continued for 3-6 hrs.

77
In High Temperature the commercially available auxiliaries like peroxide activators or stabilizers
are used to carry out bleaching at higher temperature. Bleaching can be carried out in 20-40 min
at 70 – 80oC at pH 7-8-8.0. The advantage is minimal damage to the wool, allowing higher temps
& thus rapid bleaching.

This is a BASF promoted process, bleaching is done at pH 5 with activator prestogen W at 80ᵒC
for an hour.

Hydrogen peroxide and peroxy compounds can cause progressive oxidation of disulphide bonds
in wool, leading to fibre damage which can be accentuated in subsequent dyeing. Hence
prebleached wool should be dyed preferably below 80ᵒC.

Another variant of acidic bleaching was developed by IWS & BASF. In this process, wool is
padded with 350 g/l H2O2 solution acidified by 2 g/l formic acid. By batching (cold-pad-batch)
overnight, excellent bleaching is obtained.

Bleaching with H2O2: H2O2 is used as bleaching agent sodium or calcium hypochlorite is never
used because they damage the fibre.

8.1.5.2 Reductive bleaching

Reductive bleaching of wool is carried out with following agents.
- Thiourea dioxide
- Sodium dithionite
- Zinc formaldehyde sulphoxylate
- Sodium formaldehyde sulphoxylate

Sodium dithionite is the preferred reducing agent. Bleaching is carried out at 45-65ᵒC at pH-5.5-
6 for 1 hour.

Bleaching can also be carried out with thiourea dioxide. It is a safer alternative to other reductive
bleaches.

To prevent heavy metal catalyzed decomposition of bleach bath, inclusion of a sequestering

agent is a must. The bleaching is carried out at pH 7 at 80ᵒC for an hour. Bleaching species is
thiourea dioxide.

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8.2 Pretreatment of Silk

Silk is a strong, soft, lustrous fiber extruded by certain kinds of silk worm. Molecules of silk
fibroin are polypeptide chains.

Composition of cultivated raw silk.

Component Percent
Fibroin 70 – 80%
Sericin 20 – 30%
Waxy matter 0.4 – 0.8%
Carbohydrates 1.2 – 1.6%
Inorgamic matter 0.7
Pigment 0.2

The main objective of silk degumming process is to impart soft handle and lustre to silk by
removing sericin, any impurities picked up during reeling throwing etc. Some natural wax,
coloring matter and minerals may also be removed during degumming.

Since sericin forms bulk of the gum or the outer protective coat in a silk filament, which also
happens to be a protein, the process mainly consists of cleavage of peptide bonds of sericin,
either by hydrolytic or other methods, and its subsequent removal from fibroin by solubilization
or dispersion in water.

Following are the main Degumming Processes:

a) Extraction with water.
b) Boil-off in soap.
c) Degumming with alkalies.
d) Degumming with acids.
e) Degumming with enzymes.
f) Degumming with organic amines.
Although both fibroin and sericin are proteins, they differ significantly in their constitution.

The main constituents of fibroin are glycine, alanine and serine whereas in sericin it is serine,
aspartic acid and glycine. Hence any degumming method should target the peptide bonds

79
between the amino acids found in majority in sericin. However, in practice, methods have been
developed on empirical basis.

8.2.1 Extraction with water

Sericin removal can be achieved in water at high temperatures. It is not a commercial process.
Upto 96% sericin can be removed by extracting it with water at 115oC for 3 hours. Although
there is still a doubt if the removal occurs through hydrolysis or dissolution.

8.2.2 Boil-off in soap

It is an old process and seems to be still favored commercially. Olive oil soap (Marseille soap) is
the most widely used soap. Following is a typical recipe:

Marseille soap 20-30% owf

Time 90-120 min.

Temperature 90-100oC

M:L 1:40

Since large amounts of soap are used, this method works out to be expensive. There have been
attempts to first carry out partial degumming with a spent or exhausted soap bath and complete
the degumming in a fresh bath. Alternately, addition of a small amount of alkali may result in
saving of both time and cost. Addition of upto 0.18% of free alkali does not result in weakening
of silk. However, excessive alkali in degumming liquor may result in loss of strength, lustre and
elasticity of silk.

The amount of sericin removal also depends on the type of soap used in the degumming process.
It is postulated that the degumming depends on the alkali formed on hydrolysis of soap and the
soaps hydrolyzing the most have the highest degumming power. In the table given below, this
correlation is apparent.

8.2.3 Degumming with Alkali Buffer

Though use of alkalis for degumming works out to be economical as compared to soap
degumming in terms of chemicals and labour cost, improved productivity etc., it can leave silk

80
yellowish and harsh. Hence alkalis are not recommended to be used alone. With alkalis, the pH
of the boiling bath should be maintained between 9.5-10.5. Below pH 9.5, the rate of degumming
is too slow and above 10.5, the risk of chemical damage is high. Hence many times, alkaline
buffers like sodium carbonate/sodium bicarbonate, sodium hydrogen phosphate/trisodium
phosphate and potassium tetraborate/boric acid have been used. Sodium carbonate/sodium
bicarbonate is the most widely used buffer. In addition to the buffer, rate of degumming also
depends on concentration of electrolytes in degumming bath. The rate increases with increasing
alkali concentration. At a pH of 10 and temperature of 95oC, the degumming takes 60 min with
0.01 molar Sodium carbonate/sodium bicarbonate concentrations but at same pH and
temperature, is completed in 20 min with of 0.05 molar alkali concentration. A typical recipe is
given below:

Sod. Carbonate (0.5M) 5.3 g/l

Sod. Bicarbonate (0.05M) 4.2 g/l

Non-ionic Surfactant 3g/l

Temperature 95oC

Time 20 min.

Presence of salt especially calcium salts in alkaline degumming liquor increases the degradation
of silk. Use of sequestering agents like sodium hydrogen pyrophosphate has been known to
reduce this damage.

Commercial alkali based degumming formulations generally may contain protective agent for
silk, sequestrants, wetting/emulsifying agent, buffer salts, alkali etc. examples are Miltopan SE
(Henkel), P-400 (Hepatex AG), Sopajet L (Indifar), Setafin (Henkel), Idrosolvan S40 (Bozzeto)
and Serilan PCS (ROTA).

Degumming with alkalis happens due to systemic hydrolysis of peptide bonds, a non specific
reaction.

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8.2.4 Degumming with Organic Acids

Although acidic degumming has not been explored much, it is relatively safer than alkaline
degumming. With acids, effective degumming occurs in the pH range of 1.5 and 2. Silk
degummed sampled with citric and tartaric acid are found give results. Mineral acids may result
in significant damage to silk, hence generally only organic acids are used. Weight Loss is almost
independent of the acid type.

Unlike alkalis, dilute organic acids are specific in their attack on peptide bonds linking
aspartic & glutamic acid.

Attack on above link is around 100 times faster than other bonds.

The concentration of acid is chosen such that the carboxyl groups of aspartic acid are left
undissociated. This ensures faster cleavage of petide bonds of aspartic acid as compared to other
acids.

8.2.5 Degumming with Enzymes

Degumming with enzymes is considered to be a safer method which results in minimal damage
to silk. Since it is carried out at milder temperature and pH, the natural hydrophobic impurities
are not removed effectively. One of the advantages of using enzymes for silk degumming lies in
the fact those enzymes specifically targeting peptides bonds occurring in majority in sericin can
be selected. Since the constitution of sericin and fibroin is different, such enzymes will have
minimum action on fibroin. Enzymatic degumming is considered suitable only for yarn
degumming. They do not work well on fabrics, due to their inability to enter the interstices of the
fabric.

The main enzymes used for silk degumming are trypsin, papain and bacterial enzymes.

Trypsin

Trypsin is a serine protease with the highest activity at pH range 7-9 and 37°C. Ammonium
bicarbonate (0.1 M/l) can be used as buffer. It is applied at 1- 2% owf for 1-4 h. There are
studies which claim better degumming results when alkalis are combined with proteolytic
enzymes. In other studies, it is reported that a pretreatment with alkaline solution swells sericin
and results not only in better degumming but also in better scouring (wax, fat removal).

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Papain

Papain is obtained from papyrus latex. It is the most effective at 70-90oC temperature and at

pH-5. It is a sulphydryl enzyme and hence requires a sulphydryl compound as an activator.

Earlier, potassium cyanide and hydrogen sulphide and later sodium hydrosulphide, sodium

sulphoxylate, sodium sulphite etc. have been used as activators. Papain has a wider specificity
towards polypeptides as compared to trypsin.

Bacterial enzymes

Bacterial enzymes can also be used for silk degumming. A bacterial enzyme alkalase, developed
by Novo nordisk is claimed to be more effective than trypsin or papain.

8.2.6 Degumming with Aliphatic Amines

Aliphatic amines have been shown to be effective as degumming agents. Methyl, dimethyl, ethyl
and trimethyl amines can be used. Methyl amine, due to its low boiling point is not suitable for
commercial use. Amines show good degumming (upto 90 % sericin removal) with little loss in
tensile strength. Given below is a typical recipe:

Trimethyl Amine 0.25 mol/L

N.I.D. 3 g/l
Temperature 80oC
Time 45 min.
M:L ratio 1:25
Amines can also remove impurities like processing oil etc.

8.2.7 Assessment of degumming

The simplest method to assess degumming is based on weight loss. However, in this case initial
rapid weight loss may be followed by attack on fibroin. UV absorption at 280 nm has also been
used to assess extent of degumming. Absorption is due to tyrosine and tryptophan.

A lot of staining methods are also available which are based on the ability of a large molecular
weight dye to differentiate between sericin and fibroin. For example, picrocarmine stains sericin
in intense red color while the fibroin is colored yellow. Similarly, sericin in raw silk threads is

83
stained deep blue when immersed for 24 hours in a cold solution of litmus while fibroin remains
almost unstained.

8.2.8 Bleaching of silk

The natural colour of the silk varies with the type of the silk. Bulk of the naturally occurring
colour in the silk is actually contained in sericin. Since the degumming process is not able to
remove the sericin completely, Silk fibre retains some of its natural tint after boiling off. Thus,
mulberry silk retains some of its yellowish tings and in tussah silk it is even more intensive.
Thus, the case of obtained white colour in silk by bleaching varies with the silk variety.
Generally oxidative & sometimes reductive bleaching is employed in silk bleaching

The bleaching with reducing agents is similar to that of wool bleaching.

Hydrogen peroxide is the most preferred bleaching agent. The Chlorine based bleaching agents
namely bleaching powder, sod. hypochlorite and sodium chlorite are generally not used, since
these agents tend to chlorinate the fibroin.

The alkali used is either ammonia or tetra sodium pyrophosphate. Sodium silicate as the
stabilizer should be avoided as it can lead to formation of silicic acid which can render silk harsh.
Tetra sodium pyrophosphate and fatty protein condensates are preferable.

8.3 Preparation of manmade and synthetic fibres and Blends

Synthetic or manmade fibres are generally free from natural impurities which are present in most
natural fibres. However, the following impurities may be present in synthetic or manmade fibres
which may require removal before the material is dyed or finished:

a) Sizing agents
b) Spin finishes/anti-static agents
c) Processing/coning oils (in knits)
d) Sighting colours/dirt
e) Loom stains (grease, lubricants etc.)

The sizing agents generally used with synthetic fibres are either water soluble or self
emulsifiable compositions. They are easily removed at desizing stage.

84
Therefore, scouring of synthetic fibres is less cumbersome than natural fibres.

For most of the synthetic fibres, mild alkaline conditions in presence of a surfactant are sufficient
to remove the impurities listed above.

8.3.1 Scouring of Polyester:

100% polyester made from flat-filament or textured yarns contains spin finishes, coning oils,
tinting colours, and dirt as the major impurities. All these impurities should be removed before
dyeing. Disperse dyes are nonionic dyes and exhibit solubility in coning oils; if trace of coning
oil remains in the dyed fabric, bleeding problems occur. Thus, the dye migrates to the surface,
dissolves in coning oil, and bleeds easily dunning laundering.

Scouring: - Polyester fabric is scoured with a solution of sodium carbonate (1-5 g/l) and 1-5 g/l
detergent at 60-70˚C for 30 – 90 min. Scouring is carried out in a winch, jet dyeing m/c or on a
jigger. This mild scouring easily removes all the impurities on the fabric.

In case of a loom stain, spotting with a suitable emulsified organic solvent may be necessary.

While scouring with alkali, it is important to note that harsh conditions (high alkali concentration
or higher temperature) may lead to polyester fibre hydrolysis. This can result in weight and
strength loss.

8.3.2 Bleaching of polyester:

Polyester has good natural whiteness and bleaching is often not necessary. Hydrogen peroxide
and sodium hypochlorite has little or no bleaching effect. Polyester fibres may be bleached using
an acidified solution of sodium chlorite. Bleaching of 100% polyester is rarely required except
for full white fabrics.

The recipe for bleaching of polyester is:

NaClO2 (50%) 3-5 g/l

Formic acid for pH to 3

Time 1-2 hr.

Temperature 95⁰C

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8.3.4 Scouring of Nylon:

Nylon is used mostly in knit goods. The sizes are generally not used but coning oils may be
present. These may be self emulsifiable formulations. Since nylon has acidic and basic sites
present in its structure, anionic surfactants are avoided for scouring, as they can occupy dye sites
and may be difficult to remove. The scouring conditions are generally mild alkaline with
presence of non-ionic surfactants. The conditions are:

Non-ionic surfactant 2-3 g/l

Nonionic 1-2 g/l
Soda ash 1-3 g/l
Temperature 70⁰C
Time 20-30 min

Heat set fabrics can be treated at a higher temperature (95-100⁰C) compared to unset fabrics
(70-80⁰C).

Bleaching of Nylon:

Nylon is a sufficiently white fiber but heat setting can cause some discoloration which may
require bleaching. Nylon should be preferably bleached in acidic conditions due to its sensitivity
to basic pH. Hence both hypochlorite and H2O2 are not recommended. Bleaching with
hypochlorite can reduced the tensile strength of nylon fiber. Sodium chlorite is the most suitable
agent for nylon.

Per acetic acid is another equally effective bleaching agent for nylon. H2O2 and acetic acid in
presence of a strong mineral acid such as H2SO4 gives per acetic acid

CH3COOH + H2O2 -----------------→ CH3CO O OH + H2O

It is marketed as a clear, colourless solution of 35-40% strength, mixing of acetic anhydride and
H2O2 at R.T. in the presence of catalyst (such as, NaOH or ethylene diamine tetraacetic acid
EDTA), gives per acetic acid. Bleaching composition recommended is

Per acetic acid (36-40%) = 3 g/l

Sod. Pyrophosphate = 0.25 g/l
Wetting agent = 1 g/l
Dil. NaOH to adjust pH 6-7
86
The goods are entered at R.T. and bath is heated to 80-85˚C during 30 min and bleaching is
carried out for 30-60 min at 80-85˚C. Trace metals shd be avoided since they catalytically
decompose per acetic acid.

8.3.5 Scouring of acrylic (PAN)

Polyacrylonitrile (PAN) fibers are sensitive to alkaline conditions, hence strong alkalis are
generally avoided for scouring.

Conditions
Non-ionic detergent 1-2g/l
Tri sodium phosphate 1g/l
Time 30 sec
Temperature boil
It is important to cool the goods below 60⁰C before rinsing. Sudden drop in temperature may
result in formulation of creases which may be difficult to remove later.

Bleaching of acrylic fibre

PAN can also be bleached with sodium chlorite in acidic pH. It is not recommended to bleach
PAN with either H2O2 or NaOCl in alkaline pH. Acidic pH of sodium chlorite is safer for PAN.
The recipe is

Sodium chlorite = 1-2 g/l

Sodium nitrate = 1-4 g/l
Formic or oxalic acid = 1-2 g/l

At 80-90˚C for 30 min – 60 min. Add of a small amt of oxalic acid gives permanent whiteness on
the fabric which does not turn yellow on exposure to light or heat.

8.3.6 Scouring of Viscose:

Viscose fiber also does not contain any natural impurity. It can be scoured by:
Non-ionic or ionic surfactant 1-1.5g/l
Temperature near boil
Time 20-30 min

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 Soda ash or tri sodium phosphate 1g/l

Goods should be rinsed in tension less state as the wet strength of regular viscose is poor.

8.3.7 Pretreatment of Blends

8.3.7.1 Scouring of Polyester- cotton

Since polyester is sensitive to alkaline conditions at higher temperature, milder alkaline
condition is used while scouring polyester/cotton blends.
Following recipe may be used

Na2CO3 -- 5-10 g/l

Emulsifier -- 2-5 g/l

8.3.7.2 Bleaching polyester/cotton blends

In general, the cotton component of such blends requires bleaching. For bleaching of cotton
hypochlorite, chlorite and hydrogen peroxide can be employed. If both cotton & polyester need
to be bleached, sodium chlorite bleaching is preferred.

Polyester fiber in blends with cellulosic fibres in the ratios of 65/35 and 50/50 is common
construction. When cellulose portion is rayon, the blends rarely require bleaching, but when
cotton is present bleaching is usually necessary.

Chlorine bleaching can be done using 2-3 g/l available chlorine bleaching powder solution for 2-
3 h, which is followed by dechlorinating (anti-chlor) treatment. Sodium thiosulphate, sodium
bisulphite, ammonia, H2O2 etc. can be used as dechlorinating agents.
Alkaline hydrogen peroxide bleaching is the most preferred system for polyester/ cotton blends
and bleaching can be carried out on various equipment using batch wise, semi-continuous and
continuous method.

For blends, hydrogen peroxide is the preferred route for bleaching. The following recipe can be
used for bleaching P/C blends-
H2O2 (35%) - 30-40 ml/litre

Sodium silicate - 10-12 ml/l

88
 NaOH (100%) - 2-4 g/l
The fabric is padded with the liquor, steamed and stored in a J-box at 95oC for 75 min. After the
bleaching, the fabric is washed with hot water and dried
8.3.7.3 Scouring of Polyester-wool blend
The blend of polyester and wool may contain spin finishes, lubricants, sizes etc.
These can be removed under relatively milder conditions.
The scouring is carried out with following recipe:
Non ionic 0.5 - 1%
Soda ash/ NH4OH (25%) 0.25 – 0.5 ml/lit
pH 8-9
Time 20-30 min
Temperature 40-50oC

8.3.7.4 Bleaching of Polyester/wool blends

Since wool cannot be bleached with hypochlorite and chlorite, blends of wool can only be
bleached with H2O2.

Following recipe may be used-

H2O2 (35%) - 30-40 ml/litre

Sodium pyrophosphate - 2-4 g/l
NH4OH - To maintain pH at 8.5-9.0
Time - 2-4 hrs
Temperature - 40oC
8.3.7.5 Scoring of Acrylic/wool blends
Scouring can be carried out as follows:
Time 30 min
Temperature 100oC
Non-ionic detergent 1g/l
Acetic acid (80%) 0.5ml/lit

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8.3.7.6 Bleaching of acrylic/wool blends

Hydrogen peroxide is not suitable for acrylic fibre at highly alkaline condition and moreover
acrylic fibre turns yellowish on alkaline peroxide treatment. The discolouration can be improved
by after-treatment with formic acid in presence of detergent. Acrylic/wool blends can also be
bleached by a reduction bleach or by combination of peroxide and reduction bleaching process.

8.3.7.7 Bleaching of Nylon/ Wool blends

The only safe bleaching methods to bleach such blends is either reduction bleaching or
bleaching with acidic H2O2 with following recipe:

H2O2 (35%) - 12 - 15 ml/litre

Organic stabilizer - 2-4g/l
Wetting agent - 0.25 g/l
Acetic acid - for pH (5.5-6)
Time - 2-2.5hrs
Temperature - 65oC

EXCERSIZE 8

Part I: Discuss the following questions in detail

1. Discuss the impurities present in raw wool.

2. What is the need of scouring of wool?
3. What are the different methods of wool?
4. What are the different machines used for scouring of wool?
5. Which is the suitable bleaching agent for wool?
6. What is carbonization of wool?
7. What are the different reducing agents used for bleaching of wool?
8. What are the different impurities present in silk?
9. Give the importance of silk degumming?
10. Mention the different method of degumming of silk.
11. Which is the most popular method of degumming of silk?
12. What are the different enzymes used in degumming of silk?
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13. Discuss the methods of assessment of degummed silk.
14. Describe the bleaching of silk with hydrogen peroxide.
15. What are the different impurities present in synthetic fibres?
16. How pretreatment of synthetic fiber fabric and their blend with cellulosic fiber fabric is
different from pure cellulosic fiber fabric pretreatment?

17. Describe the importance of scouring and bleaching of synthetics.

18. Discuss the process of scouring of polyester.
19. Which is the most popular bleaching agent for polyester?
20. What is the pH maintained in sodium chlorite bleaching of polyester?
21. Describe the scouring and bleaching of nylon.
22. Which is the best bleaching agent for nylon?
23. Discuss the scouring and bleaching of acrylic fibre.
24. Describe the scouring of polyester/cotton blends.
25. Discuss the scouring and bleaching of acrylic/wool blended fabric.
26. Brief the method of scouring and bleaching of nylon/wood blends.

Part II: Fill the blanks with the appropriate choice given below
1. Degumming is done on …….
a. cotton b. wool c. jute d. silk
2. The bleach which tends to destroy silk is——————
a. Chlorine b. Hydrogen peroxide c. All of above d. None
3. Scouring is the special method used for cleaning.
a. Wool b. Nylon c. Silk d. Rayon
4. Why is heat setting done in fabrics?
a. For color fasting of the fabric b. For increasing the strength of fabrics
c. For setting of fabric dimension d. For increasing of softness feeling in
fabrics
5. The most preferred bleaching agent for polyester is …………
a. sodium chlorine b. Hydrogen peroxide c. sodium chlorite d. None
6. Degumming of silk is done using ……. Enzymes.
b. Trypsin b. cellulase c. pectinase d. amylase

91
 Chapter Nine

ASSESSMENT OF VARIOUS PRETREATMENT PROCESSES

9.1 Desizing

Assessment of desizing efficiency

The weight loss can be used as criteria for assessment of desizing efficiency

The weight loss is of the order of 7-10%

The more scientific method, which is used industrially also, is TEGEWA rating
test (Applicable for starch based sizes only)

Figure. TEGEWA SCALE (the figure on top of colored strip is amount of residual starch and the
corresponding rating is given under the strip)

The TEGEWA Association comprises of manufacturers of the following: Textile, paper, leather
and fur auxiliaries and colourants, surfactants, complexing agents, antimicrobial agents,
polymeric flocculants, cosmetic raw materials, pharmaceutical excipients and allied products.

TEGEWA was established in 1951 in Wiesbaden as an association of the manufacturers of

chemicals, the name being an amalgam of these key activities: TExtilhilfsmittel” (textile
auxiliaries), “GErbstoffe” (tanning agents) and “WAschrohstoffe” (detergent raw materials).

Reagent preparation

❖ 10 g potassium iodide (KI,100%) is dissolved in 100 ml of water

❖ To the solution, 0.6358 g of iodine (100%) is added

92
 ❖ The mixture is stirred well until iodine is completely dissolved in the KI solution.
❖ To the solution, 800 ml of ethanol is added
❖ The volume is to 1000 ml by adding water

Method of testing

One or two drops of the above solution are put on the desized fabric and rubbed gently. The
fabric should be cold and free from any residual alkalinity. In a short time, the color of the
spotted area changes. The change in color is assessed with TEGEWA scale visually.

Assessment

No Colour Change = No starch is present

Pale blue to bluish violet = Presence of starch size or a blend of starch + synthetic size
Brown = Presence of modified starch or a blend of starch/PVA size

9.1.1 Degradation of Cotton during Desizing

Degradation can occur with acid or oxidative desizing if proper care is not taken during the
desizing process.

9.1.2 Acid desizing

❖
Insignificant degradation of cotton with dilute sulphuric acid (upto 10 g/l) at R.T.
❖
Degradation of cellulose can take place if the temperature increases beyond 40oC or the
concentration increases beyond 10 g/l
❖
Fluidity increases from 4 to 5.8 rhes in 4 h
❖
About 70% of the starch is removed
❖
The fabric should be washed thoroughly and traces of acid neutralized
❖
If fabric dries before acid is removed completely, cotton degrades as per the following
equations
9.2 Scouring

On scouring cotton, following changes take place:

Loss in weight (5-10%)
Significant increase in absorbency (1-3 seconds)
Further improvement is TEGEWA rating
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 Slight increase in average DP (due to removal of low mol. wt. components)
Shrinkage
9.2.1Assessment of scouring efficiency
1. Practical tests of absorbency
2. Measurements of
(a) Weight loss
(b) Protein content
(c) Residual wax content
(d) Methylene blue absorption (removal of pectic substances)

9.2.1.1Sinking time test (AATCC Test Method 17-1994).

The scoured yarn is converted to a hank (18 in periphery, 5 g wt). The hank is connected with the
help of a hook (3 g) to a sinker which is a flat cylindrical plate (25 mm diameter, 15-40 g wt).
The assembly is put on 500 ml water in a glass measuring cylinder. Initially the air entrapped in
the hank causes the hank to float but as wetting starts and the air is replaced with water, the hank
starts to sink due to attached sinker. The time required by the hank to go inside water from
floating state is known as sinking time.

9.2.1.2 Drop test

The fabric is placed flat on a table and creases are removed. A burette is placed at a certain
height from the fabric surface. Distilled water drops are allowed to fall on the fabric. The time
required for the drops to be absorbed completely is noted as wetting time.

9.2.1.3 Measurements of Weight loss

The weight of dried cotton sample before and after scouring may be used as an indicator of
scouring efficiency. This difference when expressed in % (% wt loss) should be in the range 6-
9%.

9.2.1.4 Measurements of Protein content

The protein content is determined indirectly by analysing nitrogen content after scouring.

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9.2.1.5 Measurement of residual wax content

A dry cotton sample is refluxed for 3 h in chloroform in the Soxhlet extractor and (solvent).
After extraction the sample is reweight and the wt. loss is determined which is indicative of
removal of fat and wax. For well scoured cotton, it should be ~0.2%.

9.2.1.6 Methylene blue absorption (removal of pectic substances)

The details of this are given in next section.

9.2.2 Degradation of Cotton during alkaline Scouring

Although cotton is stable in dilute alkalis at high temperatures in absence of air, presence of air
causes serious degradation. This mainly results in oxy-cellulose formation, during which some
hydroxyl groups on glucosidic units get oxidized to keto and carboxylic groups.

Assessment of the degradation can be done by either assessing the aldehyde/carboxylic group
content of cellulose, measurement of fluidity or loss in tensile strength.

Following are some of the methods for assessment of cotton cellulose degradation:

1 Copper number, a measure of the reducing groups present in cellulose.

2 Carboxyl group content by methylene blue absorption

3 Cuprammonium fluidity, which is a measure of molecular chain length of cellulose.

4 Tensile strength of the cotton material before and after scouring.

9.2.2.1 Copper number

The first stage of cellulose oxidation during cotton souring results in formation of –CHO groups
from –OH groups. These aldehyde groups have a reducing tendency and can reduce alkaline
solution of copper sulphate, resulting in formation of insoluble cuprous oxide which precipitates
on the cotton cellulose. The amount of cuprous oxide formed is proportional to the amount of
reducing groups which is expressed as Copper Number.

The test is carried out as under-

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A solution is prepared by dissolving 100g copper sulphate in 1 litre of water. Another solution is
prepared by dissolving 350 g sodium carbonate and 50 g sodium bi carbonate in another 1 litre of
water. These two solutions are mixed just before use to form Fehling’s solution.

Three groups of cotton cellulose is boiled in a solution containing 100 ml of Fehling’s solution
and 200 ml of water under reflux for 15 min. during the boiling process some copper sulphate is
reduced to cuprous oxide which gets deposited on cellulose.

This mass of cellulose is filtered & washed with water. The cellulose is then transferred to a
beaker containing 1-2 gm ferriabric alum dissolved in dilute sulphuric acid. The cuprous oxide
present in cellulose reduces ferric sulphate and forms equivalent amount of ferrous sulphate. This
is titrated against N/100 ceric sulphate solution by dissolving the ferrous sulphate in sulphuric
acid. Ortho ferrous phenathroline is used as an indicator.

Thus, copper number is defined as grams of cupric copper reduced to cuprous oxide by 100 g of
cellulose under standard treatment conditions.

The copper number is determined by the following formula:

Where V = ml of ceric solution - blank reading

N is the normality of ceric sulphate solution

W is the weight of the bone-dry cellulose sample (it depends on type of sample; for normal
samples it is 0.25 g and for highly degraded samples 0.1 g is taken

Copper number for pure cellulose is 0.5, for scoured & bleached cotton below 0.3 & for viscose
less than 1.2.

9.2.2.2 Methylene blue absorption method

Normal cellulose generally has no affinity for methylene blue, a basic dye. When cellulose in
oxidized, -OH groups convert to aldehyde group. But when the oxidation is more severe, these
aldehyde groups can oxidize to carboxylic groups. In degraded cellulose, both –CHO & -COOH

96
groups may be present. Hence there is a need to determine the degree of cellulose oxidation in
terms of –COOH groups content.

Methylene blue absorption method is based on the principle that the carboxyl groups present in
cellulose are able to absorb methylene blue dye cations quantitatively from a solution of
methylene blue dye. The scheme is shown below:

The amount of dye absorbed can be determined by analyzing the drop in concentration of
methylene blue in treatment solution using calorimetric methods.

9.2.2.3 Cuprammonium fluidity

The degradation of a polymer results in reduction of degree of polymerization. At same

concentration, the degree of polymerization is related to the viscosity of its solution. Fluidity
(ease of flow) is a property inversely related to viscosity (resistance to flow). Thus, the
degradation resulting in reduction of the DP can also be assessed by measuring fluidity. In case
of cotton, the fluidity measurements are made on solution of cotton material in cuprammonium
hydroxide solution. In the table given below, fluidity values of various forms of cellulosic
textiles are given.

Type of cellulose Fluidity values

Unbleached cotton ~2

Bleached cotton <5

Degraded cotton showing loss in tensile strength > 10

standard unbleached viscose ~ 10

9.2.2.4 Physical testing

Tensile strength, bursting strength and abrasion resistance, Tear strength can be measured

The results are influenced by both fabric structure and chemical damage.

Tear strength is also influenced by residual natural lubricants.

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9.3. Mercerisation

9.3.1 Barium Activity Number (BAN)

Mercerized cotton fibre is highly absorptive. It absorbs more iodine, dyes, moisture and alkalis
and undergoes oxidation or hydrolysis at increased rates compared to unmercerized cotton.

BAN method is based on preferential absorption of barium hydroxide from its dilute solution by
mercerized cotton as compared to unmercerized cotton under the same conditions. Barium
activity number is determined by expressing this ratio as percentage.

Barium Activity Number of

✓
Unmercerized cotton - 100
✓
Semi-mercerized cotton - 115 to 130
✓ Completely mercerized cotton ~ 155

9.4 Heat Setting

Stresses are generated during drawing, spinning, weaving or knitting and finishing
processes by extension, twisting and bending forces.

Any subsequent heat treatment or washing produces stress relieving that shows up as
shrinkage or change of shape.

Hence, they become susceptible to dimensional instabilities

Fibre Yarn Fabric Garment manufacture introduce more

Instabilities

(This can result in high thermal shrinkage, permanent deformation etc.) Hence there is a need to
get rid of these instabilities this is called setting

Objective

To achieve the dimensional stability of a yarn or fabric containing thermoplastic fibres by

achievement of a desired stress-free form of the fibres making up a textile product.

For thermoplastic fibres – this is mostly done by heat energy aided by moisture and
tension

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 For natural fibres – this is generally done by chemical treatment aided by tension and
moisture

Higher than maximum application temperature expected in downstream processing

Example of heat setting by a hypothetical experiment of stress relaxation:

Suppose a textile fibre or yarn is stretched along OA and held in the extended form. If heat is
applied to the fibre for some time, the load drops to CB from CA. If yarn is now allowed to
recover by slowly removing the stress, it does not return to its original state. A permanent
residual deformation equal to OD is retained. In other words, heat was used to relieve the stresses
the yarn had built-up during stretching. The heat applied allows the yarn to relieve stresses; the
longer the treatment the better is stress relaxation and poorer the recovery.

9.4.1 Effect of tension on Properties

Free annealing (tensionless) – reduces molecular orientation and tenacity, increases fibre
diameter and denier

Tension annealing – increase in tenacity, crystallinity, no change in diameter/denier

9.4.2 Recommended setting temperatures

Different fibre types require different setting temperatures. Even within a given polymer, the
specific fibre type may require different setting temperature. For example, bulked or textured
polyester filaments are generally heat set at lower temperatures to maintain the bulk. Setting
temperatures used in the industry for various fibre types are given in the table below:

Table. Heat setting temperatures for different fibres

Setting
Fabric Temperatures
Woven and knit goods of textured polyester filament: 170–195 °C.
Fabrics of polyester filament: 185–220 °C.
Polyester (bulked yarn) 150 °C
Blends of polyester and cellulose fibres: 180–210 °C.
Wool blends 170 °C

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 Nylon 6.6 (filament) – woven 200–210 °C
Nylon 6,6 (filament) – knitted 220–225 °C
Nylon 6 (filament) 180–190 °C
Acrylics 140 °C
Tricel 190–210 °C

9.4.3 Effect of heat setting on fibre properties

As has been discussed earlier, heat setting can result in changes in fibre structure. Thus
crystallinty, crystal properties, orientation, etc. can be affected. These changes can affect certain
fibre properties like modulus, bending rigidity, shrinkage, etc. Since the dye uptake is a function
of overall crystallinity, it can also be affected.

9.4.4 Dimensional stability (Shrinkage)

Heat setting is essentially a disorientation process and results in the shrinkage of fiber/yarn. The
shrinkage is higher for higher heat setting temperature. In the figure given below the shrinkage of
a medium tenacity PET yarn is plotted as a function of heat setting temperature in hot air. The
shrinkage results in increase in elongation and lowering in breaking load. However, the residual
shrinkage after the heat setting process drops significantly. Thus, heat set fabrics have much
better dimensional stability as compared to unheat set fabrics. For this reason, synthetic fabrics
like PET are headset in grey state as shrinkage can take place during pretreatment and dyeing.
Not only unheatset fabrics tend to shrink by large amounts during dyeing, they also tend to
crease uncontrollably and the creases are very difficult to remove later.

The shrinkage of un-heateset polyester yarn is ~15% at 175o as compared to 1% for heatset fibres
at 220oC.

9.4.5 Crease recovery

One of the important objectives of heat setting is to reduce creasing of synthetic fabrics during
wet operations (wet creasing). Wet creasing reduces with increasing setting temperature.

100
9.4.6 Dyeing

Figure 11.12 shows typical dyeing behavior of a polyester fibre dyed without carrier and heat
set at various temperatures. It is interesting to note that initially the dyeuptake of the fibre
decreases with increasing setting temperature, reaches a lowest value around 160 to 180oC, and
then starts rising. At very high temperatures, it becomes higher than un-heatset fibre. The initial
decrease occurs due to increase in crystallinity of fibre. At high setting temperatures,
crystallites grow at the expense of smaller/imperfect crystals and become more perfect. This
results in increase in the amorphous volume per crystal. The path for dye diffusion becomes
less tortuous and dye absorption increases.

However, the practice of using very high setting temperatures for improving polyester
dyeuptake is not followed. The setting temperatures used for polyester generally result in a little
drop in dyeuptake as compared to un-heatset fibre. However, heat setting results in a uniform
dyeuptake, whereas non heat set polyester fabric absorbs dye in non-uniform way and chances
of obtaining unlevel dyeing increase. In table 1 below, typical temperatures used for heat setting
various fibres are given.

9.4.7 Pilling

The problem of pilling occurs due to entanglement of protruding fibres in a yarn. These loose

fibre convert to small fuzzy balls due to rubbing or abrasion. Generally singeing is a way of
dealing with this problem. In case of synthetic fibres heat setting can reduce pill formation.

During heat setting, the loose end of the protruding fibres shrink and get embedded more firmly
in the yarn structure. Reduction in the length of loose ends reduces the chance of pill formation.

EXCERSIZE 9

Part I: Discuss the following questions in detail

1. Discuss the assessment of desizing efficiency by Tegewa scale method.

2. What are the different methods of assessment of scouring efficiency?
3. Describe in brief the following methods of measurement of scouring efficiency.
a. Sinking test
b. Drop test

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 c. Determination of wax content
4. What do you mean by degradation of cotton in scouring and bleaching?
5. What is copper number?
6. What are the different methods of determination of degradation of cotton in
scouring and bleaching?
7. Discuss the measurement of degradation of cotton by methylene blue absorption
8. Discuss the measurement of degradation of cotton by cupraamonium fluidity
method.
9. What is fluidity?
10. What is barium activity number?
11. Describe the measurement of BAN for evaluating mercerizing efficiency.
12. What should be the barium activity number for properly mercerized cotton fabric?
13. What do you mean by heat setting of synthetic fibres?
14. Discuss the effect of heat setting on shrinkage of fabric.
15. Describe the effect of heat settinh on dyeability of the polyester.
16. What is the heat setting temperatures of Polyester and Nylon?

Part II: Fill the blanks with the appropriate choice given below
1. Desizing of cotton is assessed by …….
c. Absorbency b. Tegawa scale c. Sinking d. BAN
2. Scouring efficiency of cotton scouring is evaluated by ………..
a. Absorbency b. Tegawa scale c. Sinking d. BAN
3. Singeing efficiency is measured by ………..test.
a. absorbency b. pilling c. tensile strength d. sinking
4. Mercerisation efficiency is evaluated by determination of ………
a. Barium activity number b. ash content of fabric
c. Wax content of fabric d. crease recovery angle
5. Desizing efficiency with Tegewa scale is measured on ……. Scale
a. 1-5 b. 1-8 c. 1-9 d. 1-10

102
REFERENCES
1. Chemical Technology in the pre-treatment process of textiles, S R Karmakar, 1999, Elsevier
Science.
2. http://www.osthoff-senge.com/en/vibra_plus.html
3. Gebert K Textile auxiliaries in Ullmann’s Fibres, Volume 2, Textile and Dyeing
Technologies, High Performance and Optical Fibres, Wiley VCH, 2008, Weinheim
Dickinson K, Oxidative desizing, Rev. Prog. Coloratlon, 17, 1987, 1
4. Shenai V A, Sizing and desizing in Technology of Textile Processing Vol III, Technology of
Bleaching and Mercerizing, Sevak Publications, 1996
5. Surface active agents in Chemical Technology in the pre-treatment process of textiles, S R
Karmakar, 1999, Elsevier Science.
6. Shenai V A, Sizing and desizing in Technology of Textile Processing Vol III, Technology of
Bleaching and Mercerizing, Sevak Publications, 1996
7. Analysis and Testing in Preparatory Processes in Chemical Technology in the pre-treatment
process of textiles, S R Karmakar, 1999, Elsevier Science.
8. Handbook of Fibre Science and Technology- Volume I: Chemical Properties of fibers and
fabrics fundamentals and preparation Part-A. ed. Menachem Lewin and Stephen B-Sello.
Marcel Dekker Inc., 1984, New York.
9. Cellulose-model films and the fundamental approach. Eero Kontturi, Tekla Tammelin,
Monika Osterberg, Chemical Society Reviews, 35(12):1287-304: 2007
10. https://www.converteraccessory.com/products/wrinkle/news.php
11. E. S. Olson, Textile Wet Processes,Vol I, Noyes Pub., Park Ridge, New Jersey, USA
(1983) p 153.
12. John Shore, Fluorescent brightening agents, Colorants and auxiliaries, Organic Chemistry
and Application Properties, Volume 2 – Auxiliaries, Ed.John Shore, Society of Dyers and
Colourists, 2002, Bradford
13. Preparatory Processes I in Textile preparation and dyeing, A K Roychoudhary, 2006,
Oxford and IBH
14. M L Gulrajani, Degumming Of Silk, Rev. Prog. Coloration, 22, 1992, 79
15. Leslie Miles, Drying and setting in Textile Finishing, Ed. Derek Heywood, Society of
Dyers and Colourists, Bradford, 2003
16. A K Sengupta, Heat setting in Lecture notes, Synthetic Fibres, Manufacture, Processing
and applications, Department of Textile technology, IIT Delhi, New Delhi

103
 PART II: FINISHING TECHNOLOGY
CHAPTER ONE

MECHANICAL AND CHEMICAL FINISHES

1.1 Introduction to Finishing

Finishing is the finish that fits the fabric for its purpose, or it is ultimate value addition done to the fabric.
A dyed, washed-off and dried fabric is seldom an immediately saleable product. Additional processing is
required to give the fabric and the garment made from it customer appeal. All finishing processes are
designed to increase the attractiveness or serviceability of the textile product. Finishing treatments are
basically meant to give the textile material certain desirable properties like

❖ Softness
❖ Luster
❖ Pleasant handle
❖ Drape
❖ Dimensional stability
❖ Nonslip soil release
❖ Crease recovery

1.2 Classification of finishing

1.2.1 According to the nature of Finish

Physical or Mechanical finish: It involves specific physical treatment to a fabric surface to

cause a change in the fabric appearance involving the application of physical principles
such as friction, temperature, pressure, tension and many others. Also known as dry
finish. Compacting/ shrink

I. proofing/Calendaring, Raising/napping, sueding/Polishing, Shearing, raising (Napping, Sueding),

Decating etc. are physical or mechanical finish.
II. Chemical finish: Chemicals are used followed curing and drying involving the application of
synthesis or natural chemical products, which bind to the fibres more or less permanently. Also
known as wet finish.

104
III. Combined mechanical and chemical: Involving the application of both chemical and mechanical
processes.
1.2.2 Classification according to degree of permanence

Based on degree of permanence finishing can be classified permanent finish, durable finish, semi
– durable finish and temporary finish. Permanent finish usually involves a chemical change in
fiber structure and do not change or alter throughout the life of the fabric. Durable finish: usually
last through the life of the article effectiveness becomes diminished after each cleaning Last near
the end of the normal use life of the article, the finish is nearly removed. Semi durable finish;
lasts through several laundering. Temporary finish are removed or substantially diminished the
first time the article is cleaned

1.2.3 Classification according to performance

Aesthetic finish: These finishes modify the appearance and /or hand or drape of the fabric.
Calendaring, fulling, mercerization, napping or sueding, shearing, softening, stiffness, etc.

Functional finish: These finishes improve the performance properties of the fabric, crease
resistant, flame resistant, Soil release, Waterproof etc. are some of functional finishes.

1.3 Mechanical Finishing

Mechanical Finishing is defined as any operation performed to improve fabric appearance or

function by physical manipulation. Steam or water may accompany the physical manipulation;
however, chemicals other than lubricants are seldom used.

Fabric luster, smoothness, softness, residual shrinkage, and hand are examples of the properties
that can be altered by mechanical finishing. Topics to be covered in this finishing are:
Compacting (Shrink proofing), Calendaring, raising (Napping, Sueding), Shearing, Polishing,
Corduroy Cutting, Decating.

1.3.1 Calendaring

A process of passing cloth between rollers (or "calendars"), usually under carefully controlled
heat and pressure, to produce a variety of surface textures or effects in fabric such as compact,
smooth, supple, flat and glazed. The process involves passing fabric through a calendar in which

105
a highly polished, usually heated, steel bowl rotates at a higher surface speed than the softer (e.g.
cotton or paper packed) bowl against

which it works, thus producing a glaze on the face of the fabric that is in contact with the steel
bowl. The friction ratio is the ratio of the peripheral speed of the faster steel bowl to that of the
slower bowl and is normally in the range 1.5 to 3.0.

The normal woven fabric surface is not flat, particularly in ordinary quality plain weave fabrics,
because of the round shape of the yarns, and interlacing's of warp and weft at right angles to each
other. In such fabrics it is more often seen that even when the fabric is quite regular, it is not flat.
During calendaring, the yarns in the fabric are squashed into a flattened elliptical shape; the
intersections are made to close-up between the yarns. This causes the fabric surface to become
flat and compact. The improved planeness of surface in turn improves the glaze of the fabric.
The calendar machines may have several rollers, some of which can be heated and varied in
speed, so that in addition to pressure a polishing action can be exerted to increase luster.

1.3.2 Compacting

Durable finish imparted on man-made fibres and knitted fabrics by employing heat and pressure
to shrink them to produce a creepy and bulky texture.

1.3.3 Embossing

This calendaring process allows engraving a simple pattern on the fabric. To produce a pattern in
relief by passing fabric through a calendar in which a heated metal bowl engraved with the
pattern works against a relatively soft bowl, built up of compressed paper or cotton on a metal
center.

1.3.4 Sueding

This process is carried out by means of a roller coated with abrasive material. The fabric has a
much softer hand and an improved insulating effect thanks to the fibre end pulled out of the
fabric surface.

106
1.3.5 Raising or Napping

The raising of the fibre on the face of the goods by means of teasels or rollers covered with card
clothing (steel wires) that are about one inch in height. Action by either method raises the
protruding fibres and causes the finished fabric to provide greater warmth to the wearer, makes
the cloth more compact, causes the fabric to become softer in hand or smoother in feel; increase
durability and covers the minute areas between the interlacing's of the warp and the filling.
Napped fabrics include blankets, flannel, unfinished worsted, and several types of coatings and
some dress goods. Other names for napping are Gigging, Genapping, Teaseled,

Raised

1.3.6 Sanforizer

Mechanical compacting is one method of reducing residual shrinkage. The process forces yarn
closer together and the fabric becomes thicker and heavier. Sanforizing is used to describe shrink
proofing processes. Sanforizing is a process whereby the fabric is run through a sanforizer; a
machine that has drums filled with hot steam. This process is done to control the shrinkage of the
fabric. The fabric is given an optimum dimensional stability by applying mechanic forces and
water vapour.

1.3.7 Stentering

Stentering is a mechanical finishing process of textile. It is done for the stretching of fabric by
the stenter machine. In other words, we can say Stentering is done for gripping the edges of a
moving web to support the web during heating and stretching operation.

107
1.4 Chemical Finishing

Chemical finishing refers to the use of chemicals to achieve a desired end-use property.
Processes that change the chemical composition of the fibers OR improve the surface
characteristics. Can be applied in yarn, fabric, and garment stages/form. It can be durable or
on durable based on resistance to laundering. Chemical finish is solution or emulsion of
active chemical in water. It is known as wet finishing.

1.4.1 Methods of Application

Exhaust and pad-dry-cure the application methods of chemical finishing. pad-dry-cure most
widely used. Chemicals that have strong affinities for fiber surfaces can be applied in
batch/discontinuous processes by exhaustion. Chemicals that have low/no affinity for fibers
are applied by continuous processes that involve padding with chemical solution, squeezing,
drying, and curing for fixation.

1.4.1.1 Pad application of chemicals

By passing fabric through chemical finish solution by ‘wet on dry’ or wet on wet process.
Factors affecting wet pick up are Fiber, yarn and fabric characteristics, machine settings [e.g.
squeeze pressure] and solution properties [Viscosity, surface tension]. High wet pickups are
70–100 % in padding techniques.

figure 1: 1 pad-dry-cure and application method.

For consistent chemical application: Ip pressure should be uniform across the fabric width,
Solution level & temperature in pad should be constant, Fabric speed should not vary
throughout the application.

108
1.4.1.2 Concentration relationships

In batch processes, the amount of chemical finish to be applied is usually expressed. as a

weight percentage based on the original fabric weight. This relationship is often abbreviated
as % owf (percent on weight of fabric) or % owg (percent on weight of goods) as seen in
Equation 1:

Equation 1

For example, if a softener is to be applied at 3 % o.w.f to 500 kg of fabric, then 15 kg of

softener will be used (3 % of 500 kg). It must be recognised that since nearly all chemical
finishes are provided as an aqueous solution or emulsion, a knowledge of the actual solids
concentration of the supplied chemical is needed to determine the actual increase in fabric
weight after drying.

If the solids concentration is not known or provided, it can be determined by careful

evaporation at moderate temperature followed by weighing the residual. In continuous
processes where a chemical solution or emulsion is applied to a fabric, the amount of
chemical applied to the fabric depends on the amount of finishing solution applied, the
concentration of the supplied chemical in the finishing solution or emulsion and the solids or
active compound concentration of the supplied chemical. The amount of finishing solution or
emulsion applied is referred to as the ‘wet pickup’ (wpu) of the fabric and is usually
expressed as a percentage on the weight of the dry untreated fabric (Equation 2):

Equation 2

To determine the amount of supplied chemical added to the fabric, the ‘% add-on’ is given by
Equation 3

Equation 3

where % conc is the concentration of the finishing chemical in the applied solution or
emulsion expressed as percentage by weight. Since most finishing formulas are given in
terms of grams per liter (g/l), Equation 4 can be used to convert the g/l concentration to
weight percent:

Equation 4

where the density is the applied solution or emulsion density.

109
1.4.1.3 Pad application of chemicals to dry fabric

Chemical finishes are often pad applied to dyed or printed fabrics after a drying step. In this
situation, dry fabric is passed through the chemical finish solution and the process is called a
‘wet on dry’ process. The wet pickup of a chemical solution in a pad mangle is influenced by
many factors such as fabric characteristics, machine settings and solution or emulsion
properties.

In order to obtain consistent chemical application, the nip pressure should be uniform across
the fabric width, the solution level and temperature in the pad should be constant and the
fabric speed should not vary throughout the application process.

Equation 4

where fabric mass flow is defined as: fabric mass flow = fabric speed (m min–1) × fabric
linear density (kg m–1)

In practice, however, it is more common to maintain a constant level in a wet on dry

pad application with a float valve controlling the liquid level.

1.4.1.4 Pad application of chemicals to wet fabric

To avoid the costs of a drying step after dyeing, chemical finishes are often pad applied to
wet fabric in a process called ‘wet-on-wet’. In this case, the wet pickup of the fabric exiting
the pad must be maintained at a higher level than that of the incoming fabric, usually at least
15–20 % higher. An additional complication is the fact that water entering the pad on the
incoming fabric can interchange with the finishing solution, in effect diluting the
concentration of the components and causing tailing of the finish effect. Therefore, a
chemical feed more concentrated than the pad solution must be employed.

In order to determine the pad solution or emulsion concentration of the finishing chemicals,
an effective percentage wet pickup, wpueff, is calculated from Equation 5:

wpueff = (wpu0 – wpui ) + wpui × f Equation 5

where wpu0 is the percentage wet pickup of the fabric exiting the pad, wpui is the percentage
wet pickup of the fabric entering the pad and f is the interchange factor,a measure of
interaction between incoming water and the pad solution, that can vary from 0 to 1 depending
on fabric and machine parameters. Typically, f is between 0.7 and 0.8. An initial interchange
factor is assumed and then corrected, if necessary, based on analysis of the treated fabric.

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1.4.1.5 Low wet pickup methods

Typically, pad applications of chemical finishes yield wet pickups in the 70–100 % range.
These high pickups necessarily require the removal of large amounts of water during drying.
The evaporation of this water can lead to uneven finish distribution in the dried textile owing
to migration of the finish to the fabric surface during drying.

The high rate of evaporation at the fabric surface leads to movement of the finish solution
from the wet fabric interior to the drier fabric exterior resulting in a higher concentration of
the finish at the fabric surfaces with a corresponding lower concentration in the fabric interior
regions. This migration is reduced as the finish solution becomes more and more
concentrated and viscous as drying progresses. Therefore, reducing the amount of water
initially applied will tend to reduce finish migration.

The critical application value (CAV) is defined as the minimum amount of durable press
finish liquid that can be applied to a given cotton fabric without producing a non-uniform
distribution of crosslinks after drying and curing.

There are two main types of low wet pickup applicators. The first is the saturation–removal
type where the fabric is completely saturated with the finish liquid and then the excess liquid
is removed mechanically or with a vacuum before drying for example Vacuum extraction,
porous bowl techniques, Air-jet ejectors etc.

Transfer padding (squeeze–suck technique). With the second type, a precise amount of finish
liquid is uniformly applied to the fabric using Kiss-roll, Loop transfer system, Engraved roll,
Nip padding system, Spray system and Foam application.

Exercise 1
Answer the following questions by choosing the best alternatives.
1. Which of the following is not a desirable property achieved by finishing treatments?
A) Softness B) Luster C) Spinnability D) Dimensional stability
2. Which of the following is a physical or mechanical finish?
A) Mercerization B) Soil release C) Sueding D) Flame resistance
3. A permanent finish is;
A) A finish that lasts through several launderings
B) A finish that is removed or substantially diminished the first time the article is cleaned
C) A finish that involves a chemical change in fiber structure and does not change or alter
throughout the life of the fabric

111
D) A finish that lasts near the end of the normal use life of the article and is nearly removed
4. An aesthetic finish is;
A) A finish that modifies the appearance and/or hand or drape of the fabric
B) A finish that improves the performance properties of the fabric
C) A finish that involves a chemical change in fiber structure and does not change or alter
throughout the life of the fabric
D) A finish that lasts near the end of the normal use life of the article and is nearly removed
5. What is mechanical finishing?
A) A finishing process that involves the use of chemicals
B) A finishing process that involves the use of physical manipulation without the use of
chemicals
C) A finishing process that involves both physical manipulation and the use of chemicals
D) A finishing process that involves the application of synthesis or natural chemical products,
which bind to the fibers more or less permanently
6. Which of the following is a physical or mechanical finish?
A) Crease-resistant B) Flame-resistant C) Waterproof D) Raising/napping
7. Calendaring is;
A) A process of adding color to the fabric B) A process of preparing fabric for sale
C) A process of passing cloth between rollers to produce a variety of surface textures or
effects in fabric D) A process of removing stains from fabric
8. Which of the following is NOT a desirable property that can be achieved through
finishing?
9. What is chemical finishing?
a) It is a mechanical finishing process
b) It is a process of applying chemicals to achieve desired end-use properties
c) It is a process of applying heat to achieve desired end-use properties
d) It is a process of applying dye to achieve desired end-use properties
10. _______are the stages/forms in which chemical finishing can be applied?
a) Fabric stage only b) Yarn stage only c) Garment stage only d) All of the above
11. Wet finishing involves;
a) Uses of chemicals to achieve a desired end-use property
b) Uses of water to achieve a desired end-use property
c) Uses of heat to achieve a desired end-use property
d) Uses of mechanical force to achieve a desired end-use property

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 12. _________ is the most widely used application method of chemical finishing.
a) Exhaust method b) Continuous method c) Pad-dry-cure method d) Batch method
13. What are the factors affecting the wet pick up in pad application techniques?
a) Fiber, yarn, and fabric characteristics
b) Solution properties (viscosity, surface tension)
c) Machine settings (squeeze pressure)
d) All of the above
14. What wet pickup range is achieved in high wet pickups in padding techniques?
a) 10-20% b) 30-40% c) 50-60% d) 70-100%
15. What is the main requirement for consistent chemical application in pad-dry-cure
method?
a) Solution level and temperature in pad should be constant
b) Fabric speed should not vary throughout the application
c) Nip pressure should be uniform across the fabric width
d) All of the above
16. How is the actual solids concentration of supplied chemicals determined in batch
processes?
a) By weighing the residual after careful evaporation at moderate temperature
b) By measuring the density of the supplied chemical
c) By measuring the viscosity of the supplied chemical
d) None of the above
17. What is the amount of supplied chemical added to the fabric dependent on in
continuous processes?
a) The amount of finishing solution applied
b) The concentration of the supplied chemical in the finishing solution or emulsion
c) The solids or active compound concentration of the supplied chemical
d) All of the above

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 CHAPTER TWO

DURABLE-PRESS FINISHES

2.1 Theory of Wrinkling

Cellulose fibres and especially cotton is still the most important kind of fibres, because of
their numerous advantages. One of their main disadvantages, wrinkling after washing is
overcome by a very important and special kind of finish. It is difficult to find the one best
term to describe this class of finishes. Some of the words and phrases that have been used in
the past include easy-care, minimum care, easy-to-iron, no-iron, wash, and wear, crease
resistant, durable press, permanent press, shrink proof, wrinkle resistant and wrinkle free. In
fact, all these terms do describe some important performance features of these multi-talented
finishes. In this module, the terms ‘easy-care’ and ‘durable press’ will be used preferably.

Easy-care and durable press finishes are generally applied to cellulose and cellulose blend
fabrics, but other fibres can benefit from these finishes also. The primary effects of the easy-
care and durable press finish on cellulosic fibres are reduction in swelling and shrinkage,
improved wet and dry wrinkle recovery, smoothness of appearance after drying, and retention
of intentional creases and pleats. The total crease recovery angle (CRA), that is the sum of
the crease recovery angles of the warp and the fill directions of the fabric, increases from
about 150° to about 300°.

A fabric shrinkage of less than 5 % can usually be achieved. An unavoidable side effect of
the cellulosic cross-linking finishes is a reduction in the elasticity and flexibility of the
cellulose fibers. This produces a considerable decrease in abrasion resistance and tear and
tensile strengths on natural cellulose fibers. A rule of thumb states that an increase in the
wrinkle recovery angle of 10° corresponds to a loss in abrasion and tear strength of about 7 %
in cotton fabric. The dry tear strength of regenerated cellulose fibers decreases only slightly
with a cross-linking finish, but the wet tear strength increases because of the strongly reduced
swelling.

2.2 Mechanisms of easy-care and durable press finishing

The primary cause of the shrinkage of cellulosic fibres is the fact that these fibres can readily
absorb moisture. This absorbed moisture facilitates internal polymer chain movements in the
amorphous fibre areas by lubrication. It disrupts the internal hydrogen bonding between these

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polymer chains. When a moisture laden cellulosic fibre is stressed, the internal polymer
chains of the amorphous areas are free to move to relieve that stress.

Hydrogen bonds can reform between the polymer chains in their shifted positions, in effect
locking in the new configuration. With no restoring forces available, a newly formed wrinkle
or crease will remain until additional processes (ironing for example) apply adequate
moisture and mechanical forces to overcome the internal forces. The swelling of cellulosic
fibres by moisture can be reduced by the application of self-crosslinking urea or melamine
products as well as by products that mainly crosslink with cellulose molecules. Without such
a crosslinking finish, cellulose fibres can take up more than 10 % of their weight in water. As
the fibres swell, the fabric must crease and shrink to relieve the internal stresses caused by the
swelling.

The new arrangement of the cellulose molecules in the swollen form of the fibre is fixed by
newly formed hydrogen bonds between adjacent cellulose molecules, mostly in the
amorphous fibre area. Therefore, the uneven and wrinkled appearance of the cellulose fabric
remains after drying, in contrast to fabrics made of nonswelling synthetic fibres. Two
different chemical approaches have been used commercially to produce non-swelling or
durable press cellulose fabrics.

➢ incorporation of a polymerised finish in the pores of the fibres, so that water molecules cannot
easily penetrate the fibre.
➢ The reaction of multifunctional crosslinking agents with the hydroxyl groups of adjacent
cellulose molecules that hinder the swelling of the cellulose fibre

2.3 Examples of textiles with easy-care and durable press finishes

Easy-care and durable press finishes are applied to cellulose fabrics and fabric blends with
high cellulose content that are laundered, and which should maintain a smooth, ‘just ironed’
appearance through the lifetime of the article. These include shirts, blouses, trousers, work
clothes, lining fabrics, suits, formal wear and overcoats. Although wrinkles and creases are
not as severe a problem with knitted fabrics, easy-care finishes are also useful in providing
dimensional stability to knitted fabrics.

Pile fabric for clothes and upholstery can achieve a better appearance and resilience of the
pile, in addition to the shrink and creaseproof effects. This easy-care finish is also used for
table and bed linen because the wrinkling of linen after washing is very marked. One special

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use of the cellulose crosslinking finishes are wash permanent chintz articles, produced by the
heat and high pressure of calendering the impregnated fabrics

2.4 Chemistry of easy-care and durable press finishes

2.4.1 Formaldehyde-containing products

Urea–formaldehyde (U/F) products are readily synthesised from water solutions of urea and
formaldehyde at pH 7.5–9. The resulting N,N'-dimethylol urea (DMU) is often modified by
further reaction at pH 8–9 with methanol to the more stable and liquid dimethylether of DMU
(dimethoxymethyl urea). These reactions are equilibrium reactions with significant
concentrations of the starting compounds. These equilibria are the reasons for the high
content of free and easily released formaldehyde found with U/F products. Because of their
high reactivity, unmodified U/F finish baths must be used within a few hours. The high
stiffness and firmness of the U/F finish can be important for rayon fabrics which often are
considered too limp when compared with cotton. The U/F finish gives the best elastic
resilience.

Figure 2: 1 Dimethylol urea reactions.

The main properties of U/F products are:

➢ DMU is highly reactive; finish baths must be used in a few hours.

➢ Low stability to hydrolysis, low durability to laundering.
➢ High chlorine retention
➢ High content and release of formaldehyde
➢ Very high elastic resilience

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 Figure 2: 2 Melamine–formaldehyde reactions.

Melamine–formaldehyde (M/F) products have mostly three to six reactive N-methylol groups
connected to one melamine ring. This leads to a higher crosslinking and an easy-care finish
with better wash fastnesses. Their synthesis is like the U/F products, providing tri- to
hexamethylol melamine (TMM, HMM) and their methyl ethers (tri- or hexamethoxymethyl
melamine). TMM is preferred for the easy-care finish, often only as a component of a product

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mixture to give a better permanence of the effects. HMM finds additional uses in pigment
binders and Basofil fibres

The main properties of M/F products are:

➢ Better stability to hydrolysis and better washing durability than U/F products
➢ Relatively high formaldehyde content and release
➢ Fewer problems with chlorine retention than U/F products
➢ More dimensional stability and stiffness (also for nylon and polyester).

The predominant reaction of U/F and M/F products is their self-condensation to three-
dimensional resin structures. These structures impart a very stiff, firm handle to fabrics
treated with U/F and M/F products. The self-condensation is caused by the active hydrogen
atom attached to the nitrogen of the N-methylol group. If this active hydrogen atom is
substituted by a carbon atom in a ring structure, as in ethylene urea, the reaction with the
hydroxyl groups of cellulose becomes dominant. Crosslinking of neighbouring cellulose
molecules is then the main reaction, especially activated by inductive effects of the hydroxyl
groups in the dihydroxyethylene urea heterocycle (DHEU).

N,N'-Dimethylol-4,5-dihydroxyethylene urea (DMDHEU) is the chemical basis of about 90

% of the easy-care and durable press finish products on the market. DMDHEU is synthesised
from urea, glyoxal and formaldehyde. It is less reactive than DMU and TMM and therefore
requires more active catalysts. However, finish baths containing DMDHEU are more stable
than finish baths with DMU or TMM. The reactivity of DMDHEU can be further reduced by
reaction with methanol or diethylene glycol, leading to ether modified DMDHEU products.
These alcohols are also formaldehyde scavengers and are often added to commercial finish
products for that purpose.

A typical DMDHEU commercial product is made from about 45 % DMDHEU, 9 %

diethylene glycol and 2 % methanol. This product could contain less than 0.3 % free
formaldehyde. there are two ways to incorporate diethylene glycol into these products.

a) simple mixture of the glycol and DMDHEU

b) reacting the glycol with DMDHEU to form a glycolated product.

Both products perform similarly and both types are available in the marketplace and are
referred to as ‘ultra-low formaldehyde’ (ULF) with less than 50 ppm released formaldehyde.

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Figure 2: 3 Self-condensation reactions of U/F and M/F products.

Figure 2: 4 Synthesis of DMDHEU.

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 Figure 2: 5 Crosslinking of cellulose with DMDHEU products.

The main properties of DMDHEU-based products are:

➢ Low to very low reactivity (when ether modified)

➢ Excellent durability to laundering.
➢ Low chlorine retention
➢ Medium to very low formaldehyde release (Table 5.4)
➢ The most commonly used durable press products.
2.4.2 Formaldehyde considerations

There are several aspects to the ‘formaldehyde problem’. Formaldehyde is not only a very
useful and inexpensive chemical compound but also a natural product. Traces of
formaldehyde are present in air, fruits, vegetables, wood, and in blood. Every incomplete
burning process, including cigarette smoking, produces formaldehyde. It does not build up in
the environment because oxygen in the air reacts with it to form formic acid. More than 1
ppm of formaldehyde in the air causes a pungent odour. Formaldehyde irritates mucous
membranes, causes teary eyes, induces cough, and can lead to difficulties in breathing and
headaches.

Skin contacts with aqueous solutions of formaldehyde or with textiles that contain a high
level of formaldehyde can give rise to eczema and occasional allergic reactions. In addition,
formaldehyde is a suspected human carcinogen. The most severe problems with

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formaldehyde and textiles occurred in the cut and sew industries before the introduction of
DMDHEU. In normal usage, when clothing is periodically laundered, there are no
formaldehyde-related problems. However, it is advisable to wash durable press treated
textiles before their first use. Several countries have enacted laws designating concentration
limits for formaldehyde in the workplace.

2.4.3 non-formaldehyde containing products.

N,N'-Dimethyl- 4,5-dihydroxyethylene urea (DMeDHEU)should not be confused with

DMDHEU. DMeDHEU does not contain formaldehyde. It is synthesized from the relatively
expensive N,N'-dimethyl urea and gloxal and is often referred to as DMUG (dimethylurea
glyoxalate) or DHDMI, derived from the name dihydroxy dimethyl-2-imidazolidinone. Like
DMDHEU, it can be modified by reaction with alcohols such as methanol, diethylene glycol
or 1,6-hexanediol to ether derivatives. The crosslinking reaction with cellulose is shown in
below figure.

DMeDHEU costs about twice as much as DMDHEU and to achieve comparable easy-care
and durable press effects to DMDHEU, nearly twice the amount of DMeDHEU is needed.
This poor cost performance ratio is one reason for the relatively small market penetration by
this formaldehyde-free finish. Another reason is that a completely formaldehyde-free finish is
not as commercially important since the advent of the ultra-low formaldehyde products.
However, a 1:1 mixture of DMDHEU and DMeDHEU is popular because of its reduced
formaldehyde levels with only slightly inferior physical properties at an acceptable cost.

The main properties of DMeDHEU products are:

➢ Formaldehyde free
➢ Very low reactivity
➢ Very low chlorine retention
➢ Limited durability to laundering.
➢ Yellowing effect when not ether modified.
➢ Price/effect ratio nearly 4:1 compared with DMDHEU.
➢ Development of unpleasant odours, depending on the product formulation.

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 Figure 2: 6 Crosslinking of cellulose with DMeDHEU.

1,2,3,4-Butanetetracarboxylic acid (BTCA) and similar polycarboxylic acids provide an

alternative possibility for a formaldehyde-free crease-resistant finish. The activation
mechanism of BTCA and the reaction with cellulose are shown in below fig. BTCA gives
rise to good crease recovery but with limited laundering durability owing to hydrolysis of the
ester bonds to cellulose. These polycarboxylic acids are relatively expensive, comparable in
cost to DMeDHEU. In addition, the reactions of these acids with cellulose require large
amounts of sodium hypophosphite as a catalyst. Recently, polyacrylic acid-based products,
for example maleic acid anhydride copolymers, have been introduced that provide similar
properties to BTCA finishes but at a more economical price.

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 Figure 2: 7 Crosslinking of cellulose with BTCA.

Novel cellulosic crosslinking agents with interesting properties are gained by molecular
incorporation of the phosphorus catalyst in the BTCA structure. These formaldehyde-free
phosphono- and phosphinocarboxylic acids (APCM, modified polycarboxylic acids) show
good crosslinking properties with minimal strength losses, no shade changes and good
durability for up to 20 washing cycles. The APCM products are liquid, water soluble and
neither toxic nor skin irritating.

2.5 Application methods

The most common application method for easy-care and durable press finishes is a pad–dry–
cure procedure. If the finish is cured immediately after drying, while the fabric is still in an
open width configuration, the finish is referred to as a ‘pre-cure’ finish, the finish is cured
prior to garment manufacture. Textiles with a pre-cure finish are most suited for fabrics and
apparel that require wrinkle resistance, such as sheeting, shirting, and casual trousers. For
fabrics that require crease retention, such as trousers and pleated skirts, the durable press
finish is only dried by the fabric manufacturer and cured after the garment has been made and
creased appropriately. This finish is referred to a ‘postcure’ finish or ‘delay cure’ finish, the
finish is cured after the garment has been manufactured. In the special cases where entire
garments are to be treated with a durable press finish, the finishing chemicals can be sprayed
in exact doses onto the garments before the final shape is formed and then cured.

In general, The easy-care and durable press finishes are usually applied by the following
methods:

➢ Pad-dry-cure (precure method)

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 ➢ Pad-dry-making of garment-curing of garment (‘postcure’ or ‘delay cure’ method)
➢ Spraying of garment
➢ Impregnation/dipping of garment—centrifugation-drying-pressing or ironing

Comparison of finish application methods

2.6 Compatibility with other finishes

In commercial use, easy-care and durable press finishes are frequently combined with other
finishes to provide additional properties such as water and oil repellency, flame retardancy,
soil release and the like. Often the combination of another finish with the cellulose
crosslinking finish will result in a more durable effect from the first finish. Combination with
pigment printing is very common because of similar chemistry to cellulose crosslinking
agents and binders and the similar application conditions.

2.7 Formaldehyde testing

The presence of formaldehyde in fabrics can be measured qualitatively as follows: A small

piece of fabric is added to 2–3mL of a solution of 10mg chromotropic acid per 100mL of
72% sulphuric acid. Warm the solution carefully to not more than 100°C for 1min. A red to
violet colour in the solution indicates the presence of formaldehyde.

Quantitative test in air : This is most conveniently done with test tubes designed for this
purpose. A colour change to a certain mark after a specified amount of air is drawn through
the tube gives the formaldehyde concentration. following two methods are used for
determining formaldehyde levels in resin-treated fabric in British finishing industry:

British Standard BS 6806.

Japanese Law 11

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Exercise 2

Answer the following questions by choosing the best alternatives.

1. What is the primary cause of the shrinkage of cellulosic fibers?

a) Lack of crosslinking agents b) Internal hydrogen bonding between polymer chains
c) Absorption of moisture d) Lack of abrasion resistance
2. What is the effect of easy-care and durable press finishes on cellulosic fibers?
a) Decrease in abrasion resistance b) Increase in swelling and
shrinkage
c) Reduction in smoothness of appearance after drying d) Improvement in wet and dry
wrinkle recovery
3. What is the main disadvantage of cotton and cellulose fibers?
a) Lack of durability b) Lack of elasticity c) Wrinkling after washing d) Absorption of
moisture
4. What is the chemistry behind easy-care and durable press finishes?
a) Incorporation of a polymerized finish in the pores of the fibers
b) Reaction of multifunctional crosslinking agents with hydroxyl groups of adjacent cellulose
molecules c) Both a and b d) None of the above
5. What is the rule of thumb regarding the relationship between wrinkle recovery angle
and abrasion and tear strength in cotton fabric?
a) An increase in the wrinkle recovery angle of 1° corresponds to a loss in abrasion and tear
strength of about 1%
b) An increase in the wrinkle recovery angle of 10° corresponds to a loss in abrasion and tear
strength of about 7%
c) An increase in the wrinkle recovery angle of 15° corresponds to a loss in abrasion and tear
strength of about 10%
6. What is the effect of cross-linking finishes on the abrasion and tear strength of natural
cellulose fibers?
a) No effect b) Decrease in abrasion resistance and tear and tensile strengths
c) Increase in abrasion resistance and tear and tensile strengths
d) Decrease in tear strength but increase in wet tear strength
7. Which of the following fibers can benefit from easy-care and durable press finishes?
a) Only cellulose and cellulose blend fabrics b) Only synthetic fibers
c) Only wool and wool blend fabrics d) All kinds of fabrics
8. ___________ is the goal of applying easy-care and durable press finishes to textiles?

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a) To increase the wrinkling of fabrics after washing
b) To reduce the shrinkage of fabrics after washing
c) To reduce the smoothness of appearance of fabrics after drying
d) To increase the elasticity of fabrics
9. Which of the following textiles can benefit from easy-care finishes?
a) Only knitted fabrics b) Only pile fabric for clothes and upholstery
c) Only formal wear and overcoats d) Shirts,
10. Which type of finish is suitable for fabrics that require crease retention?
a) Pre-cure finish b) Delay cure finish c) post-cure finish d) Spray finish
11. Which finish is commonly combined with easy-care and durable press finishes to
provide additional properties such as water and oil repellency?
a) Pigment printing b) Formaldehyde testing c) Flame retardancy d) Soil release
12. How can the presence of formaldehyde in fabrics be measured qualitatively?
a) By adding a small piece of fabric to a chromotropic acid solution
b) By drawing air through a test tube
c) By spraying a formaldehyde solution onto the fabric
d) By impregnating/dipping the garment in a formaldehyde solution

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 CHAPTER THREE

REPELLENT FINISHES

3.1 Introduction

Finishes that repel water, oil and dry dirt are important in all parts of the textile market for
clothing, home, and technical textiles. Finishes that repel water, oil, dirt etc. are called
repellent finish. The followings are some of the repellent finishes.

Stain Repellency

Stain Repellency is the ability of a treated fabric to withstand penetration of liquid soils
under static conditions involving only the weight of the drop and capillary forces.

Oil Repellency

Oil Repellency is tested by placing a drop of oil on the fabric and observing whether the drop
resides on top the fabric or whether it penetrates. A homologous series of hydrocarbons
decreasing in surface tension is used to rate the fabric's oil repellency. The hydrocarbon with
the lowest surface tension to remain on top and not penetrate is indicative of the fabric's
repellency. The lower the surface tension of the liquid, the better the fabric's resistance to oily
stains.

Water Repellency

Water Repellency: Water repellent fabrics are those which resist being wetted by water;
water drops will roll off the fabric. Water repellency is achieved using different product
groups, but oil repellency is attained only with fluorocarbon polymers. The purpose of water
repellent finish is that the drops of water should not spread on the surface of the textile and
should not wet the fabric. Water repellency of a fabric depends on several factors including
nature of the fibers, yarn structure, fabric porosity, finish applied and water impact force.
Any residual sizing agents or surfactants present on the fabric can damage the repellency
properties. Repellent finishes are usually compatible with easy-care and durable press
finishes, as well as many softeners.

It is important to distinguish between water-repellent and water-proof fabrics. water

repellency is taken to be ‘the relative degree of resistance of a fabric to surface wetting, water
penetration, water absorption or any combination of these properties. Water Repellent Fabrics
have open pores and are permeable to air and water vapor. The term ‘waterproof’ is normally
used to represent the conditions where a textile material can prevent the absorption and

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penetration of water into its structure. Thus, a waterproof surface provides a barrier to water
under all practical end-use conditions.

3.2 Theory of wetting

Wetting is the ability of a liquid to maintain contact with a solid surface, resulting from
intermolecular interactions when they are brought together. The degree of wetting Retardant
Finishes, (wettability) is determined by the balance between adhesive and cohesive forces.
Wetting deals with the three phases of materials, gas, liquid and solid. Adhesive forces
between a liquid and solid cause a liquid drop to spread across the surface. On the other hand,
cohesive forces within the liquid cause the drop to ball up and avoid contact with the surface.
When a drop of liquid on a solid surface does not spread, the drop will assume a shape that
appears constant and exhibits an angle θ, called the contact angle. The angle is characteristic
of the liquid/solid interaction; therefore, the equilibrium contact angle serves as an indication
of wettability of the solid by the liquid.

The physicochemical basis for the wetting of a solid surface by a liquid may be explained as
figure below. A drop of liquid (L) placed on a textile surface (T) in air will spread out until it
makes a contact angle θ defined by the plane of the solid surface, and the tangent to the
liquid–air interface θ is measured in liquid. If the liquid drop spreads completely, the contact
angle is considered to be zero. For this to happen, it is obvious that the attraction between
solid and liquid must be at least as great as the liquid–liquid attraction. In most real
situations, the influence of gravity will distort the liquid solubility so that an actual 180
degrees angle would not be formed.

Figure 3: 1 Spreading of Liquids on Smooth Surfaces

Where: L/V = the interfacial energy between liquid/vapor

S/L = the interfacial energy between solid/liquid

S/V = the interfacial energy between solid/vapor

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 Θ = equilibrium contact angle

On smooth surfaces, the contact angle rarely exceeds 120 degrees. In practice, a contact angle
greater than 90 degrees indicates a poor wetting of the solid by the liquid. Solid surfaces that
form advancing contact angles less than 90 degrees as hydrophilic or wetting, and those that
form higher than 90 degrees as hydrophobic or nonwetting. Geometrical factors (e.g., surface
roughness and porosity) have a profound effect on contact angles and wettability as well as
the chemical nature and physicochemical characteristics of the solid surface are also
important.

Figure 3: 2 Degrees of wetting

A contact angle of less than 90 degrees (i.e., low contact angle) usually indicates that wetting
of the surface is very favorable, and the fluid will spread over a large area of the surface.
Contact angles greater than 90 degrees (high contact angle) generally means that wetting of
the surface is unfavorable, so the fluid will minimize contact with the surface and form a
compact liquid droplet. For water, a wettable surface may also be termed hydrophilic and a
non-wettable surface hydrophobic. Superhydrophobic surfaces have contact angles greater
than 150 degrees, showing almost no contact between the liquid drop and the surface. This is

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sometimes referred to as the ‘lotus effect’. For nonaqueous liquids, the term lyophilic is used
for low contact angle conditions, and lyophobic is used when higher contact angles result.

Relation between contact angle and wettability

3.3 High-energy versus low-energy surfaces

Traditionally, solid surfaces have been divided into high-energy and low energy types of
Solids such as metals, glasses and ceramics are known as hard solids because the chemical
bonds that hold them together (e.g., covalent, ionic, or metallic) are very strong. Thus, it
takes a large input of energy to break these solids, so they are termed high energy. Most
molecular liquids achieve complete wetting with high-energy surfaces. The other type of
solids is weak molecular crystals (e.g., fluorocarbons, hydrocarbons, etc.) where the
molecules are held together essentially by physical forces (e.g., van der Waals and hydrogen
bonds). Since these solids are held together by weak forces, a very low input of energy is
required to break them, thus they are termed low energy. Depending on the type of liquid
chosen, low-energy surfaces can permit either complete or partial wetting.

3.3.1 Critical surface tension

The critical surface tension of a solid is defined as the surface tension of a liquid that just
completely spreads on a surface. only liquids with surface tension values lower than γC
would spread on the surface, whereas liquids with surface tension values greater than γC
would form a finite contact angle on the solid. The critical surface tension is mainly
influenced by the outermost layer of atoms at the solid's surface. It has been established that
repellent finishes that contain either a hydrocarbon base with a γC value of about 30 mN/m or
polysiloxane (silicone) finishes with a γC value of around 24 mN/m can provide very good

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water repellency. However, the surface tension values of hydrocarbon-based oils are much
lower than water and are generally within the range 20–31 mN/m.

Critical surface tensions of smooth polymeric surfaces

To repel hydrocarbon-based oils with surface tension values (γLV) of around 20–31 mN/m, it
is necessary to use finishes with even lower critical surface tension values (γC). Fluorocarbon
(fluorochemical) finishes are available with critical surface tension values below 15 mN/m,
and these provide satisfactory water- and oil-repellency. The incorporation of a wetting agent
into water lowers the surface tension. The presence of impurities in water also lowers the
surface tension. The surface of the raw cotton fibre is covered with a thin coating of natural
waxes, which makes raw cotton inherently water repellent. Scouring treatment markedly
increase the critical surface tension of the fibre as it removes the waxes from the fibre
surface.

3.4 Mechanism of repellency

Repellent finishes achieve their properties by reducing the free energy at fibre surfaces. If the
adhesive interactions between a fibre and a drop of liquid placed on the fibre are greater than
the internal cohesive interactions within the liquid, the drop will spread and vice versa.
Surfaces that exhibit low interactions with liquids are referred to as low energy surfaces.
Their critical surface energy or surface tension γC must be lower than the surface tension of
the liquid γL (the internal cohesive interaction) that is repelled. γL of water, at 73 mN m–1, is
two to three times greater than γL of oils (20– 35 mN m–1). Therefore, oil repellency finishes
with fluorocarbons (γC = 10–20 mN m–1) always achieve water repellency, but fluorine-free
products, for example silicones (γC = 24–30 mN m–1) will not repel oil. Low energy surfaces

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also provide a measure of dry soil repellency by preventing soil particles from strongly
adhering to fibre surfaces and facilitates easy dislodge of the soil mechanically.

The resistance of a fabric to wetting is determined by the following parameters.

➢ The chemical nature of the fibre surfaces (polar or nonpolar groups.)

➢ The geometry and roughness of the fibre surfaces
➢ The nature of the capillary inter-fiber and inter-yarn spacing in the fabric

The surface energy of textile materials can be reduced in several ways.

❖ Incorporate water-repellent finishes on the fibre and fabric surfaces, in the fibre pores and in
the spacing between the fibres and the yarns.
❖ The chemical reaction of the repellent material with the fibre surface. Examples of these are
fatty acid resins.
❖ Formation of a repellent film on the fibre surface.
❖ To use special fabric constructions, like stretched polytetrafluoroethylene films, and
microporous coatings.

3.5 Water proofing and water repellency

3.5.1 water repellency

The term ‘water repellent’ is a relative term because there is always some attraction between
a solid and a liquid in contact, though the force of attraction may be small. Water repellency
may be defined as ‘the relative degree of resistance of a fabric to surface wetting, water
penetration, water absorption or any combination of these properties. If a fabric allows air but
prevents water to pass through itself, it is known as Water Repellent finish. Water-repellent
fabrics will permit the passage of liquid water once hydro-static pressure is high enough.
Water-Proof Fabrics are resistant to the penetration of water under much higher hydrostatic
pressure than are water-repellent fabrics. These fabrics have fewer open pores and are less
permeable to the passage of air and water vapor. For water repellency, a higher fabric
thickness or higher count of yarn is very important. Thin fabrics generally provide poor water
repellency even when treated with water-repellent finishes, unless the interyarn pores are
blocked by coating or with a high chemical add-on of a water-repellent finish.

The water-repellent fabrics are mostly based upon woven fabrics because these can be tightly
woven to decrease the interyarn capillary spaces (or pores). The weft- and warp-knitted
fabrics have an open structure due to large interyarn spaces, so water penetrates readily
through these structures unless an impermeable coating is given. Different types of

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nonwoven fabrics may be treated with water-repellent finishes, provided the fabric has a
smooth surface and the interfibre or interyarn pores are small. The felting of woollen fabric
during the milling process and production of pressed wool felts can lead to a thicker and
denser fabric structure with improved inherent fabric water repellency.

3.5.2 Water proofing

The term ‘waterproof’ is normally taken to represent the conditions in which a textile can
prevent the absorption of water and the penetration of water into its structure. Thus, a
waterproof surface provides a barrier to water under all practical end use conditions. This
finish makes the wearer feel uneasy and uncomfortable as the air circulation is not there. In
absolute terms, a waterproof fabric is fully resistant to penetration by water, implying that the
fabric water penetration resistance is equivalent to its hydraulic bursting strength. However,
in practice a minimum performance of no penetration by water below a hydrostatic pressure
of 100cm (10kPa) is taken to represent a waterproof fabric. The waterproof fabrics are
usually produced by coating the fabric with a solid polymer such as synthetic neoprene
rubber, polyvinyl chloride or polyurethanes.

As they are impermeable both to the passage of air and of water vapour, they are not
‘breathable’. This will not create any problem for many nonapparel end uses like technical
textiles, industrial fabrics, and outdoor textiles such as tarpaulins or awnings. However, a
fabric in garment form must allow air and especially moisture generated by the exudation of
perspiration from the skin during physical activity to pass through the fabric. This allows the
wearer of the garment to maintain warm, dry conditions with high levels of thermophysical
and thermos-physiological comfort.

Distinguish between water-repellent and waterproof fabrics

Distinguish between water-repellent and water-proof fabrics

Fabrics have open pores and are permeable Fabrics have fewer open pores and are less permeable to
to air and water vapour the passage of air and water vapour.

Fabrics will permit the passage of liquid Fabrics are resistant to the penetration of water
water once hydro-static pressure is high. under much higher pressure.

A fabric Is made water-repellent byWaterproofing requires filling the pores as well as

depositing a hydrophobic material on the depositing a hydrophobic material on the fibre’s
fibre’s surface surface.

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3.5.3 Undesirable Effects of water repellency

In addition to the desired repellency effects, other undesirable fabric properties are often
found with repellent finishes.

➢ problems with static electricity

➢ poor soil removal in aqueous laundering
➢ stiffer fabric hand
➢ greying (soil redeposition) during aqueous laundering and increased flammability.

Some fabric properties that are often improved by repellent finishes include;

➢ better durable press properties

➢ more rapid drying and ironing
➢ increased resistance to acids, bases, and other chemicals.

3.6 Stain and soil retardancy

The production of self-cleaning textiles is of great interest to the textile industry. This field
concerns various textile products, such as baby clothes. Such type of textiles should be
essentially stain repellent and resistant to ageing during use. Performance textiles are a new
paradigm for the textile industry and represent one of the fastest-growing sectors of the
industry. Performance textiles are textiles that provide additional functions such as
repellency, resistance or protection from a specified element including fabrics that resist
wrinkles, soils, or odours and/or protect from environmental conditions.

Many fabrics require treatment to improve stain repellent, stain release and soil-repellent
properties, according to their end use. The articles like raincoat, outerwear, upholstery and
bedspreads require stain repellency, washable materials like apparels, sheets and table cloths
require good stain release properties, while carpets and upholstery require soil repellency.
Stain repellency is promoted by hydrophobic finishing.

Paraffin derivatives and melamine-modified fatty acids are economic, but they are not
durable and give rise to emission problems during production.

Silicone products give more soft and permanent effects, but they can cause problems
in subsequent coating and also can attract dirt.

Fluorocarbons provide permanent water, oil and dirt repellency, but are very costly.

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Stain blockers

Carpets are usually made from wool and/or nylon. They are accidentally stained by spillages
of coffee, tea, soft drinks and other liquids and coloured foodstuffs. Certain water-borne food
stains are actually acid dyes and are adsorbed by the nylon fibres. This colouring matter will
dye nylon in the same way as acid dyes. These stains cannot be prevented or removed by
even the best of the antisoil products. Even the best of fluorocarbon-treated nylon carpets
may be stained. A very recent innovation is the introduction of stain-blocking technology that
renders nylon carpets resistant to these stains as well. The technology involves the treatment
of nylon carpets with certain syntans that tie up the remaining amino groups. Syntans and
stain blockers are generally condensates of formaldehyde with phenolsulphonic acids,
naphtholsulphonic acids and sulphonates of dihydroxydiphenylsulphone, or mixtures of
these.

Syntan

Many stain blockers give rise to fibre yellowing after application, and the yellowing increases
on exposure to ultraviolet radiation and also adversely affect the colourfastness to light.

Petal effect and lotus effect

The term ‘petal effect’ describes the fact that a water droplet on the surface of a rose petal is
spherical in shape, but it cannot roll off even if the petal is turned upside down. The water
drops maintain their spherical shape due to the superhydrophobicity of the petal (contact
angle of about 152.4 degrees), but do not roll off because the petal surface has a high
adhesive force with water.

The lotus effect has been named after the unusual properties of the leaf surfaces of the lotus
plant, which are remarkably water and soil repellent. The surface of the lotus leaf is covered
by a thin extracuticellular membrane termed the cuticle, which is covered by waxes forming

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characteristic microstructures due to self-organisation. On smooth wax layers (surface area
contact 10 percent), the contact angle of water may reach 110 degrees, but, because of the
surface roughness of the wax layer, whose dimensions can be measured in micrometres, a
very pronounced superhydrophobicity is generated, with contact angles up to 170 degrees and
surface area contact as low as 7%. As a result, the area for the adhesion of water is markedly
diminished, and air is enclosed between the droplets and the wax crystals.

3.7 Repellent Chemistry

Some of the water-repellent finishes are Metal salts, Paraffin, Pyridinium-based, resin
formers, Organometallic complexes, Silicone, Fluorochemical and Metal salt.

3.7.1 Paraffin repellents

Typically, the products are emulsions that contain aluminium or zirconium salts of fatty acids
(usually stearic acid). These materials increase the finish’s adhesion to polar fibre surfaces by
forming polar–non-polar junctions as shown in Fig. below. The paraffinic portion of the
repellent mixture is attracted to the hydrophobic regions, while the polar ends of the fatty
acid are attracted to the metal salts at the fibre surface. These finishes can be applied by both
exhaustion and padding. They are compatible with most kinds of finishes, but they increase
flammability. Although they are available at relatively low cost and generate uniform
waterproof effects, the lack of durability to laundering and dry cleaning and their low air and
vapour permeability limits the use of paraffin-based repellents.

Figure 3: 3 Fatty acid metal salts. A, hydrophobic interactions; B, polar interactions; C, fibre
surface

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3.7.2 Stearic acid–melamine repellents

Compounds formed by reacting stearic acid and formaldehyde with melamine constitute
another class of water-repellent materials. The hydrophobic character of the stearic acid
groups provides the water repellency, while the remaining N-methylol groups can react with
cellulose or with each other (crosslinking) to generate permanent effects.

Advantages of the stearic acid–melamine repellents include increased durability to

laundering and a full hand imparted to treated fabrics. Some products of this type can be
effectively applied by exhaustion procedures.

Disadvantages of stearic acid–melamine repellents include problems like durable press

finishes (a tendency to exhibit finish mark-off, decreased fabric tear strength and abrasion
resistance, changes in shade of dyed fabric, and release of formaldehyde).

Figure 3: 4 Stearic acid–melamine derivative.

3.7.3 Silicone water repellents

Polydimethylsiloxane products that are useful as water repellents can form a hydrophobic
layer around fibres. The unique structure of the polydimethlysiloxanes provides the ability to
form hydrogen bonds with fibres as well as display a hydrophobic outer surface. To gain
some measure of durability, silicones designed as water-repellent treatments usually consist
of three components, a silanol, a silane and a catalyst such as tin. The outward oriented
methyl groups generate the water repellency. During the drying step after pad application, the
silanol and silane components can react to form a three-dimensional crosslinked sheath
around the fibre.

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 Figure 3: 5 Silicon water repellent

Silicone double layer on the fibre. A, polar surface; B, hydrophobic attraction of the methyl
groups; C, hydrogen bonds to polar fibre surface; D, fibre surface.

Advantages of silicone water repellents

➢ high degree of water repellency at relatively low ( 0.5–1 % owf) concentrations

➢ very soft fabric hand
➢ improved sewability and shape retention
➢ improved appearance and feel of pile fabrics.
➢ Some modified silicone repellents can be exhaust applied (to pressure-sensitive fabrics)

The disadvantages of silicone repellents

➢ increased pilling and seam slippage

➢ reduced repellency if excessive amounts are applied
➢ only moderate durability to laundering and dry cleaning (adsorption of surfactants)
➢ no oil and soil repellency

The silicone finish may enhance the attraction of hydrophobic dirt. In addition, the
wastewater, especially the residual baths, from these finish application processes are toxic to
fish.

3.7.4 Fluorocarbon-based repellents

Fluorocarbons (FC) provide fibre surfaces with the lowest surface energies of all the repellent
finishes in use. Both oil and water repellency can be achieved. FC repellents are synthesised
by incorporating perfluoro alkyl groups into acrylic or urethane monomers that can then be
polymerised to form fabric finishes. Originally, the perfluoro alkyl groups were produced by

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electrochemical fluorination, but today they are produced by telomerisation. The final
polymer, when applied to a fibre, should form a structure that presents a dense CF3 outer
surface for maximum repellency. The length of the perfluorinated side chains should be about
8–10 carbons. The small spacer group, mostly ethylene, can be modified to improve
emulsification and solubility of the polymer. Comonomers (X, Y, for example stearyl- or
laurylmethacrylate, butylacrylate, methylol- or epoxy-functional acrylates and block
copolymers from dihydroxydimethylpolysiloxane) affect fabric hand, film formation and
durability. In this way and by adding appropriate emulsifiers, FC products can be widely
modified for many special performance profiles.

Figure 3: 6 Fluorocarbon-based repellents

Most FC products are padded, dried and cured. Heat treatment causes an orientation of the
perfluoro side chains to almost crystalline structures. This is crucial for optimal repellency.
Washing and dry cleaning disturb this orientation and reduce finish performance. The
orientation must be regenerated by a new heat treatment (ironing, pressing or tumble drying).
But with some new FC products, drying in air is sufficient (laundry–air–dry or LAD
products). Tailored FCs and blocked isocyanates, the so-called boosters, are used for this
effect. Depending on the kind of blocking group, the isocyanate is activated at different
temperatures and then reacts with the functional groups of the FC, the fibre or with itself
(crosslinking). This fixation on the fibre surface provides durability to washing, dry cleaning
and rubbing as a second important effect. Boosters also cause better film formation and
thereby higher repellency effects. However, high amounts of boosters adversely affect fabric
hand.

advantages of fluorocarbon-repellent finishes

➢ low active addons (< 1 % owf)

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 ➢ more rapid drying of treated fabrics
➢ improved soil release during household laundering or stain resistance on nylon,

Disadvantages of fluorocarbon repellents

➢ high cost, greying during laundering.

➢ potentially hazardous aerosols
➢ the need for special treatment of wastewater from application processes
➢ cannot be applied effectively by exhaustion (but there are some new FC products that are
exceptions to this rule).

Low-curing FCs are another new development. They get their repellency without heat, only
after drying at room temperature. This is of interest for the impregnation of garments,
upholstery, and carpets. An inevitable disadvantage is their low durability because of the lack
of fixation by crosslinking.

3.8 Test methods

The water repellency of fabrics is evaluated by one of the three main types of test methods:

Spray tests to simulate exposure to rain.

Hydrostatic pressure tests, which measure the water penetration as a function of

pressure exerted by water standing on the fabric.

Sorption of water by the fabric immersed in water being evaluated, which should be
suitably preconditioned prior to testing under standardised condition.

Test for oil repellency

Hydrocarbon resistance test (AATCC Test Method 118—1997) used to detect the presence of
a fluorochemical finish or other low surface energy finish by evaluating the fabric resistance
to wetting by a selected series of liquid hydrocarbons of different surface tensions.

Exercise 3

Answer the following questions by choosing the best alternatives.

1. Repellent finishes are?

A) Finishes that repel water and oil only B) Finishes that repel dry dirt only

C) Finishes that repel water, oil and dry dirt D) Finishes that repel water and dry dirt only

2. What is stain repellency?

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A) The ability of a treated fabric to resist penetration of liquid soils under dynamic conditions
involving only the weight of the drop and capillary forces

B) The ability of a treated fabric to withstand penetration of liquid soils under static
conditions involving only the weight of the drop and capillary forces

C) The ability of a treated fabric to repel water

D) The ability of a treated fabric to repel oil

3. Water repellency can be achieved by?

A) Using fluorocarbon polymers only

B) Using different product groups, but oil repellency is attained only with fluorocarbon polymers

C) By treating the fabric with a hydrocarbon series

D) By treating the fabric with surfactants

4. What is the difference between water-repellent and waterproof fabrics?

A) Water-repellent fabrics are permeable to air and water vapor, while waterproof fabrics
prevent the absorption and penetration of water into their structure.

B) Water-repellent fabrics prevent the absorption and penetration of water into their structure,
while waterproof fabrics are permeable to air and water vapor.

C) Water-repellent and waterproof fabrics are the same thing.

D) Water-repellent and waterproof fabrics both prevent the absorption and penetration of
water into their structure.

5. The degree of wetting is determined by?

A) The balance between adhesive and cohesive forces

B) The chemical nature and physicochemical characteristics of the liquid

C) The degree of surface roughness of the solid surface

D) The degree of porosity of the solid surface

6. A contact angle greater than 90 degrees indicate?

A) Poor wetting of the solid by the liquid

B) Favorable wetting of the solid by the liquid

C) The complete wetting of the solid by the liquid

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D) The inability of the liquid to spread on the surface of the solid

7. A hydrophilic surface is;

A) A surface that forms a contact angle of less than 90 degrees

B) A surface that forms a contact angle of greater than 90 degrees

C) A surface that is repellent to water

D) A surface that is repellent to oil

8. What are performance textiles?

a) Textiles that provide additional functions such as repellency, resistance, or protection from
specified elements

b) Textiles that are designed for high-performance sports

c) Textiles that are expensive and high-end

d) Textiles that are only used for decorative purposes

9. What is the lotus effect?

a) The surface of the lotus leaf is covered by a thin extracuticular membrane termed the cuticle.

b) A water droplet on the surface of a lotus leaf maintains its spherical shape due to the
superhydrophobicity of the leaf.

c) The contact angle of water on a lotus leaf may reach 170 degrees due to the surface roughness of
the wax layer.

d) All of the above

10. _____________ is the advantage of stearic acid-melamine repellents?

a) They are inexpensive b) They have low durability to laundering

c) They provide a full hand imparted to treated fabrics d) They are flammable

11. Which of the following is not a water-repellent finish?

a) Paraffin b) Fluorochemical c) Silicone d) Nylon

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 CHAPTER FOUR

RETARDANT FINISH

4.1 Flame Retardant finishes

A fabric is deemed to be flame retardant if it does not ignite and create a self-sustaining flame
when subjected to a heat source. Therefore, a pile fabric made from rayon fibers is highly
flammable while a tightly woven fabric made from high twist yarns easily passes the 45-
degree ignition test. Neither however pass the vertical ignition test. Flame retardancy may be
conferred on textile fabrics by use of inherently flame-resistant fibers, use of chemical
aftertreatments or both.

Inherently flame retardancy may arise from

➢ chemical structure which is thermally stable in the first instant or transforms to one (e.g., the
polyaramids or other aromatic structures)
➢ incorporation of flame-retardant additives during the production of manmade fibers or by the
synthesis of conventional fibre-forming polymers.

Chemical aftertreatments include surface or topical treatments, coatings and functional

finishes which become a part of the final fibre structure.

Flame-retardant treatments require application of a relatively large quantity of chemicals,

about 10–30% of the weight of material. Hence, the aesthetic properties (softness, stiffness,
lustre, handle, drape, etc.), physical properties (washability, soil repellence and soil release
and static charge accumulation), tensile properties, creasing and pilling properties may
change.

4.2.1 Thermal properties of textile materials

Combustion is an exothermic process that requires three components:

❖ Heat
❖ Oxygen
❖ Suitable fuel

When left unchecked, combustion becomes self-catalysing and will continue until the
oxygen, the fuel supply or the excess heat is depleted. When textile material is heated,
chemical and physical changes occur depending on the temperature and chemical
composition of the material.

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 ➢ Thermoplastic fibres soften at the glass transition temperature (Tg) and subsequently melt at
Tm. At some higher temperature Tp (temperature of pyrolysis), both thermoplastic and
nonthermoplastic materials chemically decompose or pyrolyse into lower molecular weight
fragments and continue through the temperature at which combustion occurs (Tc). For
thermoplastic fibres, Tg and/or Tm are lower than Tp and/or Tc, while for nonthermoplastic
fibres, Tg and/or Tm are higher than Tp and/or Tc.
➢ In the case of nonthermoplastic natural fibres, pyrolysis and combustion start before softening
and melting. Thermoplastic synthetic fibres melt and drip away from a flame before pyrolysis
and combustion temperatures are reached. However, if the melt does not shrink away from
flame front, pyrolysis and combustion temperatures are eventually reached and ignition
occurs.
4.1.2 Combustion Cycle for Fibers

The thermal processes and combustion products of organic products occur in a progressive
and definable cycle. When heat is applied, the fibre's temperature increases until the pyrolysis
temperature (Tp) is reached. At this temperature, the fibre undergoes irreversible chemical
changes, producing nonflammable gases flammable gases tars and carbonaceous char. As the
temperature continues to rise, the tars also pyrolyse, producing more flammable and
nonflammable gases and char. When the combustion temperature (TC) is reached, the
flammable gases combine with oxygen in the process called combustion, which is a series of
gas-phase free radical reactions.

These highly exothermic reactions generate large amounts of heat and light, and the
generated heat provides additional thermal heat for the pyrolysis process to continue. The
burning behaviour of textiles is determined more by the speed or rate of heat release than by
the amount of generated heat.

Pyrolysis; Irreversible chemical decomposition due to nonoxidative heating

Ignition Initiation of combustion

Flammability Tendency of a material to burn in the presence of a flame.

Flame retardant Chemical compounds capable of imparting flame resistance or reduced

flammability to a material to which is applied.

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 Figure 4: 1 Combustion cycle for fibres.

After combustion, the polymer may degrade without flame, burst into flame or change
physically by melting, shrinking or charring. The combustion products may further
decomposed and ignited. In other words, upon heating, a polymer may be liquefied with or
without decomposition, converted into carbon residues (chars) or release combustible or
noncombustible gases. The role of flame retardants (FRs) is to inhibit the formation of
combustible products and/or to alter the normal distribution of decomposition product
originating from the original material.

4.1.3 Flammability of textile fibers

4.1.3.1 Burning behavior of natural fabrics

The flammability characteristics of commercially available fibre vary widely. It has been
established that the size and depth of the burn injury is related to heat transfer rather than the
rate of flame spread. Heavier fabrics produce more heat per unit area, although the flame
spreads on them at slower rate. All fabrics burn, but some are more combustible than others.
Untreated natural fibers such as cotton, linen and silk burn more readily than wool, which is
more difficult to ignite and burns with a low flame velocity. However, though wool fibers
have natural flame retardancy, woolen fabrics burn easily due to open fabrics structure and
the presence of dyes and finishes. Cellulosic fibers, namely cotton and rayon, burn readily
with afterglow and formation of char.

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4.1.3.1 Burning behavior of synthetic fabrics

Synthetic fabrics, such as nylon, acrylic or polyester, resist ignition. However, the fabric will
melt once ignited. The hot sticky melts are of very high temperature and can cause deep and
severe skin burns. One major concern regarding synthetics such as polyester is that they tend
to shrink at relative low temperatures. In clothing, this may be extremely dangerous; for
example, synthetic fiber underwear can shrink onto the body when the outerwear burns,
thereby removing the previously present insulating layer of air. Polyvinyl chloride and
polyvinylidene chloride fibers do not support combustion and nylon 6, nylon 6,6 and
polypropylene melt slowly without burning. However, polyester, and acrylic melt and burn
readily.

Blended fabrics may be more hazardous, as in most cases they combine high rate of burning
with the problem of melting resulting in more severe skin injuries. Loosely woven fabrics
burn more easily than tightly woven fabrics. The surface texture with loose or fluffy piles
ignites more readily than fabric with hard, tight surface. Garment designs also affect
flammability because clothing that fits closely to the body is less likely to stray into a flame
source; if it ignites, it tends to self-extinguish.

Various thermal parameters of textile fibers

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Nomex and Kevlar, Kynol, PBI, Ryton, Inidex and Curlon are inherently thermal resistant.
Thermal resistant polyester can be prepared by;

➢ Copolymerisation of FRs into basic fibre polymer chain

➢ Introduction of an additive during polymerisation or extrusion
➢ Application of chemical system(s) as a textile finish.
4.1.4 Limiting oxygen index

It is the minimum content of oxygen in an O/N mixture. Amount of oxygen in the fuel mix
needed to support combustion that is Minimum quantity of oxygen a fibre needs to burn. For
effective flame retardancy LOI should be 26 and above.

Limiting Oxygen Values of Different Fibres

The relation between LOI and flammability of different textile fibres is as follows:

❖ LOI ≤ 19—easy ignition, rapid burning (cotton, acrylic, viscose, and polypropylene)
❖ 19 ≤ LOI ≤ 22—normal ignition and burning behaviour (polyester, nylon 6 and nylon 6,6)
❖ LOI around 25, almost ignition-resistant (wool)
❖ LOI > 26, flame-retardant (modacrylic, meta-aramide, para-aramide)
❖ LOI > 30, flame-resistant under severe conditions, for example, heavy air ventilation
(melamine/phenol formaldehyde, polybenzimidazole or PBI, PTEE etc.)
❖ LOI around 100, not burning even in pure oxygen, only melting (glass and ceramic fibres)

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4.1.5 Flame Retardants

The term ‘flame retardant’ is used to describe fabrics which will not support combustion and
are self-extinguishing. In case of accidental fire, this type of fabrics will not contribute to the
spreading of flame. Other terms like flame-resistant, flameproof, and fireproof are often
meaningless or misleading because nearly all fabrics are combustible to some degree. Flame
retardants (FR) are chemicals which are added to combustible materials to render them
resistant to fire. If the material is ignited, the flame retardant will slow down combustion and
prevent fire from spreading to other items. Several types of compounds and polymers are
used as FR for textile materials, including inorganic acids, acid salts and hydrates,
organophosphorus and organobromine compounds, antimony salts/halogen systems etc. From
an application point of view, fiber FR systems may be classified as follows.

Nonreactive systems

a. Topical deposition
b. Two-stage precipitation
c. Exhaustion from bath
d. Incorporation in fiber before spinning.

Reactive systems

a. Reaction of FR with fiber

b. Graft copolymerization with fiber
c. In situ polymerization of FR compounds
d. FR fibers Copolymerization of compounds with fiber-forming monomers
e. Inherently FR fibers
4.1.5 Mechanism of flame retardancy

The principle of flame retardancy is based on the Interruption or Prevention of combustion of

fibre. Attempts to disrupt combustion cycle for textile substrates have focused on several
approaches/Mechanisms.

❖ Removal of heat
❖ Increase decomposition temperature Tp
❖ Decrease the number of combustible gases and promote char formation.
❖ Prevent the access of oxygen to the flame or dilute the fuel gases.
❖ Increase the combustion temperature, Tc, of the fuels.

One method is to provide a heat sink on or in the fiber by use of materials that thermally
decompose through strongly endothermic reactions. If enough heat can be absorbed by these

148
reactions, the pyrolysis temperature of the fiber is not reached, and no combustion takes
place. Examples of this method are the use of alumina trihydrate and calcium carbonate as
fillers in polymers and coatings.

Figure 4: 2 Endothermic decomposition reaction

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

Formation of foamed glass

A third way to achieve flame retardancy is to influence the pyrolysis reaction to produce less
flammable volatiles and more residual char. This ‘condensed phase’ mechanism can be seen
in the action of phosphorous-containing flame retardants ( e.g. Di-ammonium Phosphate,
(NH4)2HPO4) which, after having produced phosphoric acid through thermal decomposition,
crosslink with hydroxyl-containing polymers thereby altering the pyrolysis to yield less
flammable by product

Figure 4: 3 Crosslinking with phosphoric acid

A fourth approach to preventing combustion is to interfere with the free radical reactions that
provide the heat needed for the process to continue. Materials that act in this ‘gas phase’

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mechanism include volatile halogen containing compounds e.g. Antimony halides (SbCl3 or
SbBr3) which, during combustion, yield hydrogen halides that form relatively long lived, less
reactive free radicals. Flame retardant mechanism can also be divided into Condensed phase
and Vapor phase. Condensed phase’ mechanism is based on removal of heat and the
enhancement of the decomposition temperature. It involves one or more of the following
approaches.

❖ Heat Sink on / in the fiber (Alumina trihydrate’ and calcium carbonate as fillers)
❖ Insulating Layer (Boric acid and its hydrated salts)
❖ Reaction to produce fewer flammable volatiles and more residual char (phosphoric acid
crosslinked with hydroxyls)

Gas phase or vapour phase mechanism Interfere with the free radical reactions that provide
the heat needed for the process to continue.

4.1.6 Flame-retardant chemistry

The most important commercial flame retardants can be classified into three broad categories.

➢ Primary flame retardants based on phosphorous.

➢ synergistic retardancy enhancers that have only small flame retarding effects by themselves,
but greatly enhance the flame retardancy of primary flame.
➢ adjunctive flame retardants that exhibit their activity through physical effects
4.1.7 Flame retardants for cellulose

One important thermal degradation mechanism of cellulose fibres (cotton, rayon, linen, etc.)
is the formation of the small depolymerisation product levoglucosan. Levoglucosan and its
volatile pyrolysis products are extremely flammable materials and are the main contributors
to cellulose combustion. Compounds that can hinder levoglucosan formation are expected to
function as flame retardants for cellulose. The crosslinking and the single type of
esterification of cellulose polymer chains by phosphoric acid reduces levoglucosan
generation, catalyses dehydration and carbonisation, and thus functions as an effective
flameretardant mechanism.

4.1.7.1 non-durable flame retardants for cellulose

1. Boric Acid/Borax

A mixture of boric acid/borax (sodium borate) is a commonly used non-durable flame

retardant finish for cellulosic fibers. It is the safest about carbon monoxide and smoke
production during burning.

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 Figure 4: 4 Formation of foamed glass

2. Ammonium Salts

Ammonium salts of strong acids, especially phosphoric acid (P/N synergism) are particularly
useful as nondurable flame retardants for cellulose. Three commercially important products
are diammonium phosphate, ammonium sulfamate and ammonium bromide. These salts
readily form the corresponding strong acids upon heating. Diammonium phosphate and
ammonium sulfamate are used at ~ 15 % solids addon and function as condensed phase flame
retardants, not only by crosslinking but also by dehydrating cellulose to polymeric char with
reduced formation of flammable by-products. The water insoluble ammonium polyphosphate
is an effective flame retardant and is added to coatings and binder systems, for example for
pigment printing. Ammonium bromide is applied at ~ 10 % solids add-on and is effective in
the gas phase.

4.1.7.2 Durable flame retardants for cellulose

Although inorganic salts can provide excellent flame-retardant properties for cellulose,
reasonable laundering durability must be incorporated into any finish destined for apparel
use. The most successful durable flame retardants for cellulose are based on phosphorous-
and nitrogen-containing chemical systems that can react with the fiber or form crosslinked
structures on the fiber. The key ingredient of one of these finishes is tetrakis
(hydroxymethyl)phosphonium chloride (THPC), made from phosphine, formaldehyde, and
hydrochloric acid. THPC reacts with urea to form an insoluble structure on cellulose in a
pad–dry–cure process.

Figure 4: 5 Synthesis of THPC

Treating the cured finish with hydrogen peroxide to convert the phosphorous atoms to their
highest oxidation state results in cellulosic goods with very durable flame retardancy.
Applying 25 % THPC with 15 % urea yields a final phosphorous add-on of 3.5–4 %, which is

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adequate for most fabrics. Although the THPC–urea system can give highly effective and
durable flame retardancy to cellulose, treated fabrics are stiff and have significantly impaired
tensile and tear strengths as well as releasing formaldehyde during processing. Another
successful commercial approach to durable phosphorous-containing finishes is the use of N-
methylol dimethylphosphonopropionamide in combination with trimethylol melamine and
phosphoric acid as catalyst in a pad– dry–cure process.

4.1.8 Flame-retarding fibre blends

Fibre blends, especially blends of natural fibres with synthetic fibres, usually exhibit a
flammability that is worse than that of either component alone. Natural fibres develop a great
deal of char during pyrolysis, whereas synthetic fibres often melt and drip when heated. This
combination of thermal properties in a fabric made from a fibre blend result in a situation
where the melted synthetic material is held in the contact with the heat source by the charred
natural fibre. In order to flame retard natural/synthetic fibre blends, high levels of flame
retardants are often required. One approach to this dilemma is to add the necessary amounts
of retardant as a fabric coating. By using decabromodiphenyl oxide (DBDPO) in combination
with antimony trioxide, a cotton/polyester blend fabric has been produced that exhibits
durable flame retardancy. The finish required 37 % add-on of the retardants in addition to a
latex binder and softener.

Figure 4: 6 Flame-retardant system for fibre blends.

4.1.9 Evaluation of flame retardants

Many factors influence the flammability of textiles, including the fibre type, the fabric weight
and construction, the method of ignition, the extent of heat and material exchange, and the
presence or absence of flame retardants. Differing performance requirements and government
regulations have led to the development of numerous test methods. A measure that enables an
obvious assessment of flame protection properties is the limiting oxygen index (LOI),
determined according to ASTM D-2863. The LOI is defined as the content of oxygen in an
oxygen/nitrogen mixture that keeps the sample at the limit of burning:

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 LOI = 100 × O2: (O2 + N2)

As the oxygen content of air is 20 % corresponding to LOI = 20 all textiles with lower LOI
values will burn quite easily in air and those with LOI values much higher than 20 will not
burn. For all methods, strict adherence to the testing protocol is crucial to obtaining reliable
and repeatable results.

4.1.10 Requirements of Flame-retardant Textiles

The requirements for a commercially successful flame-retardant textile product have been
given as meeting flammability requirements: having little or no adverse effect on the textile’s
physical properties; retaining the textile’s aesthetics and physiological properties; being
produced by a simple process with conventional equipment and inexpensive chemicals; and
being durable to repeated home launderings, and tumble dryings and dry cleaning. Easy to
apply with conventional equipment.

4.1.11 Applications of flame retardant textiles

Flame retardant treated textiles find application in various areas at home, in offices, in public
buildings, in transport systems, at work, etc. Such applications could include products like
sleepwear, bedlinen, blankets, upholstered furniture covers, carpets, curtains, sunshades, sun
blinds, tarpaulins, tents, and flags as well as protective clothes for workers and fire fighters. It
also includes manufacturing of uniforms for fire fighters and military/police personnel High
performance sports applications, upholstery for home furnishing, sleepwear for children and
elderly people and architectural fabrics.

Flame retardant textile materials help to save lives, prevent injuries and property losses, and
protect the environment by helping to prevent fi res from starting and limiting fi re damage.

4.2 UV protective finishes

Long term human exposure to solar UV radiation may result in acute and chronic health
effects on the skin, eyes and immune system. Sunburn (erythema) is the most common acute
effect of excessive UV radiation exposure. The World Health Organization (WHO)
recommends that loose-fitting, full-length clothing be used for outdoor activities to protect
our skin from UV rays. Textiles, coatings and finishes derived from synthetic and naturally
occurring polymers absorb solar ultraviolet radiation, and then undergo photolytic, photo
oxidative and thermo-oxidative reactions that result in the degradation of the material in the

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forms of discoloration, chalking and reduced mechanical properties. Hence, the development
of effective UV protective textile finishing is of great importance to human health, society
and the environment.

4.2.1 The definition and effects of UV Radiation

Ultraviolet rays constitute a very low fraction of the solar spectrum, but they influence all
living organisms and their metabolisms. These radiations can cause a range of effects from
simple tanning to highly malignant skin cancers, if unprotected. Long-term exposure to UV
light can result in the acceleration of skin ageing, photodermatosis (acne), phototoxic
reactions to drugs, erythema (skin reddening), sunburn, increased risk of melanoma (skin
cancer), eye damage (opacification of the cornea) and DNA damage. The term UV A
represents the region 320–400nm, the term UV B represents the region between UV C and
UV A (i.e., 290–320nm) and the UVC region represents the region below 290m. The order of
potency has been decided as UVC>UVB>UVA>.

The very high energy of the UV-C photons is mostly absorbed by ozone in the higher
regions. But the energies of UV A and UV B photons that reach the earth surface exceed the
carbon-carbon single bond energy of 335kJ/mol. Most damage to skin is done by radiation
less than 300nm. The wavelengths of maximum danger to skin are 305–310nm. Therefore, to
be useful in protecting the wearer from solar UV radiation, textiles must demonstrate
effectiveness in the 300–320nm range

Table Health effects of various UV components

Name of UV Wavelength Health effect

component range (nm)

UVA 120–400 Cataract, sunburn, indirect DNA damage,

suppression of immune system

UVB 290–320 Skin or eye burn, skin cancer, ageing,

suppression of immune system

UVC 190–290 Skin or eye burn

To quantify the protective effect of textiles, the solar protection factor (SPF) is determined.
The SPF is the ratio of the potential erythemal effect to the actual erythemal effect

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transmitted through the fabric by the radiation and can be calculated from spectroscopic
measurements. The larger the SPF, the more protective the fabric is to UV radiation. In
Europe and Australia, the SPF is referred to as the ultraviolet protection factor (UPF). The
SPF is also used with so-called ‘sun blocking’ skin creams, giving a relative measure of how
much longer a person can be exposed to sunlight before skin damage occurs. Typically, a
fabric with an SPF of > 40 is considered to provide excellent protection against UV.

4.2.2 Mechanism of UV protection

When radiation strikes a fibre surface, it can be reflected, absorbed, transmitted through the
fibre, or pass between fibres radiation reflected, absorbed or transmitted depend on many
factors, including the fibre type, the fibre surface smoothness, the fabric cover factor and the
presence or absence of fibre delustrants, dyes and UV absorbers.

Figure 4: 7 Radiation in contact with a textile surface

Cotton and silk fibres offer little protection to UV radiation since the radiation can pass
through without being markedly absorbed. Wool and polyester, on the other hand, have
significant higher SPFs since these fibres will absorb UV radiation. Nylon falls in between
these extremes. One factor influencing nylon and polyester absorbance is the presence of the
delustrant TiO2, a material that strongly absorbs UV radiation. By definition, the theoretical
maximum SPF is the reciprocal of 1 minus the cover factor.

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Tight micro-fibre fabrics provide a better UV protection than fabrics made from normal sized
fibres with the same specific weight and type of construction. Many dyes absorb UV
radiation as well as visible light. A cotton fabric dyed to a deep shade can achieve SPF values
of 50 or higher just from the presence of the dye.

4.2.3 Protection factor

Protection factor is used to quantify the protective effect of material.

➢ SPF/UPF is the ratio of actual potential erythemal effect to the erythemal effect
transmitted through the fabric. Larger the UPF/SPF, the more protective the fabric
to UV radiation

UPF Rating and Protective Category

UPF rating Protective category UV radiation blocked (%)

40–50 + Excellent 97.5–99 +

25–39 Very good 96.0–97.4

15–25 Good 93.3–95.9

4.2.4 Methods of ultraviolet protection

There are two possibilities of reducing UV transmittance by fabrics

➢ Spacing the yarns as closely as possible.

➢ Improving the absorption & reflection properties by use of UV absorbers

4.2.5 Chemistry and mechanisms of UV protection finishes

the required properties of UV protective finishing chemicals should include but not be limited
to

➢ efficient absorption of UVB radiation at 290–320 nm

➢ quick transformation of the high UV energy into vibrational energy in UV absorber molecules
and then into heat energy in the surroundings without photodegradation.

There are two types of UV absorbing/scattering molecules and particles used commercially:

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 ➢ Inorganic UV blocking particles.
➢ Organic UV absorbing molecules.

4.2.5.1 Inorganic UV blocking chemicals

Inorganic oxides such as TiO 2 , CeO 2 and ZnO are the most widely used for protection
against UV radiation. These metal oxides share the same UV protection mechanism; the
attenuation of the UV radiation in these materials is accomplished by both band gap
absorption and scattering of light. In absorption the loss of intensity of light is due to the
conversion of light energy to other forms of energy such as lattice vibration (heat) during the
polarization of molecules in the medium,

4.2.5.2 Organic UV protection finishes

Organic UV absorbers have been used to reduce the damaging effects on textile materials and
health risks of UV radiation. The UV absorber molecules must be colourless or nearly
colourless compounds having high absorption coefficients in the UV range of 290–400 nm
spectra. In order to offer effective protection against UV radiation, the UV protection finish
molecules must quickly transform the absorbed energy into less harmful vibrational (phonon)
energy before reaching the surrounding substrate and must exhibit good photostability.

4.2.6 Application methods

➢ Incorporation into spinning dope prior
➢ Padding, exhaust
➢ Pad-dry-cure
➢ pad thermosol methods

Exercise 4
Answer the following questions by choosing the best alternatives.
1. What is a fabric deemed to be if it does not ignite and create a self-sustaining flame when
subjected to a heat source?
a) Flammable b) Inherently flame-resistant c) Non-flammable d) Non-reactive
2. What are the two ways to confer flame retardancy on textile fabrics?
a) Use of inherently flame-resistant fibers only
b) Use of chemical aftertreatments only
c) Use of both inherently flame-resistant fibers and chemical aftertreatments
d) Use of natural fibers only
3. What percentage of chemicals is required for flame-retardant treatments?

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a) 5–10% of the weight of material b) 10–30% of the weight of material
c) 30–50% of the weight of material d) 50–70% of the weight of material
4. What are the three components required for combustion?
a) Heat, oxygen, and water b) Heat, oxygen, and fuel
c) Heat, fuel, and water d) Oxygen, fuel, and water
5. _________ is the temperature at which both thermoplastic and non-thermoplastic materials
chemically decompose into lower molecular weight fragments?
a) Tg b) Tm c) Tp d) Tc
Answer: c) Tp
6. __________is the temperature at which nonthermoplastic natural fibres start pyrolysis and
combustion?
a) Tg b) Tm c) Tp d) Tc
7. Which natural fibers are more difficult to ignite and burn with a low flame velocity?
a) Cotton and linen b) Wool c) Silk d) Rayon
8. What are flame retardants?
a. Materials that contribute to the spreading of flame b. Materials that are resistant to fire
c. Materials that make fabrics combustible d. Materials that ignite fabrics
9. Which is an example of a heat sink material used in textiles?
a. Boric acid b. Antimony halides c. Calcium carbonate d. Phosphoric acid
Answer: c. Calcium carbonate.
10. What is the category of flame retardants that only have small flame retarding effects by
themselves but greatly enhance the flame retardancy of primary flame retardants?
a. Primary flame retardants based on phosphorous b. Synergistic retardancy enhancers.
c. Adjunctive flame retardants d. Fibre FR systems
Answer: b. Synergistic retardancy enhancers.
11. What is the main contributor to cellulose combustion?
a. Boric acid b. Calcium carbonate
c. Levoglucosan and its volatile pyrolysis products d. Antimony halides
12. Which thermal degradation product of cellulose fibres contributes to cellulose combustion?
a. Levofloxacin b. Levoglucosan c. Levodopa d. Levothyroxine
13. Which of the following compounds hinders the formation of levoglucosan and functions as a
flame retardant for cellulose?
a. Ammonium Salts b. Boric Acid/Borax c. Sodium Chloride d. Potassium Nitrate
14. Which of the following ammonium salts is used as a flame retardant for cellulose in coatings
and binder systems?

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a. Ammonium Sulfate b. Ammonium Bromide c. Ammonium Nitrate d. Diammonium Phosphate
15. Which of the following is a commercially successful durable flame retardant for cellulose?
a. Sodium Borate b. N-methylol dimethylphosphonopropionamide
c. Ammonium Bromide d. Sodium Chloride
16. Which of the following finishes is known for its highly effective and durable flame retardancy
to cellulose?
a. Sodium Borate b. Ammonium Sulfate c. THPC–urea system d. Diammonium
Phosphate
17. Which of the following materials in fibre blends often melt and drip when heated?
a. Synthetic fibres b. Natural fibres c. Both natural and synthetic fibres d. None of
the above
18. Which of the following is a flame-retardant system for fibre blends?
a. THPC–urea system b. Ammonium Sulfate
c. Sodium Borate d. DBDPO in combination with antimony trioxide
19. Which of the following test methods is used to determine the limiting oxygen index (LOI)?
a. ASTM D-2863 b. ASTM D-5420 c. ASTM D-6241 d. ASTM D-6784
20. What factors influence the flammability of textiles?
a. Fibre type b. Fabric weight and construction c. Method of ignition d. All of the above

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 CHAPTER FIVE

ANTI FINISHES

5.1 Antimicrobial finishes

Textiles made from cotton fibres are breathable, absorbent and comfortable to wear because
of their porous hydrophilic structures. Because the structure retains water and oxygen easily,
it provides a suitable environment for microbial growth. Therefore, it is necessary to impart
antimicrobial properties to cotton fabrics, particularly in view of the growing emphasis on
health and hygiene care. Due to consumers’ demand for hygienic clothing and activewear, a
substantial market for antimicrobial textile products has been created. In recent years,
antimicrobial textiles have advanced rapidly for use in various industries such as textile,
pharmaceutical, medical, engineering, agricultural and food.

5.1.1 Microbes or microorganisms

They are single-cell organisms so tiny that millions can fit into the eye of a needle. They are
the tiniest creatures not seen by the naked eye. They include a variety of microorganisms like
bacteria, fungi, algae and viruses. They are the oldest form of life on earth. Microbe found
everywhere in air we breathe, soil, on the fabrics etc.

Bacteria

Bacteria are unicellular organisms, which grow very rapidly under warmth and moisture.
They can be dangerous and cause infection or beneficial, as in the processes of fermentation
or decomposition. Further, subdivisions in the bacteria family are Gram-positive
(Staphylococcus aureus), Gram-negative (Escherichia coli), spore-bearing or nonspore-
bearing types.

Fungi

Fungi, moulds or mildew are complex organisms with slow growth rates; they stain the fabric
and deteriorate the performance properties of the fabrics They are a kingdom separate from
bacteria, plants, and animals. Fungi lack chlorophyll, leaves, true stems, and roots, but their
cell walls contain chitin, which is only found in the animal kingdom. Fungi reproduce by the
production of spores. Fungi are active at a pH level of 6.5.

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Microfungi

These are fungi such as mould, mildew, yeasts and so on; they do not produce a macroscopic
fruiting body like a mushroom.

5.1.2 Antimicrobial

The negative effect on the vitality of the microorganisms is generally referred to as

antimicrobial. A biocide is defined as a chemical substance or microorganism intended to
destroy, deter, render harmless or exert a controlling effect on any harmful organism by
chemical or biological means. Biocides, fungicides and bacteriocides are the products that
kill microbes, namely living organisms, fungi and bacteria, respectively. Biostats, fungistats
and bacteriostats are the substances capable of inhibiting the growth of living organisms,
fungi and bacteria, respectively.

5.1.3 Growth of microorganism

Natural fibres, such as cotton and linen, are readily prone to be infested by microorganisms
like bacteria and fungi. Synthetic fibres are not totally immune to microorganisms; for
example, polyurethane fibres and coatings can be damaged, and the structure of the substrates
and chemical processes may induce the growth of microbes. Humid and warm
environments further aggravate the problem. Of course, because of evolution, natural fibres
are more easily attacked. Proteins in keratinous fibres and carbohydrates in cotton can act as
nutrients and energy sources under certain conditions. Wool is more likely to suffer a
bacterial attack than cotton, and cotton is more likely than wool to be attacked by fungi.
Manmade fibres such as nylon, acrylics and polyester, which all have inherent resistance to
microbial decomposition, came into wider use to replace cotton in many industrial fabrics.

Even comparatively resistant fibres can become susceptible to microbial infestation by the
application of textile auxiliaries such as brighteners, starch, dyes, spin finish oil, etc. Besides
the chemical composition of the textile, physical environment in which they are used also
determine the susceptibility to microbial attack. The presence of human body fluids like
sweat, sebum, blood, dust, dirt and food stains on fabric provides a nutrient-rich environment
for microbial growth.

5.1.4 Effects of microbial growth on textiles and human health

The microbial growth on textile fabrics will result in the emission of obnoxious odours from
infected fabric. It may also lead to pigmentation or discolouration, loss of fabric strength and

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transmit infections among humans. The clothing can form an ideal breeding ground for
microorganisms found on the skin. High moisture and body heat provide optimal conditions
for growth for most microorganisms, and they can double in number every 20–30min. Any
textile made from cellulosic materials, namely cotton, viscose, jute, flax, hemp or blends of
fibres, can be degraded under appropriate conditions by microorganisms leading to the
breakdown of the fibre, loss of tensile strength and premature failure of the finished product.
The rate at which degradation takes place is dependent on a wide range of factors, including
the type of fibre used, construction of the material or goods, other chemical treatments
applied, the end use of the product and the climatic conditions under which the product is
used.

5.1.5 Types of antimicrobial finishing agent

According to the origin, there are two types of antimicrobial finishing agents, these are
natural and synthesis. According to the mode of action also leaching and non-leaching and
based on the antimicrobial effectivity they are divided into biostatic and biocides.

5.1.5 1 Synthetic antibacterial agents

synthetic agents are triclosan, polybiguanides, N-halamine and halogenated phenols, metals
and metal salts such as silver, zinc, copper, Quaternary ammonium compounds, silver,
polyhexamethylene biguanides. Use of these antimicrobial compounds may result in a shift in
the skin microflora composition and lead to outgrowth of pathogen. The synthetic
antimicrobial agent shows good antibacterial activity and durability, but toxic nature of some
artificial agents and their non-degradability in the environment has shifted the inclination of
their utilization towards natural products as viable alternatives.

5.1.5.2 Natural antibacterial agents

Plants possess a wide variety of secondary metabolites which have been found in vitro to
have antimicrobial properties. Extracts from different parts of diverse species of plants like
roots, leaves, flowers, and seeds exhibit antimicrobial properties.

5.1.6 Properties of an effective antimicrobial finish

The growth rate of microbes can be astoundingly rapid. The bacteria population, for example,
will double every 20 to 30 min under ideal conditions (36–40 °C or 77–98 °F, pH 5–9). At
this rate, one single bacteria cell can increase to 1 048 576 cells in just 7 hours. Therefore,

➢ Antimicrobial finishes must be quick acting to be effective.

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 ➢ The antimicrobial must kill or stop the growth of microbes
➢ Must maintain this property through multiple cleaning cycles or outdoor exposure.
➢ The antimicrobial must be safe for the manufacturer to apply and the consumer to wear.
➢ The finish must meet strict government regulations and have a minimal environmental
impact.
➢ The antimicrobial finish must be easily applied at the textile mill.
➢ Should be compatible with other finishing agents, have little if any adverse effects on other
fabric properties including wear comfort.
➢ Should be of low cost.
5.1.7 Mechanisms of antimicrobial finishes

Despite the long list of requirements, a variety of chemical finishes have been used to
produce textiles with demonstrable antimicrobial properties. These products can be divided
into two types based on the mode of attack on microbes.

➢ Controlled release or leaching type mechanism.

➢ Bound or non-leaching mechanism

In controlled release the antimicrobial is slowly released from a reservoir either on the fabric
surface or in the interior of the fibre. This ‘leaching’ type of antimicrobial can be very
effective against microbes on the fibre surface or in the surrounding environment. However,
eventually the reservoir will be depleted, and the finish will no longer be effective. In
addition, the antimicrobial that is released to the environment may interfere with other
desirable microbes, such as those present in waste treatment facilities.

Non-leaching or bound type antimicrobial finish can control only those microbes that are
present on the fibre surface, not in the surrounding environment. ‘Bound’ antimicrobials,
because of their attachment to the fibre, can potentially be abraded away or become
deactivated and lose long term durability. Antimicrobial finishes that control the growth and
spread of microbes are more properly called biostats, i.e. bacteriostats, fungistats. Products
that actually kill microbes are biocides, i.e. bacteriocides, fungicides. This distinction is
important when dealing with governmental regulations since biocides are strongly controlled.

The actual mechanisms by which antimicrobial finishes control microbial growth are.

➢ preventing cell reproduction

➢ blocking of enzymes
➢ reaction with the cell membrane (for example with silver ions) to the destruction of
the cell walls and poisoning the cell from within.

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5.1.8 Evaluation of antimicrobial finishes

Antimicrobial activity can be determined by qualitative or quantitative test methods. Two

types of antimicrobial tests are dominant, the agar-based zone of inhibition tests and the
bacteria counting tests. The relatively new ISO/DIS 20645 and the corresponding EN ISO
20645 are based on the agar diffusion test and ISO 11721 is a burial test (part 1 for the
determination of an antimicrobial finish and part 2 for the determination of the long-term
resistance).

5.2 Insect resist, mite protection

5.2.1 Insect resist

Protection against biological attack includes antimicrobial finishes and insect resist finishes,
including protection against dust mites. Insect resist finishes are chemical treatments that
protect wool and other animal fibres from attack by the larvae of certain moths and beetles.
Only keratin containing fibres are damaged by these insects. Dust mites cause health
problems, such as allergy, asthma and neurodermitis. Mites are not insects; they belong to the
spider group of animals. Keratin-digesting pests include the clothes moth, brown house moth,
carpet beetle and fur beetle.

5.2.1.1 Mechanisms of insect resist finishes

Insect resist finishes fall into two types, poisons that interfere with the keratin digesting
process of the larvae and nerve poisons that have been specifically formulated from
agricultural pesticides for textile applications. Of the two types, digestion-affecting poisons
are more species specific, killing the feeding larvae by blocking enzymes needed for
digestion. Nerve poisons are more general control agents, affecting a broader range of
insects. Both types are considered to enter through the larvae‘s digestive tract because insect
resist treated wool only kills insects that ingest the fibre. Each category has distinct
advantages and disadvantages. Digestive poisons present a lower environmental hazard than
nerve poisons but are not as effective against some pests such as the brown house moth.
Nerve poisons are usually more rapidly biodegraded than digestive poisons, but also exhibit
less durability.

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5.2.1.2 Application Area

The most important market for insect resist finishes is the carpet industry. More than two-
thirds of these finishes are used with floor coverings and wall hangings. Other significant
markets include home furnishing and upholstery fabrics, blankets, uniforms, apparel and furs.

5.2.1.3 Application Methods

Insect resist finishes are mostly applied during dyeing. The best light fastness and wet
fastness properties are obtained when the finish can fully penetrate the fibres. Application of
insect resist finishes during scouring is also possible when wool yarns for carpets are scoured
in hank form or when fabrics for blankets, apparel and upholstery are prepared as piece
goods. Combining the finish with spinning lubricants and then to apply the combination to
loose wool prior to spinning is also possible. This method of finish application produces
yarns with only a superficial treatment with much lower fastness than applications made
during dyeing or scouring. Chemical cleaning of wool textiles as smaller carpets, wall
hangings, furs or uniforms can easily be combined with the application of insect resist
finishes. Dip and cautious spray application is used for the protection of wool and silk
textile exhibits in museums.

5.2.2 Finishes for protection from dust mites.

Mites are a group of spiders, characterized by the fusion of the chest with the lower body.
Dust mites live and proliferate in house textiles such as bedding, mattresses, quilts and also,
but to a lesser extent in carpets, upholstery and pillows. Their main nutrients are skin scales
which are produced and scraped off by the regeneration of the human skin. Comfortable
temperature and moisture conditions that are found in modern houses are not only agreeable
for human inhabitants but also for dust mites and microorganisms. Bedding and mattresses
especially are a paradise for dust mites, providing ideal living conditions.

Simple protection from these problems is achieved by repeated airing, lower room
temperature, washing and cleaning. There are several chemical approaches to solving the dust
mite problem in addition to mechanical solutions. Mite-specific biocides are either durably
bonded to the fibre or control released. Microencapsulation is another interesting possibility
for application. Direct chemical protection with specific products against dust mites is and
may be combined with mite-tight textiles. reduction by antimicrobial finishes helps to control
the mite population.

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5.3 Antistatic finishes

5.3.1 The concept of antistatic finishes

Most textile fibres do not conduct electricity efficiently and can be classified as dielectric
materials, demonstrating insulating properties when dry. Whenever two surfaces come into
contact, electrons can flow from one to the other. Conducting materials allow this electron
flow to be equalised instantly when the surfaces are separated. Insulating materials, on the
other hand, can retain the electrical charge difference for some time. Rubbing is not
necessary for this charge difference to occur, but it usually increases the amount of charge
produced significantly. Triboelectrification is the term used for electrical charges generated
by frictional forces. Fibres can be ordered in a ‘triboelectric’ series such that each fibre type
becomes positively charged when rubbed with fibres below it in the series.

If polyester and wool fibres touch and then separate, the polyester fibres become negatively
charged and the wool fibres positively charged. If, however, polyester and polyethylene
fibres touch and separate, the polyester fibres become positively charged and the
polyethylene fibres negatively charged. The greater the separation of two fibres in the series,
the greater the charge generated by their contact. When the charge difference between the
two fibres reaches the electrical discharge potential of air (~3 × 106 Vm–1), the charge is
released by an electrical discharge accompanied by light and sound. The crackling noise
heard when an acrylic sweater is pulled over a cotton shirt and the spark seen when touching
a metal doorknob after walking across a carpet are examples of these discharges. The
electrical charging of fibres by friction is affected by the nature of the mechanical contact, the
ranking of the fibres in the triboelectric series, the humidity of the environment, and the
presence or absence of moisture on the fibres

All synthetic fibres are treated with a finish very shortly after their exit from the spinnerets.
This ‘spin finish’ contains lubricating oils and other components, including antistatic agents.
The high speeds of modern fibre processing would not be possible without these finishes.
Chemical processing aids in yarn making, knitting, weaving and nonwoven manufacture also
contain antistatic agents. Having accomplished their purpose, these processing aids are
usually removed during fabric preparation.

5.3.2 Effects of static charge on textiles

Static electricity can cause many processing problems for textile materials, especially those
made from hydrophobic synthetic fibres. In most dry textile processes, fibres and fabrics

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move at high speeds over various surfaces which can generate electrostatic charging from
frictional forces. This electrical charge can cause fibres and yarns to repel each other, leading
to ballooning. Fabrics and non-wovens are also affected by static charges, causing materials
handling problems. Consumers are aware of the clinging of garments and the small electrical
shocks caused by walking on carpets in low humidity conditions. Computers and other
electronic equipment can be damaged by static discharges. Safety requirements for many
textiles include antistatic limits at a defined relative humidity (mostly ranging from 65 to 25
%).

5.3.3 Mechanisms of antistatic finishes

The principal mechanisms of antistatic finishes are increasing the conductivity of the fibre
surface and reducing frictional forces through lubrication. Increasing conductivity produces a
lower charge buildup and a more rapid dissipation while increased lubricity decreases the
initial charge buildup. Antistatic agents that increase fibre surface conductivity form an
intermediate layer on the surface. This layer is typically hygroscopic. The increased moisture
content leads to higher conductivity. The presence of mobile ions on the surface is very
important for increased conductivity. The effectiveness of hygroscopic antistatic finishes
depends greatly on the humidity of the surrounding air during actual use.

Most non-polymeric antistatic finishes are also surfactants that can orient themselves in
specific ways at fibre surfaces. The hydrophobic structure parts of the molecule act as
lubricants to reduce charge buildup. This is particularly true with cationic antistatic
surfactants that align with the hydrophobic group away from the fibre surface, similar to
cationic softeners. The main antistatic effect from anionic and non-ionic surfactants is
increased conductivity from mobile ions and the hydration layer that surrounds the
hydrophilic portion of the molecule since the surface orientation for these materials places the
hydrated layer at the air interface.

5.3.4 Chemistry of antistatic finishes

5.3.4.1 Non-durable finishes

Both durable and non-durable effects are possible with antistatic finishes. Nondurable
antistatic agents are preferred for fibre and yarn processing finishes since ease of removal is
important. Other important requirements of spin finish and fibre lubricants are heat resistance
and oil solubility. This group of mostly hygroscopic materials includes surfactants, organic
salts, glycols, polyethylene glycols, polyelectrolytes, quaternary ammonium salts with fatty

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alkyl chains, polyethylene oxide compounds and esters of salts of alkylphosphonium acids.
The general requirements for non-durable antistites are;

❖ low volatility
❖ low flammability
❖ nonyellowing (heat stable)
❖ non-corrosive.

Like many other cationic materials, cationic antistats have an affinity for textile fibres and
can be applied by exhaustion processes. The last group of non-durable antistats is composed
of non-ionic compounds such as ethoxylated fatty esters, alcohols and alkylamines Mixtures
of cationic and non-ionic surfactants demonstrate synergistic antistatic properties. The non-
ionic materials provide increased moisture absorption, and the cationic products provide the
mobile counterions.

5.3.4.2 Durable antistats

Obtaining antistatic properties that are durable to repeated launderings from a single finish
application is difficult to achieve. The basic principle is to form a crosslinked polymer
network containing hydrophilic groups. Typically, polyamines are reacted with polyglycols
to make such structures. These polymers can be formed prior to application to fabrics, or they
can be formed in situ on the fibre surface after pad application. The amount of hydrophilic
character in the final polymer can be varied to meet individual requirements. The larger the
hydrophilic portion, the more moisture is absorbed and the greater the antistatic effect
obtained. Difficulties with crosslinked hydrophilic polymers include interferences with soil
release and soil-redeposition properties. Durable antistatic finishes include
polyhydroxypolyamines, polyalkylene and polyacrylic copolymers.

5.3.5 Conductive fibres

Electrically conductive fibres have been produced by several methods: dispersing carbon
particles or other antistatic agents in polymer melts prior to extrusion, depositing carbon
(epitropic fibres) or metallic (for example nano-silver) coatings onto fibre surfaces (for
example Ni, CuS), incorporating hydrophilic comonomers, and by fabricating fibres from
stainless steel, aluminum, or other metals. Although excellent durable control of static
electricity is achieved by incorporating these fibres into fabrics during spinning, knitting, or
weaving, these conductive fibres are always black or metallic in appearance and can be easily

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seen in most textiles, even at low levels of use (mostly 0.2–2 % wt/wt). This drawback limits
conductive fibres to industrial fabrics and very specialized apparel and carpeting.

Exercise 5

Answer the following questions by choosing the best alternatives.

1. One of the following is not a microbe or microorganism.

A) Bacteria B) Fungi C) Algae D) Plants
2. The negative effect on the vitality of microorganisms generally referred____
A) Antibiotic B) Antimicrobial C) Antiseptic D) Antifungal
3. _____________fibres are more susceptible to bacterial attack than synthetic fibers.
A) Cellulosic fibres B) Nylon fibres C) Acrylic fibres D) Polyester fibres
4. __________provides a suitable environment for microbial growth on cotton fabrics.
A) High temperature and moisture B) Low temperature and moisture
C) High temperature and low moisture D) Low temperature and high moisture
Answer: A
5. One of the following is not a synthetic antimicrobial agent.
A) Silver B) Triclosan C) Polybiguanides D) Chitin
6. What is the effect of microbial growth on textile fabrics?
A) Pigmentation or discoloration B) Loss of fabric strength
C) Emission of obnoxious odours D) All of the above
7. What is the effect of microbial growth on humans?
A) Transmit infections B) Allergic reactions C) Skin irritation D) All of the above
8. _________are the two types of antimicrobial finishes based on their mode of attack
on microbes.
a) Bound and non-bound type mechanism b) Controlled release and bound type
mechanism c) Bacteriostats and fungicides d) Biocides and antimicrobials
9. ____________ antimicrobial finish can control only those microbes present on the
fibre surface and not in the surrounding environment.
a) Controlled release b) Biostats c) Bound type d) Fungistats
10. ________ the three mechanisms by which antimicrobial finishes control microbial
growth?
a) Reducing moisture, blocking enzymes, destroying the cell walls
b) Blocking enzymes, preventing cell reproduction, reaction with the cell membrane
c) Destroying the cell walls, preventing cell reproduction, reducing moisture
d) Reducing moisture, blocking enzymes, preventing cell reproduction

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 11. __________ test method is used to determine antimicrobial activity by measuring the
diameter of the zone of inhibition.
a) Burial test b) Bacteria counting test c) Agar diffusion test d) ISO/DIS 20645
12. Which type of finish for insect resist interferes with the keratin digesting process of
the larvae.
a) Digestive poisons b) Nerve poisons c) Spinning lubricants d) Agricultural pesticides
13. What is the most significant market for insect resist finishes?
a) Upholstery fabrics b) Blankets c) Wall hangings d) Carpet industry
14. Where do dust mites live and proliferate?
a) Carpets and pillows b) Bedding and mattresses
c) Upholstery and quilts d) Curtains and towels
15. What is the simple protection from dust mites achieved by?
a) Repeated cleaning b) Insect resist finishes c) Non-leaching antimicrobial finishes d)
Biocides
16. Triboelectrification is;
A. The release of electrical charge by an electrical discharge accompanied by light and
sound.
B. The ability of fibres to conduct electricity efficiently.
C. The electrical charging of fibres by frictional forces.
D. The ability of fibres to repel each other due to electrical charge buildup.
17. The significance of antistatic finishes for synthetic fibres is_________
A. They contain lubricating oils and other components.
B. They improve the conductivity of the fibre surface.
C. They prevent static electricity from causing processing problems for textile materials.
D. Both A and C.
18. One of the following is the effect of static charge on textiles?
A. It causes fibres and yarns to attract each other.
B. It leads to a more rapid dissipation of charge buildup.
C. It causes fibres and yarns to repel each other, leading to ballooning.
D. It increases the charge buildup on the surface of the fibre.
19. What is the principal mechanism of antistatic finishes?
A. Increasing the conductivity of the fibre surface.
B. Reducing frictional forces through lubrication.
C. Both A and B.
D. None of the above.
20. Which of the following is true about non-durable antistatic agents?

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A. They are preferred for fibre and yarn processing finishes.
B. They can cause fibres and yarns to repel each other.
C. They are usually difficult to remove.
D. They must be heat resistant and oil soluble.
21. What are the general requirements for non-durable antistats?
A. High volatility, high flammability, and yellowing.
B. Low volatility, low flammability, and non-corrosive.
C. High volatility, low flammability, and heat stable.
D. Low volatility, high flammability, and corrosive.
22. Which of the following is not affected by static charges?
A. Consumers. B. Textile materials.
C. Computers and other electronic equipment. D. Hydrophilic fibres.
23. What is the significance of the humidity of the surrounding air during actual use of
hygroscopic antistatic finishes?
A. It affects the ease of removal of the antistatic finish.
B. It affects the heat resistance of the antistatic finish.
C. It affects the oil solubility of the antistatic finish.
D. It affects the effectiveness of the antistatic finish.
24. What is the main antistatic effect from anionic and non-ionic surfactants?
A. Increased conductivity from mobile ions and the hydration layer that surrounds the
hydrophilic portion of the molecule.
B. Reduced conductivity from mobile ions and the hydration layer that surrounds the
hydrophobic portion of the molecule.
C. Increased frictional forces through lubrication.
D. Increased charge buildup on the surface of the fibre.

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 CHAPTER SIX

HAND MODIFICATION OF TEXTILES

6.1 Soft Finishes

Hand or Handle are the terms used to describe how a fabric drapes around an object or feels
to the touch. During preparation, textiles can become embrittled Because natural oils and
waxes are removed. Finishing with softeners can overcome this deficiency and even improve
on the original suppleness. Chemicals that accomplish this are called Handbuilders. To
change the hand properties of a fabric, we can apply mechanical, physical, chemical or
combined techniques. When the hand is made to drape more or to feel silkier, the fabric is
said to have been softened. Chemicals that do this are called Softeners. The hand of a fabric
is a subjective sensation felt by the skin when a textile fabric is touched with the fingertips
and gently compressed.

The softeners are mainly used for textile processing for the following:

➢ To provide desired softness often described as smooth, supple, supersoft, elastic, dry
or slashy.
➢ To influence or to improve technical properties, namely, antistatic, hydrophilicity,
elasticity, sewability and rubbing fastness.
➢ To confer natural touch on synthetic fibres and to improve their wearing comfort by
the regulation of moisture content or smoothness

The perceived softness of a textile is the combination of several measurable physical

phenomena such as

➢ Elasticity,
➢ Compressibility and
➢ Smoothness
It is also worth noting that no standard methods have been developed or established to
determine exactly what the softness of a fabric is. This evaluation is almost personal and
carried out on the basis of the operator’s experience. It is possible to distinguish the following
types of softness:
➢ Surface softness
➢ Surface smoothness
➢ Elasticity (compression and stretching)

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Many softeners are derived from naturally occurring Fats, Oils and Waxes. Sources and
reactions of fats, oils and waxes. Some softeners are derived from synthetic raw materials.
Many of the compounds that work as softeners also function as surfactants or water
repellents.

6.1.1 Reasons for using softener.

Mechanical and chemical processes, Resin finishing of textile material and soaping of textile
material that make the surface of the material harsh. As consumers are much more caring
about the touch of textile material using softeners to obtain the required hand is mandatory.
With chemical softeners, textiles can achieve an agreeable, soft hand, better drape, and
pliability, softness, flexibility and achieve the desired quality of fabric handle. Other
properties improved by softeners include the feeling of added fullness, antistatic properties,
and sew-ability. Disadvantages sometimes seen with chemical softeners include reduced
crock fastness, yellowing of white goods, changes in hue of dyed goods and fabric seam
slippage.

6.1.2 Classification of textile softeners according to their ionogenity

Based on charge on parent molecule/ ionic natures softener can be classified as anionic,
cationic, non-ionic, and amphoteric Softeners. They may also silicone (Silicone Emulsions)
type or Polyethylene Softeners

Classification according to iogenity

Ionic activity Electric charge

Cationic At acid pH's very positive Quaternary ammonium salts, Amino-

amide, Cyclic cationics (e.g.
imidazolines)

Anionic Negative Sulphate, Sulphonates

Non-ionic No charge Ethoxylates, Esters, Polyethylenes,

Silicones, Waxes

Silicone At acid PH slightly positive

softeners

Amphoteric Dependent on PH slightly negative Sulphobetaines, Fatty amino acids,

to slightly positive Amine oxides

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6.1.3 Softening Mechanism

Softening agents behave like lubricants facilitates fibre sliding within the fabric structure,
reduce the coefficient of friction between fibers yarns, and fabric and giving the sensation of
softness. Softeners provide their main effects on the surface of the fibers. The physical
arrangement of the usual softener molecules on the fiber surface is shown in Fig below. They
orient themselves toward the fiber creating a new surface consisting of molecular chains that
provide the characteristic softening and lubricity. Small softener molecules penetrate the fiber
and provide plasticisation of fiber forming polymer. It depends on the ionic nature of the
softener molecule and the relative hydrophobicity of the fiber surface.

Cationic softeners orient themselves with their positively charged ends toward the partially
negatively charged fiber (zeta potential), creating a new surface of hydrophobic carbon
chains that provide the characteristic excellent softening and lubricity. Anionic softeners, on
the other hand, orient themselves with their negatively charged ends repelled away from the
negatively charged fiber surface. This leads to higher hydrophilicity but less softening than
with cationic softeners. The orientation of non-ionic softeners depends on the nature of the
fiber surface, with the hydrophilic portion of the softener being attracted to hydrophilic
surfaces and the hydrophobic portion being attracted to hydrophobic surfaces. Non-ionic
softeners are applied to synthetic fibers & their blends like polyester and polyester/cotton
blends.

Figure 6: 1Schematic orientation of softners on the fibers surface(a) cationic softner and (b) non
ionic softner at fiber surface. Non ionic softner at (c) hydrophobic and (d) hydrophilic fiber surface

6.1.4 Requrements of softners

Softners used in textiles should fulfill the following basic requirements

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 ➢ Easy to apply and good compatibility with other chemicals.
➢ Minimum change in shade of the material and color fastness of dyed material
➢ No yellowing of dyed and finished material.
➢ Nonvolatile and non-toxic
➢ No pungent smell
➢ Easily biodegradable and durable to washing and dry cleaning
➢ Available in forms convenient to handle: stable liquid, predilutable and dosable
➢ stable in high temperature
➢ Low foaming and shear stable; does not deposit on rollers
➢ Preferably applicable by exhaust processes with good properties
➢ Good price–performance relationship

6.1.5 Products type & their chemistry

Most softeners consist of molecules with both a hydrophobic and a hydrophilic part.
Therefore, they can be classified as surfactants (surface active agents) and are to be found
concentrated at the fiber surfaces. Most softeners have a low water solubility. Therefore,
softening products are usually sold as oil in water emulsions containing 20–30 % solids. The
softener molecules typically contain a long alkyl group, sometimes branched, of more than 16
and up to 22 carbon atoms, but most have 18 corresponding to the stearyl residue
(CH3(CH2)16COOH). Exceptions to this molecular structure are the special categories of
silicones and polyethylene softeners. About one-third of the softeners used in the textile
industry are silicone based.

6.1.6.1 Salient features of cationic softeners

They are Quaternary ammonium compounds with best softness effect due hydrophobic
groups are oriented away from fiber surface. They provide Improved washing fastness by
half to one rating, improved tensile properties, Poor wetting properties & sew-ability and
durable to laundering. They can be applied by both exhaustion (High liquor to goods ratio)
and Pad dry method. Cationic softeners are easily removed from wastewater by adsorption
and by precipitation with anionic compounds. The disadvantages of cationic softeners
includes non-compatibility with anionic products (Anionic Fluorescent Brightening agents)
because precipitation takes place because of positive ion, may react with residual chlorine
from bleach bath, attracting soil because of static charge generated at hydrophobic portion
and cause yellowing upon exposure to high temperatures because of free amine group,

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adversely affect the light fastness of direct and reactive dyes, toxic to fish and poor
biodegradability.

6.1.6.2 Salient features of anionic softeners

The chemical nature of anionic softeners are Sulphates and Sulphonates which are heat stable
at normal textile processing temperatures. Anionic softeners are Compatible with other
components of dye and bleach baths, easy to wash off and provide strong antistatic effects.
They provide good rewetting properties because their anionic groups are oriented outward
and are surrounded by a thick hydration layer. Anionic softeners especially used for special
applications, such as medical textiles, or in combination with anionic fluorescent brightening
agents. They are inferior in softness than cationic softeners, sensitive to water hardness and
electrolytes in finishing bath, less durable to laundry and dry cleaning, cannot be applied by
exhaust method and can be applied by Pad-dry only.

6.1.6.3 Non-ionic softeners based on Polyethylene

Polyethylene can be modified by air oxidation in the melt at high pressure to add hydrophilic
character (mainly carboxylic acid groups & to a lesser degree fatty alcohols). Emulsification
in the presence of alkali will provide higher quality, more stable products. It shows high
lubricity (reduced surface friction), stable to extreme pH conditions, stable to heat at normal
textile processing condition, cheaper in price, with most textile chemicals and can be easily
applied by pad dry.

However, it has poor durability to dry cleaning, poorest softness among all types of softeners,
wet and crock fastness are adversely affected and cannot be applied by exhaust because of
poor affinity.

6.1.6.4 Ethoxylated Nonionic Softeners

These poly glycol ethers are synthesized by the addition of ethylene oxide to fatty alcohols,
carboxylic acids, esters, amides or amines. They are surfactants and often used as antistatic
agents, as components of fiber spin finishes. They provide high substantivity and
hydrophilicity, non-yellowing, low softening effect and lubricity and generate foam during
processing.

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6.1.7 Silicon Softeners

Silicon softeners are both Non-ionic and cationic softeners provide very high softness &
unique hand feel because of low Tg (100C) & high molecular flexibility of silicon chain, high
lubricity, good sew-ability, elastic resilience, crease recovery, good abrasion resistance and
tear strength and good temperature stability. The mechanism of softening by silicone
treatment is due to a flexible film formation. The reduced energy required for a bond rotation
makes the siloxane backbone more flexible. The deposition of flexible film reduces interfibre
and interyarn friction. silicone finishing of textile produces an exceptional soft handle
combined with other properties such as:

➢ Smoothness

➢ Greasy feel

➢ Excellent body

➢ Improved crease resistance

➢ Improved tear strength

➢ Improved sewability

➢ Good antistatic and antipilling properties

Because of their inorganic–organic structure and the flexibility of the siloxane bonds,
silicones have the following unique properties:

➢ Thermal/oxidative stability

➢ Low-temperature flowability

➢ Low change of viscosity with temperature

➢ High compressibility (5) Low surface tension (spreadability)

➢ Low fire hazard

Silicones exhibit some unique properties including thermal oxidative stability, low
temperature flowability, low viscosity change against temperature, high compressibility, low
surface tension, hydrophobicity, good electric properties and low fire hazard because of their
inorganic–organic structure and the flexibility of the silicone bonds. One of the key features
of silicone materials is their effectiveness at very low concentrations. Very small amounts of
silicones are required to achieve the desired properties, which can improve the cost of textile
operations and ensure a minimum environmental impact

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Organo-modified silicones

Dimethylsiloxane homopolymers show a very poor softening and hardly reduce fibre
wettability. This is due to poor interaction with the fibre and consequent uneven distribution
on the surface. Methyl oils or polydimethylsiloxanes are the group of silicones first used for
the softening of textile materials. Besides softeners, they are used as: wetting agents; water
repellents; lubricants in spinning, winding and sewing; defoamers and as agents in
elastomeric finishes and coatings.

Aminosilicones

Amino oils or aminosilicones clearly dominate the current softeners market due to their
elegant handle. More than 90% of all commercially available aminosilicone softeners are
aminoethylaminopropyl silicones. Aminosilicones are prone to thermo-yellowing; the extent
of colour changes depends on the type of the amino side chains, amino content, curing
temperature and time.

Epoxysilicones

Epoxysilicones, due to polar interactions between polymer side chains and cellu lose, are
much better softeners than dimethylsiloxanes and give measurable hydro phobic effects.
They have strong interactions with the fibre, giving it a durable finish. Aminosilicones are
superior to epoxysilicones, most probably due to better ori entation and better distribution
on the surface due to strong dipole–dipole hydrogen bonding and electrostatic interactions
with the fibres, especially with cellulose

Carboxysilicones

These types impart a silky finish, along with a bounciness and bulkiness to the fibre. The
emulsions are nonyellowing and are generally applied to nylons and polyesters.

Hydroxysilicones

They impart an elastomeric feel to the fibre.

Hydrophilic silicones

The first generation of hydrophilic silicones, available commercially for decades, contains
polyether, namely, polyethyleneoxide (PEO) and/or polypropyleneoxide, aminopolyether
siloxane and polyether siloxane. These silicones with polyglycol groups show excellent
hydrophilicity and act almost as wetting agents. The tendency of yellowing is lower and

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almost zero for some structures. However, the bulky PEO groups disturb the ideal orientation
on the fibre, resulting in inferior softness as compared to classical aminosilicones.

6.1.7.1 Silicon Softeners on Polar Surface

Provide very high softness & unique hand feel because of low Tg (100C) & high molecular
flexibility of silicon chain.

C- Fiber surface with partially negative charge; b- amino group with partially cationic charge;
a- hydrophobic group (Poly dimethyl siloxane chain).

6.1.7.2 Silicon Softeners on non-polar Polyester

Provide very high softness & unique hand feel because of low Tg (100C) & high molecular
flexibility of silicon chain.

d- Hydrophobic Fiber surface (PET); b- amino group with partially cationic charge; a-
hydrophobic group (Poly dimethyl siloxane chain).

Having good durability, they provide high degree of permanence for those products that form
cross-linked films. In textile finishing, silicones are also used as water repellents, coatings
and as de-foamers. Sometimes contain volatile siloxane oligomers they may cause pollution
problems along with volatile emulsifiers in the waste air from stenter machine.

Measurement of softness

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The American Association of Textile Chemists and Colorists has published guidelines for
subjective hand evaluation (AATCC Evaluation Procedure 5, 1990) (AATCC, 1997)

Handle-O-Meter

In Handle-O-Meter (ASTM, 2006), the stiffness of fabric is determined by measuring the

force required to push a specimen (maximum 20 cm or 8in.) into a slot of predetermined
width (two flat plate supports separated by a fixed distance) made with a metal blade
(attached to a motor driven beam) working at a predetermined capacity.

KTU-Griff-Tester

geometrical behaviour of a specimen can be described by referring to the model where the
variation of the outer contour of a disc-shaped specimen is approximated by the sine-curve
function.

6.2 Hand building finishes

The purpose of applying hand builders is to add bulk, weight, or stiffness to a fabric. For
some fabrics, this change must be permanent and withstand washing and dry-cleaning. In
other applications, the change is temporary, so hand builders are classified as either durable
or nondurable.

6.2.1 Hand building classification

Depending on the effect on fabric handle, handle modifier finishes can be roughly divided
into two groups:

1. The first group provides an increase in fullness, which is a feeling of increased

bulk or weight.

2. The second group provides stiffness or a resistance to bending

Fabrics needing hand building finishing are:

➢ Starch finishing after washing of garments made particularly form light weight
fabrics.
➢ Table linen
➢ Fabrics having low ends and picks density.
➢ Interlining fabric for collars of shirts, suits, and other dress wear work wear
➢ Fabrics like apron, lab coats, window blinds, mattress cover, laces etc.

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6.2.3 Hand builder chemistry

6.2.3.1 Non-durable

Nondurable hand-building finishes lose their effect after one or two launderings. The two
major product types of nondurable handle builders are starch derivatives and polyvinyl
alcohol (PVA). Non-durable hand builders are use impart better over-the-counter appearance
to many fabrics. Starched fabrics have a greater consumer appeal than limp fabrics. They
also improve the handling of flimsy fabrics in cutting and sewing operations since stiff
fabrics are easier to manipulate than limp fabrics. Another reason for nondurable
handbuilders is that some fabrics are traditionally expected to be stiff. For example,
consumers expect Denim jeans to be stiff and boardy. They expect jeans to break in, become
soft and comfortable and fade with repeated washing. Most water-soluble film forming
polymers can serve as non-durable hand builders. However, starch and polyvinyl alcohol are
the ones used most often.

1. Starch

Thin boiling starches and dextrin are preferred as finishes because high solids solutions can
be prepared without the viscosity becoming so high that they cannot be applied with
conventional padders. The starches used for finishing do not retrograde.

Figure 6: 2 Chemical structure of starch

The most outstanding properties of starch are:

➢ Cost effective
➢ Easily available
➢ Highly viscous (lesser amount of starch in paste)

The starch is available from different sources and has varied properties. Some of the sources
of starches are wheat, potato, rice, maize, sago, etc. The principal property of all starch grains

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is that at a certain temperature during an aqueous heating cycle, the cell wall of the grain
bursts and the starch becomes gelatinised, producing a viscous liquid. Each individual starch
has a different gelatinisation temperature and viscosity characteristics. The presence of other
components in the starch mixture can alter the film properties, and it is normal for the final
processing liquor to be a mixture. The final fabric property depends on a number of factors,
as well as the effect of the individual starches. Starch is insoluble in cold water; it only swells
when it comes in contact with water. The best-known chemically produced solubilised
product is dextrin or British gum, which has low viscosity and good adhesive properties

The criteria for the selection of starch are:

➢ Stickiness during drying and calendering

➢ Ease of penetration into fabric
➢ Transparency of film formed on dyed material
➢ Effects of crushing
➢ Smoothness of starched fabric

2. Polyvinyl Alcohol

When used as finishes, fabric stiffness can be achieved with higher molecular weight
polymers at lower add-ons. However, increased bulk and weight can be obtained with higher
add-ons of lower molecular weight polymers without over stiffening the fabric.

Figure 6: 3 Polyvinyl alcohol chemical structure

Naturally occurring starch requires a long boiling to break the starch wall. Modified thin- or
short-boiling starches are more popular because:

➢ Less variation of viscosity with concentration

➢ Take-up is well controlled
➢ Shorter boiling time
➢ More adhesion to the fabric

6.2.3.2 Durable

Hand building finishes that retain their stiffening and fullness effects after repeated
launderings are durable hand builder finishes. Durable hand builders are used to improve the

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aesthetics of rayon fabrics. Fabrics made from conventional rayon fibers are limp and raggy
and are very much improved with melamine resins. Durable hand builders are also used to
increase a fabric's weight and to improve toughness and abrasion resistance. Aqueous
emulsions of polymers that form water-insoluble films on the fiber surface when dried can be
used as durable hand builder. Thermosetting and thermoplastic polymers can serve as
durable hand builders. Cost, ease of application and ultimate fabric properties are factors to
consider when choosing the appropriate material from various available alternatives.

1. Thermosetting Polymers

Urea/formaldehyde and in particular, melamine/formaldehyde are thermosetting resins that

stiffen fabric. While used primarily for crosslinking cellulosic fibers, they can also be used on
other fibers as handbuilders.

a. Melamine/Formaldehyde

These resins form three-dimensional cross-linked polymers that impart bulk and resilience to
fabrics. They are used on synthetic fibers, e.g. polyester, nylon acrylics, as well as cellulosics
and are durable to repeated laundering and dry cleaning.

b. Urea/Formaldehyde

Alkylated U/F's, e.g. butylated U/F are thermosetting hand builders. They are often used on
rayon fabrics. However, the U/F's are not as durable to repeated laundry as are the M/F's.

2. Thermoplastic Polymers

Stable water dispersion of high molecular weight thermoplastic polymers serves as durable
hand builders. Vinyl and acrylic polymers are available as latexes or stable water dispersions
and come as very high molecular weights materials with a wide range of Tg's. They can also
be tailored to be crosslinkable. The property of the dried film mainly depends on the
combination of monomers used in the polymerization step. Film hardness, stiffness,
flexibility, elasticity, adhesiveness, color, solvent resistance etc. are all a function of the
monomers. As finishes, film properties of the latex can be used to engineer the fabric hand.
For example, polymers with a very high Tg add stiffness without adding weight. Poly
(methylmethacrylate) latexes dry down to form very stiff films. So, it doesn't take much add-
on to stiffen a fabric. On the other hand, ethyl or butyl acrylate polymers dry down into
softer, flexible films. They can be used to build-up weight without making the fabric
excessively stiff.

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6.3 Bio finishing

6.3.1 Bio Polishing

Bio polishing is a finishing process that improves fabric quality by mainly reducing fuzziness
and pilling property of cellulosic fibre. The objective of the process is elimination of micro
fibrils of cotton through the action of cellulase enzyme. The main characteristics imparted to
the fabric during biopolishing treatment are cleaner surface, lustre, softer feel, and tendency
of the fabric to pill ends. This mode of finishing has been specifically developed to achieve
clearer pile on terry towel goods. A treatment with a cellulase enzyme, gives clearer look to
the pile, improves absorbency and softness . This process is done after de-sizing. This results
in removal of surface hairs which are responsible for improvement in the hand and feel of the
fabric due to surface etching.

Bio-polishing treatment conditions are more easily controlled in batch processes for which
winches, jiggers, jet or overflow machines are suitable. Bio-polishing is best carried out after
bleaching and before dyeing. Bio-polishing give cleaner appearance to the garment besides
wash down effect. If it was sulphur or pigment dyed goods or ring dyed fabric, wash down
effect as well as cleaning of fabric surface could be obtained. It results into surface hair
removal, reduced pilling, better print registration and color brightness. In conventional
process protruded fibers are removed by singeing process and smoothness imparted by
chemical treatment. The conventional methods are temporary, and chemicals are removed
after few washing and fuzz is formed.

The fuzz on the surface spoils the fabric appearance and generates customer’s dissatisfaction
whereas bio-polishing is permanent and it not only keeps the fabric in good condition after
repeated washing but also enhances feel, color, drapability etc consequently products become
more attractive to the customer and fetch better prices.

6.3.1.1 Process condition

Typical process conditions for an industrial bio-polishing/ de-pilling process are pH 4.5–6.0,
temperature 45–65°C, liquid ratio 3 : 1–20 : 1 and an dwell time of 15–60 minutes. The
dwell time depends on the type of machine, the liquid ratio, the fabric and the desired effect.

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 Figure 6: 4 Biosingieng

Advantages of Bio-polishing:

➢ Improved pilling resistance

➢ A clearer, lint and fuzz-free surface structure
➢ Improved drape ability and softness
➢ The effects are durable
➢ Slight improvement in absorbency
➢ Fashionable effects on fabric like distressed look of denim
6.3.2 Bio-denim Washing

In enzyme washing, cellulase enzymes are used. Hydrolysis of the cellulose is catalysed by
cellulase. It causes the surface fibres to become weakened and later they get removed when
there is fabric to metal abrasion. Another use of cellulase enzyme is in the fading of denims.
Denims are manufactured from indigo dyed warp yarns. The dyes are mainly absorbed on the
surface of the fibre, a phenomenon technically termed as ring dyeing. The fibre surface
etching with cellulase enzymes results in exposure of the un-dyed core of the fibres which
gives a faded look to the denim. The dye removal is further facilitated by the mechanical
abrasion. Earlier the effect was obtained by washing denim with pumice stones. Pumice
stones are soft, light and porous in nature. About 1–2 kg pumice stones per pair of jeans were
used to get the desired worn-out look.

Though stone washing gives the desired result, but it has got several disadvantages. The
major problem with stone washing is that lot of sludge gets deposited in the effluent tank due

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to worn out of pumice. The sludge has to be separated from effluent water and disposed off.
The use of stones was, therefore, replaced by cellulase enzymes.

Figure 6: 5 Pumice stone

Cellulase treatment of denim fabric has some disadvantages, too. There may be chances of
back staining in cellulase treatment. To remove the back staining, the garments are rigorously
washed. However, this adds to usage of water for the washing. When indigo dye is released
to the wash liquor during washing, the solution turns dark blue. Indigo dye has two amino
groups which are capable of getting protonated in an acidic media. Due to protonation, the
dyestuff gains an overall positive charge; on the contrary, cellulose maintains its negative
charges in an aquoeus media. Positive and negative charges attract one another in solution.
Therefore, in acidic pH the affinity of indigo for cotton increases.

Some of this indigo redeposit on the whiter parts of the denim fabric which spoils the color
contrast of the stone wash effect. This phenomenon is known as “back-staining”. Back-
staining problem is more evident with acid cellulase. The use of neutral cellulase is
recommended to control the back staining problem because of their better control in
resistance to back staining. The temperature and the pH used are specific to the type of
cellulase employed. Usually, neutral cellulase are applied at pH 6–7, while acid cellulase are
applied at pH 4.5–5.5.

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 Figure 6: 6 Back staining on denim

6.3.3 Enzymatic Ageing

The finishing of denim garments by pumice stones (stone washed garments) to achieve an
aged or worn appearance has been radically improved by the application of cellulase enzymes
(also called cellulase washing or bio-stoning). This stonewash effect is due to abrasion of the
fabric thereby locally removing the surface-bound indigo dye and revealing the white interior
of the yarn. In the traditional stonewash process, abrasion is caused by pumice stones and by
garments rubbing against the washer drum. The pumice stones damage the washer drum and
reduce the fabric strength due to abrasion.

The application of cellulase prevents damage to the washing machine, eliminates the need for
disposal of used stones and results in an improved quality of wastewater because of the
absence of pumice stone dust. Owing to the absence of stones (several kilograms) the
garment load may be increased up to 50% resulting in increased productivity. The use of
cellulase results in a softer fabric and, because of the reduced abrasion of the fabric, an
increased strength compared to the traditional stonewash process. The application of cellulase
is, owing to the global market size for stonewashed denim garments. This is a very successful
application of enzymes in the textile industry. The cellulase enzymes need to be inactivated
after the desired stonewash effect is obtained. Insufficient inactivation will result in extended
degradation of cellulose and therefore an undesirable strength loss and weight reduction.

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 Figure 6: 7 Stone washing effect on denim

6.3.4 Bio-Carbonizing

Polyester/cellulosic (90/10), blends after dyeing and/ or printing are occasionally treated with
strong solution of sulphuric acid to dissolve cellulosic component. The resultant goods are
soft and have a peculiar fluffy feel. This process is risky due to highly corrosive acid that is
also difficult to treat in an Effluent Treatment Plant (ETP). The goods are treated with
cellulase enzyme-based formulation to achieve dissolution of cellulosic fibres. In the bio-
carbonizing process the goods are treated with a cellulose enzyme-based formulation to
achieve dissolution of cellulosic component. The goods are padded in a warm solution of this
product and batched on a roll under normal conditions and are washed off after 12–16 hours.
This process offers an eco-friendly option against the use of strong acids.

Exercise 6

Answer the following questions by choosing the best alternatives

1. The purpose of applying hand builders to a fabric is:

a. To make the fabric thinner. b. To make the fabric softer.
c. To add bulk, weight, or stiffness to the fabric d. To add more colors to the fabric
2. The type of fabrics that need hand building finishing is;
a. Heavy weight fabrics b. Light weight fabrics
c. Both heavy and light weight fabrics d. None of the above
3. Which of the following is not a fabric that needs hand building finishing?
a. Table linen b. Fabrics with low ends and picks density

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c. Cotton t-shirts d. Interlining fabric for collars
4. What is the difference between durable and non-durable hand building finishes?
a. Durable finishes are the same with non-durable finishes in terms of permanence.
b. Durable finishes are temporary, while non-durable finishes are permanent.
c. Durable finishes retain their effect after repeated launderings, while non-durable finishes
lose their effect after one or two launderings.
d. Non-durable finishes are used to improve the aesthetics of rayon fabrics, while durable
finishes are used to add bulk or weight to a fabric
5. Which of the following is not a reason for using non-durable hand builders?
a. To improve the handling of flimsy fabrics in cutting and sewing operations
b. To make jeans soft and comfortable.
c. To add bulk or weight to a fabric.
d. To make a fabric more breathable.
6. What are the two major product types of non-durable handle builders?
a. Cotton and wool b. Polyester and silk
c. Starch derivatives and polyvinyl alcohol (PVA) d. Acrylic and rayon
7. Which of the following is not one of the outstanding properties of starch?
a. Cost effective b. Easily available c. Highly viscous d. Soluble in cold water
8. ___________ is the principal property of all starch grains?
a. Bursting at a certain temperature during an aqueous heating cycle and become gelatinized.
b. Insolubility in cold water
c. Having different gelatinization temperature and viscosity characteristics.
d. Deriving from the same plant source.
9. Which of the following is a reason for using nondurable hand builders?
A. To make fabrics more transparent B. To reduce the weight of heavy fabrics
C. To improve the handling of flimsy fabrics in cutting and sewing operations.
D. To make fabrics more flexible.
10. Which of the following is a type of nondurable hand builder?
A. Urea/formaldehyde B. Melamine/formaldehyde C. Polyvinyl alcohol D. Silicone
11. __________ is the best-known chemically produced solubilized product that is used
as a nondurable hand builder.
A. Dextrin B. Polyvinyl alcohol C. Melamine/formaldehyde D. Urea/formaldehyde
12. What is the objective of the biopolishing process?
A) To increase fuzziness and pilling property of cellulosic fiber.
B) To eliminate micro fibrils of cotton through the action of cellulose enzyme.
C) To reduce the quality of the fabric surface.

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D) To enhance the surface hair growth of the fabric.
13. What are the main characteristics imparted to the fabric during biopolishing
treatment?
A) Fuzziness and pilling property.
B) Cleaner surface, luster, softer feel, and tendency of the fabric to pill ends.
C) Harder feel and decreased absorbency.
D) Shiny surface and better print registration.
14. What is the best time to carry out bio-polishing?
A) Before bleaching B) After dyeing C) After singeing process D) After printing
15. What are the advantages of bio-polishing?
A) Increased fuzziness and pilling resistance B) A clearer, lint and fuzz-free surface structure
C) Decreased drape ability and softness D) Temporary
16. What causes the fading of denims in bio-denim washing?
A) Mechanical abrasion B) Bleaching C) Chemical treatment D) Increased absorbency
17. What is the major problem with stone washing?
A) The deposition of sludge in the effluent tank B) Excessive use of water for washing
C) Back staining D) None of the above
Answer: A
18. What is back staining in enzymatic ageing?
A) The phenomenon of getting the faded look of denim. B) The removal of dye from denim.
C) The spoiling of the color contrast of the stone wash effect. D) The process of cellulase
enzyme washing.
19. Which cellulase enzyme is recommended to control the back staining problem?
A) Acid cellulase B) Neutral cellulase C) Basic cellulase D) Alkaline cellulase
20. What is bio-stoning?
A) The finishing of denim garments by pumice stones.
B) The finishing of denim garments by cellulase enzymes.
C) The finishing of silk garments.
D) The finishing of woolen garments.
21. Why do textiles become embrittled during preparation?
a) Due to the addition of natural oils and waxes b) Due to the removal of natural oils and
waxes
c) Due to mechanical processes d) Due to chemical processes
22. ___________ are properties textiles that can be influenced or improved by softeners
in processing?
a) Hydrophobicity and elasticity b) Antistatic, hydrophilicity and sewability

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c) Rubbing fastness and fullness d) All of the above
23. The perceived softness of a textile based on?
a) Elasticity, compressibility and smoothness b) Hand and handle
c) Surface softness, surface smoothness and elasticity d) Moisture content and smoothness
24. Why is it difficult to determine the softness of a fabric?
a) There are no standard methods developed to measure it
b) Softness is a purely subjective sensation
c) Both a) and b) d) None of the above
25. What are the sources of many softeners?
a) Synthetic raw materials b) Fats, oils and waxes c) Water repellents d) Surfactants
26. What are the disadvantages of chemical softeners?
a) Reduced crock fastness b) Yellowing of white goods c) Changes in hue of dyed goods
d) All of the above
27. How do softening agents behave?
a) They reduce the coefficient of friction between fiber c) They provide the sensation of
softness b) They facilitate fiber sliding within the fabric structure d) All of the above
28. What is the mechanism of softening by silicone treatment?
A) Film formation B) Bond rotation
C) Chemical reaction D) None of the above
29. Which type of silicone softener imparts a silky finish, bounciness, and bulkiness to
the fiber?
A) Organo-modified silicones B) Aminosilicones
C) Carboxysilicones D) Hydroxysilicones
30. What is the most commonly used amino silicone softener?
A) Polyether B) Polypropyleneoxide
C) Aminoethylaminopropyl silicones D) Polydimethylsiloxanes
31. ______________is a type of silicone softener which is prone to thermo-yellowing?
A) Organo-modified silicones B) Aminosilicones
C) Epoxysilicones D) Carboxysilicones
32. What is the unique property of silicones that makes them effective at very low
concentrations?
A) Inorganic-organic structure B) High compressibility
C) Low surface tension D) All of the above

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 CHAPTER SEVEN

OTHER CHEMICAL FINISHES

7.1 Anti-pilling finishes

Pilling is a phenomenon exhibited by fabrics formed from spun yarns (yarns made from
staple fibres). Pills are masses of tangled fibers that appear on fabric surfaces during wear or
laundering. Fabrics with pills have an unsightly appearance and an unpleasant handle. Loose
fibers are pulled from yarns and are formed into spherical balls by the frictional forces of
abrasion. These balls of tangled fibers are held to the fabric surface by longer fibers called
anchor fibers. Fabrics made from cotton, wool or rayon do not usually display pilling
problems since the anchor fibers are easily broken and pills fall from the fabric soon after
they are formed. When fabrics are made from polyester or nylon spun yarns, however, the
stronger anchor fibers are not easily broken and the pills that are formed are not released
quickly from the fabric, leading to appearance problems.

In the case of fiber blends, such as cotton and polyester, the pilling can be particularly severe
with the weaker cotton fibers easily entangled with and then held to the fabric surface by the
stronger polyester fibers. The same is true for blends of synthetic fibers with wool. Pills on
one fabric can contain fibers from other fabrics that were involved in the abrasion, for
example, pills on pajamas may contain fibers from the bed sheets. Fabric and yarn
construction play a major role in pilling. Tighter constructions (woven versus knit, high twist
versus low twist) show less problems than do looser constructions. Although pilling affects
only the fabric aesthetics and does not cause any functional problems, it is important to
minimise or prevent pilling in order to maintain customer satisfaction.

7.1.2 Pilling mechanism

The number of pills on a fabric surface at any time is the result of a dynamic equilibrium
between two opposing effects, pill formation and pill wear off. Through abrasion, loose fibers
are pulled to the fiber surface and form a layer of ‘fuzz’. The loose fibers are then entangled
by the applied abrasion to form pills. As the abrasion continues, the anchor fibers are
eventually broken, and the pills break off. When the rate of pill formation and the rate of pill
break off are equal, an equilibrium state exists. When the abrasion lasts long enough, the
source of loose fibers becomes exhausted, the rate of pill formation decreases, and the total

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number of pills decreases. As can be seen, after an initial period of pill growth, the total
number of pills is maximized and then decreased as pill loss increases.

Figure 7: 1 Pilling mechanism.

The key fibre property that determines pill loss is the flex life of the anchor fibres. The higher
the flex life, the longer the pill remains on the fabric surface. The specific details of these
curves depend on fabric and yarn characteristics as well as on the mechanical forces acting on
the fabric.

7.1.2 Mechanisms and chemistry of anti-pilling finishes

Several chemical finishing approaches have been taken to prevent pills from accumulating on
fabric surfaces. The first approach is to prevent loose fibres from forming the initial ‘fuzz’ by
applying polymeric coatings that bind the fibres into the fabric surface. These finishes
typically include friction reducing lubricants to minimize abrasion damage. The most useful
polymers are acrylic copolymers since they can be easily modified to yield tough, flexible
films with good adhesion to fibre surfaces. The second chemical finish approach to reduce
pilling is to cause the pills to fall off the fabric as soon as they are formed. This can be
accomplished by reducing fibre strength. For synthetic fibres, changes in the polymer
structure can be made prior to extrusion. A third approach to reducing pilling tendency is
applicable to 100 % cotton fabrics. Enzymatic finishes by using cellulase enzymes during wet
processing can remove enough of the loose fibres in the yarns so that pilling is greatly
reduced.

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7.2 Non-Slip finishes

Non-slip finishes are easy to understand. The main effect of non-slip finishes is to increase
the adhesion between fibres and yarns regardless of fabric construction, the generic term for
these finishes would be fibre and yarn bonding finishes. Other terms that can be used include
anti-slip, non-shift and slip-proofing finishes. Adhesion between yarns is especially important
in woven fabrics at the seams and in highly stretched areas like the elbows of shirts, blouses
and jackets. Slippage of warp and fill yarns can also be a problem during preparation, dyeing,
printing and finishing.

7.2.1 Mechanisms of non-slip finishes

The primary mechanism for the effectiveness of non-slip finishes is increased adhesion
between fibres, filaments and yarns. This increased adhesion is accomplished by two
approaches. The first is the addition of inorganic solids to the surface of the fibres to increase
frictional forces. The second is to use film-forming polymers to hold the yarns physically in
place. Often commercial non-slip products contain both friction enhancers and film formers.

7.2.2 Chemistry of non-slip finishes

The most common friction enhancing agents are based on dispersions of silicic acid called
‘sols’. These products can be formed in a variety of particle sizes from 5 to 150 µm and yield
dispersions that range from clear to milky white. When the sols are deposited on the fibre
surface, the surface becomes much rougher and frictional forces between fibres become much
larger.

The polymeric film formers used as non-slip finishes are typically copolymers of vinyl,
acrylic and methacrylic monomers. These materials are similar in structure to the copolymers
used as hand builders.

7.2.3 Application methods and combinability

Non-slip finishes are mostly applied by the pad–dry process, combined as needed with hand
builders, repellents or cellulose crosslinkers (easy-care finish). The combination of silicic
acid sols with softeners or silicone-based water repellents is crucial – their effects are

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contrasting. Performance problems can occur when non-slip finishes are combined with
repellent finishes. Polymeric non-slip products, more than silicic acid sols, can reduce
repellency performance. One solution is to apply the non-slip finish, dry the fabric, then
apply the repellent finish. Enhanced performance of anti-pilling and handbuilding finishes
can be seen when these are combined with a non-slip finish. Back-coating is mostly achieved
by nip-padding or using a doctor (squeegee) or by foam application or spray techniques (for
a lower add-on). Another one-side application is rotary printing (screens with regular
perforation).

Exercise 7
Multiple Choice Questions
1. ________ are masses of tangled fibers that appear on fabric surfaces during wear or
laundering.
A. Size materials B. Pills C. Warp D. Cone
2. The higher the flex life, the _________ the pill remains on the fabric surface.
A. Longer B. Shorter C. Optimum D. None of the above
3. Which one of the following is not chemical finishing approach to prevent pills from
accumulating on fabric surfaces.
A. To prevent loose fibres from forming the initial ‘fuzz’ by applying polymeric coatings
that bind the fibres into the fabric surface.
B. To reduce pilling is to cause the pills to fall off the fabric as soon as they are formed.
C. To increase dimensional stability of the fabric
D. To reducing pilling tendency is applicable to 100 % cotton fabrics.
3. No- slip finish are mostly applied by ___________
A. The pad-dry process B. Nip Coating C. Back-coating D. Rotary Printing

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Paul, R. (Ed.). (2014). Functional finishes for textiles: improving comfort, performance and
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