ECO FRIENDLY PROCESSING OF WOOL
SRIKRISHNA NATARAJAN
DEPARTMENT OF TEXTILE TECHNOLOGY INDIAN INSTITUTE OF TECHNOLOGY DELHI
NOVEMBER 2017
© Indian Institute of Technology Delhi (IITD), New Delhi, 2017
ECO FRIENDLY PROCESSING OF WOOL
by
SRIKRISHNA NATARAJAN
Department of Textile Technology
Submitted
In fulfillment of the requirements for the award of the degree of Doctor of Philosophy to the
INDIAN INSTITUTE OF TECHNOLOGY DELHI
NOVEMBER 2017
i
CERTIFICATE
This is to certify that the thesis entitled “Eco friendly processing of wool” submitted by Mr. Srikrishna Natarajan to the Indian Institute of Technology Delhi for the award of the degree of Doctor of Philosophy, in the Department of Textile Technology, is a record of bonafide research work carried out by him. Mr. Srikrishna Natarajan has worked under my guidance and supervision and has fulfilled the requirements for the submission of this thesis.
The results contained in this thesis are original and have not been submitted in partial or full, to any other university or institute for the award of any degree or diploma.
Prof. Deepti Gupta
Department of Textile Technology
Indian Institute of Technology Delhi Hauz Khas, New Delhi – 110016.
iii
ACKNOWLEDGEMENTS
It is a moment of great pleasure and contentment for me to express my sense of gratitude to my supervisor, Prof. Deepti Gupta, Department of Textile Technology, IIT Delhi, for providing constant guidance, encouragement, careful attention and constructive criticism during the tenure of PhD. This journey would not have been possible without her support and motivation. She has not just encouraged and guided me but also shaped a better personality out of me. It was a joyful experience for me to work under her.
I thank the present Head of Department, Prof B.K. Behera, and the previous Heads Prof. R. Chattopadhyay and Prof. Kushal Sen for their support throughout this project.
I would like to thank members of my S.R.C- Prof. B.S. Butola, Prof. S Mukopadhyay &
Prof. A Rathore, who have contributed significantly to the progress of this research work.
I would like to extend sincere thanks to Prof. M.N.Gupta, Department of Chemistry and Prof. Aditya Mittal, KSBS, for their valuable guidance and permission to use their lab facilities.
I also thank Mrs. Chanchal Acharya for helping me with experiments on enzyme kinetics.
I thank Ms. Jyoti Sharma for her help and Ms. Manisha Yadav for formatting the thesis.
Sincere thanks are due to Mr. Virendra Sharma, Mr. Shiv Upadhyay, Mr. V.A. Passi, Mr. Jagdeesh and Mr. Suresh of TC lab for their support. I thank Mr. Sehgal (Stores), Mr. Rajkumar (Computer lab), Mr. Biswal and Mr. Vikas Khatkar (Testing lab), Mr.
Amarjeet (X-ray), Mr. Sharma, Mr. Kuldeep (SEM) and other members of various laboratories for providing support.
All my PhD fellow friends - especially Vikas K Singh, Anu Mishra, Krishnasamy Jagatheesan, Ramamoorthy, Gnanayudhayan, deserve to be acknowledged for their support and encouragement. This tedious and exhaustive journey would not have been possible without the moral support, affection and care of my mother, brother, sister in law and niece who always stood beside me through the thick and thins. Last but not the least, I find loss of words to express my deep sense of gratitude to my friend, philosopher and guide Dr. S. Periyasamy who constantly guided and encouraged me during this work.
(Srikrishna Natarajan)
v ABSTRACT
In this thesis, industrial waste products of natural origin were used to impart value adding properties to wool fabric.
Wool was coloured by in situ polymerization of catechol by potato juice using one and two bath method. In the two bath process, maximum colour depth was obtained with 4% catechol w/v, pH 4.5, 95°C. For the one step method, a statistical design of experiments was employed to determine the optimum parameters for obtaining a range of colours on wool. Mechanism of colour formation was attributed to formation of melanin by oxidative polymerization of catechol by potato juice. Structure of colourant showed the presence of ether linkages.
Strength, elongation, wetting and antioxidant property of wool was enhanced after colouration. Theoretical studies on kinetics of colour formation reaction showed catechol to be an excellent substrate for potato juice. Kinetic constants for the reaction VMax and KM were found to be 0.01814 + 0.002 Abs/min and 0.4148 mM respectively.
Melanin produced for colouration of wool in the first study, was successfully used as a simultaneous reductant cum capping agent for synthesis of silver nano particles from silver nitrate. Process parameters were optimized (0.1% catechol, 25% potato juice, pH 6.5, 950C,45 min) to obtain melanin having maximum reduction potential. Monodispersed, spherical silver nanoparticles, with average particle size of 45 ± 5 nm were obtained with 100% yield. The nanoparticles were applied to wool fabric by exhaust method. Treated fabric showed high antimicrobial activity against S.aureus and E.coli.
A robust and reproducible test method was developed for testing shrinkage of wool fabric in the laboratory, to simulate the results obtained by ISO 6330 test method. The proposed test method involves Relaxation shrinkage test (1 g/l detergent, pH 6, 40˚C, 60 minutes) followed by Felting shrinkage test (0.3g/l detergent, pH 6, 40˚C, 60min, 1:20) on samples of size 12x12cm. The process can be tuned to simulate various laundering conditions.
Wool was made shrink proof by an eco friendly process based on functionalization of wool by UV exposure, followed by coating of scales by sericin. Treated wool fabric showed smooth appearance and enhanced dyeability by acid and reactive dyes.
vii
इस सस , ऊन न न न
न न स न ऊन न न , 4% / , 4.5, 95 स स स स , ऊन न इ न न स इन इ स स नन ठन ठन ठ न स न न न ऊन , , स ठन न स स नन स स स स VMax इन 0.01814 + 0.002 स / न 0.4148
नन न न ऊन , स न इ स न न स स न नन न न न (0.1% , 25% स, 6.5, 950 स , 45 न ) न इ , न न , स 45 ± 5 न स 100% स न स ऊन न न स स फ
सओ 6330 न , ऊन स न न स स स न (1 / , 6, 40 ˚ स , 60 न ) , स (0.3 / , 6, 40 ˚ स , 60 न , 1:20) 12x12cm न न न न न न न स
ऊन अनावरण ऊन न स इस स सन ऊन अम्ऱ प्रतिक्रियाशीऱ न न इ
ix
CONTENT SUMMARY
Page No.
Certificate i
Acknowledgements iii
Abstract v
Content summary ix
Table of contents xi
List of figures xix
List of tables xxiii
List of symbols & abbreviations xxv
Chapter 1 Introduction 1
Objectives 3
Layout of the thesis 4
Chapter 2 Structure and properties of wool 7
Chapter 3 In situ colouration of wool 21
Chapter 4 Synthesis, characterization and application of silver nanoparticles
73
Chapter 5 Development of test method for assessing shrinkage of wool fabric
115
Chapter 6 Clean process for shrink proofing of wool 141
Chapter 7 Conclusions 169
References 173
List of publications 205
Brief Biodata of the author 209
xi
TABLE OF CONTENTS
Page No.
Chapter I Introduction 1
1.1 Introduction 3
1.2 Objective 4
1.3 Layout of the thesis 4
Chapter II Structure and properties of wool 2.1 Wool fibre
2.1.1 Morphological structure 2.1.2 Chemical composition 2.1.3 Physical properties 2.1.4 Chemical properties 2.2 Dyeing of wool
2.2.1 Dyeing with synthetic dyes 2.2.2 Dyeing with natural dyes 2.2.3 Dyeing with microbial dyes 2.2.4 Enzymatic colouration of wool
7 9 9 10 11 14 14 15 15 17 19 Chapter III In situ colouration of wool
3.1 Introduction
3.1.1 Oxidoreductase enzymes 3.1.1.1 Peroxidases
3.1.3.2 Polyphenol oxidases (PPO) 3.1.2 Studies conducted on enzymatic colouration 3.1.3 Composition of potato tuber
3.2 Materials and methods
3.2.1 Characterisation of potato juice 3.2.1.1 Protein assay
3.2.1.2 Enzyme assay and kinetic studies 3.2.1.3 Michaelis-Menten kinetics 3.2.1.4 Total phenolic content 3.2.2 Wool fabric
3.2.3 Colouration of wool
3.2.3.1 Two bath method Colouration After treatment
21 23 23 24 25 25 27 30 31 31 32 33 33 34 34 35 35 36
xii
3.2.3.2 One bath (simultaneous) method Experimental design plan
3.2.4 Assessment of colour properties 3.2.4.1 Colour value 3.2.4.2 Colour fastness 3.2.5 Characterisation studies
3.2.5.1 FT-IR spectra 3.2.5.2 XRD spectra
3.2.6 Performance properties of coloured fabric 3.2.6.1 Tensile strength
3.2.6.2 Antioxidant property 3.2.6.3 Fabric wetting 3.2.6.4 Vertical wicking 3.2.6.5 Antimicrobial effect
3.2.7 Comparison of potato varieties and storage stability of potato juice
3.2.8 Characterisation of colourant produced ex situ 3.2.8.1 Parameters affecting colour value 3.2.8.2 UV spectral analysis
3.3 Results and discussion
3.3.1 Characterisation of potato juice 3.3.2 Two bath colouration method
3.3.2.1 Concentration of catechol 3.3.2.2 Mechanism of colour formation 3.3.2.2 Time of treatment
3.3.2.3 Temperature of treatment 3.3.3 Effect of process parameters in bath2
3.3.3.1 pH of bath
3.3.3.2 Concentration of potato juice 3.3.3.3 Time of treatment
3.3.3.4 Temperature of treatment 3.3.4 One bath colouration method
3.3.4.1 Design of Experiments 3.3.4.2 Statistical analysis 3.3.4.3 Contour plots
36 36 37 37 38 38 38 38 38 38 39 39 39 40
40 40 41 41 41 41 42 42 43 44 44 44 45 46 47 47 48 48 49 52
xiii
3.3.5 Characterisation of coloured fabrics 3.3.5.1 Reflectance spectra 3.3.5.2 Colour fastness 3.3.5.3 FT-IR studies 3.3.5.4 XRD studies 3.3.5.5 Tensile strength 3.3.5.6 Antioxidant property 3.3.5.7 Moisture transport 3.3.5.8 Antimicrobial property
3.3.6 Spectroscopic characterisation of synthesized colourant 3.3.6.1 UV-Vis spectra
3.3.6.2 FT-IR spectra 3.3.7 Reaction kinetics
3.3.8 Process parameters influencing the depth of colour 3.3.9 Comparison of enzyme activity of different varieties of
potato
3.3.10 Storage stability of juice extracted from various varieties of potato
3.3.11 Conclusions
52 54 56 56 57 58 58 59 59 60 61 62 64 67
70
72
Chapter IV Synthesis, characterization and application of silver nanoparticles on wool
4.1 Introduction
4.1.1 Antimicrobial action of silver nanoparticles 4.1.2 Synthesis of silver nanoparticles
4.1.2.1 Top down synthesis 4.1.2.2 Bottom up synthesis
4.1.2.3 Chemical reduction method
4.1.2.4 Biological methods for synthesis of silver nanoparticles
Plant extracts Leaf extracts Bark extracts
Inflorescence/flower extract Fruit/peel extracts
Seeds
73
75 75 76 76 77 78 78
78 79 83 83 84 84
xiv Biopolymers Polysaccharides Silk protein Melanins 4.1.3 Silver nanoparticles on wool 4.2 Materials and methods
4.2.1 Synthesis of reductant
4.2.2 Synthesis of silver nano particles 4.2.3 Characterisation of reductant
4.2.3.1 Reducing power assay
4.2.3.2 Radical scavenging activity (RSA) assay
4.2.4 Characterization of silver nanoparticles 4.2.4.1 UV–visible spectroscopy 4.2.4.2 DLS
4.2.4.3 Electron microscopy 4.2.4.4 ICP-MS
4.2.5 Application of silver nanoparticles on wool
4.2.5.1 Determination of concentration of silver on fabric
4.2.6 Characterisation of wool fabric treated with silver nanoparticles
4.2.6.1 Colour 4.2.6.2 Morphology 4.2.6.3 Elemental Analysis 4.2.6.4 Antimicrobial activity
4.2.6.5 Durability of antimicrobial effect 4.3 Results and discussion
4.3.1 Parameters affecting the reducing ability of melanin 4.3.1.1 pH of treatment bath
4.3.1.2 Temperature
4.3.1.3 Concentration of catechol 4.3.1.4 Concentration of potato juice
4.3.2 Estimating the yield and concentration of silver nano particles
84 85 87 87 88 89 89 90 90 90 90
91 91 92 92 92 93 93
94
94 95 95 95 96 96 96 97 98 99 100 101
xv 4.3.3 Reducing power assay
4.3.4 Radical scavenging activity (RSA) assay 4.3.5 Characterisation of silver nanoparticles 4.3.6 Application of silver nanoparticles on wool
4.3.6.1 Effect of the Bath pH 4.3.6.2 Temperature
4.3.6.3 Time
4.3.7 Characterisation of wool fabric treated with silver nano particles
4.3.7.1 SEM analysis 4.3.7.2 EDX studies
4.3.8 Antimicrobial activity of wool treated with silver hydrosol
4.3.9 Durability of antimicrobial effect 4.3.10 Conclusions
102 103 105 106 106 107 107 108
109 109 111
112 113 Chapter V Development of test method for assessing shrinkage of
wool fabric 5.1 Introduction
5.1.1 Mechanism of shrinking of wool
5.1.2 Measuring the shrinkage of wool fabric during laundering
5.2 Materials and Methods 5.2.1 Wool Fabric
5.2.2 Characterisation of test samples 5.2.3 Chemicals
5.2.4 Preparation of Buffer Solution 5.2.5 Testing of shrinkage
Wascator method AATCC methods
Comparison of laboratory machines 5.2.6 Measurement of shrinkage
5.2.7 Study of process parameters in a Launderometer 5.2.8 Microscopic analysis
5.3 Results and discussion
5.3.1 Development of launderometer based test method
115
117 117 119
120 120 121 122 122 122 123 123 123 124 125 125 125 127
xvi
5.3.1.1 Concentration of detergent 5.3.1.2 Time
5.3.1.3 Temperature 5.3.1.4 pH
5.3.1.5 Materials to liquor ratio 5.3.2 Reproducibility of test method 5.3.3 Validation of the test method 5.3.4 Discussion
5.3.5 Conclusions
127 129 130 132 134 135 136 138 139 Chapter VI Clean process for shrink proof finishing of wool
6.1 Introduction
6.1.1 Subtractive method of shrink proofing 6.1.2 Additive method
6.1.3 Combined method
6.1.4 Ecofriendly shrink proofing processes 6.1.4.1 Enzymatic processing 6.1.4.2 Physical treatments
Plasma
UV/ozone treatment Synthetic polymers Natural polymers
Sericin
Properties of sericin 6.2 Materials and methods
6.2.1 Wool fabric
6.2.2 Extraction of sericin
6.2.3 Irradiation of wool with UV light
6.2.4 Treatment of irradiated wool with sericin 6.2.5 Testing for fabric for shrinkage
6.2.6 Characterisation and evaluation of treated fabric 6.2.6.1 SEM studies
6.2.6.2 TOF-SIMS studies 6.2.6.3 Fabric performance tests
Yellowness Index 6.2.7 Dyeability of shrink proof wool
141 143 143 143 144 144 144 145 145 146 146 147 147 147 148 148 149 149 149 150 150 150 150 151 151 151
xvii 6.2.7.1 Acid dye 6.2.7.2 Reactive dye
6.2.7.3 Determination of dye bath exhaustion 6.2.7.3 Dye fixation
6.2.7.4 Determination of color strength and colour fastness
6.3 Results and discussion
6.3.1 Effect of process parameters on shrink proofing of wool 6.3.1.1 Duration of UV exposure
6.3.1.2 Application of sericin bath pH of sericin bath
Concentration of sericin bath
6.3.1.3 Testing and evaluation of shrink proof wool
Fibre morphology Fibre Surface chemistry Fabric Characterisation Surface wetting
Weight add on, bending length and tensile strength
6.3.1.4 Dyeability of shrink proof wool
Dyeing with Acid dye Navimill Yellow 56N Exhaustion
Colour value Colour fastness
Dyeing with Reactive dye Drimalan Black FBRI
Exhaustion Fixation
Colour strength
Colour fastness of wool 6.3.2 Conclusions
151 151 152 152 152
152 153 153 154 154 156
158 158 160 161 162
162 163 163 163 164 164 165
165 165 166 166 167
Chapter VII Conclusions 169
xix
LIST OF FIGURES
Figure No. Figure Caption Page No.
2.1 Wool fibre structure 9
2.2 General formula of amino acid. 10
2.3 Chemical structure of natural dyes 16
3.1 Classification of Oxidoreductases 24
3.2 Polymerisation of phenols catalysed by Horse radish peroxidase (HRP)
24
3.3 Oxidation of monophenols and diphenols to o-quinones by PPO 25
3.4 Laccase catalyzed reaction of p-diphenol 25
3.5 Calibration curve of BSA 31
3.6 Calibration curve of Gallic acid 34
3.7 Standard method used in two bath colouration process 35
3.8 Effect of concentration of catechol 42
3.9 Schematic of in situ colouration of wool, (a) Enzymatic oxidation and b) Non enzymatic secondary reactions.
43
3.10 Effect of time of treatment with catechol 43
3.11 Effect of temperature of treatment of catechol on K/S 44
3.12 Effect of pH on colour value 45
3.13 Effect of concentration of potato juice 46
3.14 Colour value of samples treated with potato juice for varying duration of time
46
3.15 Effect of temperature of treatment of PJ on K/S 47 3.16 Contour plots obtained from RSM a) Temperature: 90°C, b)
Concentration of catechol: 5%, c) Concentration of potato juice:
25%, (d) Concentration of potato juice: 5%, (e) Concentration of catechol: 1%, (f) Temperature: 60˚C & (g) Temperature:
30˚C.
52
3.17 Reflectance spectra of coloured wool. 54
3.18 Synthesis of melanin pigment 55
3.19 FT-IR spectra of fabrics 56
xx
Figure No. Figure Caption Page No.
3.20 XRD spectra of fabrics 57
3.21 Tensile properties of test samples 58
3.22 Vertical wicking height of test samples 59
3.23 UV- vis spectra of the mixture of catechol and potato juice after varying duration of incubation
60
3.24 FT-IR spectra of Catechol and Colourant. 61
3.25 Reaction scheme showing the formation of Poly (catechol). 62 3.26 Michaelis –Menten plot for potato juice with varying
concentrations of catechol showing the KM and VMax values
63
3.27 Double reciprocal Lineweaver -Burk plot 64
3.28 Effect of pH on depth of colour 65
3.29 Effect of temperature on depth of colour 65
3.30 Effect of time of treatment on depth of colour 66 3.31 Effect of concentration of catechol on depth of colour 66 3.32 Effect of concentration of potato juice on depth of colour 67 3.33 Enzyme activity determined for different varieties of potato 68 3.34 Colour value obtained with different varieties of potato 69 3.35 Correlation between enzyme activity and K/S value 69 3.36 Effect of storage time of potato varieties on enzyme activity 71 3.37 Effect of length of storage time of PJ on K/S 71 4.1 Morphological change and cell wall damage of bacterial cell 76 4.2 Possible chemical constituents of plant extract responsible for
the bio reduction of metal ions
79
4.3 Calibration curve of silver nitrate 93
4.4 Calibration curve of silver nanoparticles 94
4.5 Silver nitrate solutions reduced with melanin synthesized at different pH
97
4.6 Spectra of AgNO3 solutions reduced with melanin synthesized at varying pH (0.1% C, 25% PJ, 95˚C)
98
xxi
Figure No. Figure Caption Page No.
4.7 Effect of temperature of melanin synthesis (˚C) (0.1% C, 25%
PJ, pH 6.5)
99
4.8 Effect of catechol concentration used in melanin synthesis on absorbance of silver nanosol (25% PJ, pH 6.5, 95˚C).
100
4.9 Effect of potato juice concentration on spectra (0.1% Catechol, pH 6.5, 95˚C)
101
4.10 Schematic showing synthesis of silver nanoparticles by melanin 101 4.11 Absorbance (700nm) of ferric chloride solution reduced with
ascorbic acid and melanin
103
4.12 Inhibition (%) of DPPH free radicals by melanin and ascorbic acid
104
4.13 TEM images of silver nanoparticles recorded at different magnifications, the scale bar corresponds to (a) 50 nm (b) 100 nm & (c) 200 nm
105
4.14 Size distribution of silver nanoparticles prepared using melanin 106 4.15 K/S of wool fabrics treated with silver hydrosol at various pH
(60˚C, 30 min)
107
4.16 K/S of wool treated with silver hydrosol at different temperature (pH )
107
4.17 Effect of time of exhaustion on K/S values of wool treated with silver hydrosol
108
4.18 Wool fabrics treated with different concentration of silver nanoparticles
108
4.19 SEM images of untreated wool a) treated with silver nanoparticles b) 150 ppm c) 200 ppm
109
4.20 EDX spectra of (a) untreated wool; wool treated with b) 150 ppm (c) 200 ppm silver nanoparticles
111
4.21 Antimicrobial testing of nano silver treated wool against S.
aureus a) Control b) 150 ppm c) 200ppm and E.coli (d) Untreated, (e) 150ppm (f) 200ppm
112
4.22 Durability of antimicrobial activity to washing (a) Control S.aureus (b) after 10th wash (c) after 20th wash (d) Control E.coli (e) after 10th wash (f) after 20th wash
113
5.1 Differential frictional effect (a) between fibres lying in same direction, (b) between fibres against the scales, (c) between fibres with scales, (d) on plane surface against scales (e) on plane surface with scales.
118
xxii
Figure No. Figure Caption Page No.
5.2 Picture of a Wascator 120
5.3 Microscopic images of test fabrics used for validation study 121
5.4 Cutting and marking of test sample 124
5.5 Area shrinkage of wool observed in various test methods 127 5.6 Effect of detergent concentration on area shrinkage 128 5.7 Effect of time of treatment on area shrinkage 130 5.8 Effect of temperature of treatment on area shrinkage 132
5.9 Effect of bath pH on area shrinkage 132
5.10 Effect of material to liquor ratio on area shrinkage 135
5.11 Test of reproducibility of the test method 135
5.12 Validation of the test method 138
6.1 Microstructure of raw silk fibre as by image SEM 148 6.2 Effect of duration of UV exposure on shrinkage, tensile strength
and yellowness index of wool
154
6.3 Effect of pH of sericin liquor on shrinkage of wool 155 6.4 Effect of concentration of sericin and duration of UV exposure
on shrinkage.
156
6.5 Optical micrographs of wool a) Untreated b) Untreated after shrinkage test c) Irradiated for 5 min (5UV). d) Irradiated for 5 min + 1 g/l sericin e) Irradiated for 5 min + 2.5 g/1 sericin
157
6.6 SEM images of wool a) Untreated wool b) UV irradiated for 5min c) UV irradiated for 5 min+5gpl sericin
159
6.7 Structure of 18-methyl eicosanoic acid 160
6.8 The structure of F-Layer (18-MEA) present on the cuticle layers 160 6.9 TOF – SIMS spectra of wool (a) Untreated (b) UV irradiated
for 5 min
161
6.10 Microscopic images showing wetting of wool a) Untreated b) b) UV irradiated for 5 min+5gpl sericin
162
xxiii
LIST OF TABLES
Table No. Table Caption Page No.
2.1 Elemental composition of dry wool 11
2.2 Amino acids present in wool 13
3.1 Studies conducted on enzymatic colouration of textiles 29
3.2 Typical composition of potato tubers 30
3.3 Reagents used for enzyme assay and kinetic studies. 32 3.4 Process variables studied in two bath (sequential) method 35
3.5 Levels used in Box and Behnken design 37
3.6 Experiment conditions obtained by Box and Behnken surface response Design
37
3.7 Variables used in the study 41
3.8 Colour characteristics of test samples treated as per DOE 49 3.9 Recipe options for obtaining a specific K/S value on wool 50
3.10 Range of shades obtained on wool 53
3.11 Colour fastness of test samples 54
3.12 Antioxidant activity and wetting time of selected samples 55 3.13 Comparison of enzyme activity in various varieties of potato (t-
test)
68
3.14 Statistical significance of K/S values on enzyme activity of potato varieties by t-test
70
4.1 Biosynthesis of silver nanoparticles using plant extracts 80 4.2 Synthesis of silver nanoparticles using biopolymers 85 4.3 Process parameters varied for synthesis of melanin 89 4.4 Variables studied in exhaustion of silver nanoparticles on wool
fabric
93
4.5 Effect of reductant (melanin) concentration on yield of silver nanopartcles
102
4.6 Absorbance (517 nm) of melanin and ascorbic acid 104 4.7 Antimicrobial activity of wool treated with silver nanoparticles 111
xxiv
Table No. Table Caption Page No.
4.8 Durability to washing of the treated wool fabrics 112
5.1 Specifications of fabrics used in the study 121
5.2 Testing conditions 123
5.3 Process variables used for development of launderometer based test method
125
5.4 Shrinkage of wool observed in various methods 126 5.5 Shrinkage of wool observed at various concentrations of
detergent
128
5.6 Shrinkage of wool observed at different time of treatment 129 5.7 Shrinkage of wool observed at different temperature of
treatment
131
5.8 Shrinkage of wool observed at different pH 133
5.9 Shrinkage of wool observed at various materials to liquor ratio 134
5.10 Test of reproducibility of the test method 136
5.11 Validation of test method 137
6.1 Properties of samples treated with variable concentration of sericin
162
6.2 Exhaustion (%) of acid dyes 163
6.3 Colour strength of acid dyed wool 164
6.4 Colour fastness of the acid dyed wool 165
6.5 Exhaustion of Drimalan Black FBRI on wool fabric 165 6.6 Fixation of Drimalan Black FBRI on wool fabric 166 6.7 Effect of concentration of sericin on colour strength of reactive
dyed wool
166
6.8 Colour fastness of wool 167
xxv
LIST OF SYMBOLS & ABBREVIATIONS
S.No Symbol/Abbreviation Full form
1 AOX Absorbable organic halogen
2 18-MEA 18-methyl eicosanoic acid
3 CMC Cell membrane complex
4 DFE Directional frictional effect
5 L-DOPA L-3, 4 dihydroxy phenyl alanine
6 HRP Horse radish peroxidases
7 PPO Polyphenol oxidases
8 DABSA 2,5, diamino benzene sulfonic acid
9 ABTS 2, 2 azino-bis-(3-ethylthiazoline-6 sulfonate
10 HBT 1- hydroxybenzotriazole
11 DMP 2, 6- Dimethoxyphenol
12 EDC 3-(3-dimethyl aminopropyl) carbodiiamide hydrochloride
13 BSA Bovine serum Albumin
14 BR Bradford reagent
15 EDTA Ethylene di amine tetra acetic acid
16 E Enzyme
17 ES Enzyme substrate complex
18 V0 Change in initial rate or velocity
19 [S] Substrate
20 VMax Velocity maximum at the maximum substrate concentration
21 KM Michaelis constant
22 FC reagent Folin-Ciocalteau (FC) reagent
23 GAE Gallic acid equivalent
24 RFD Ready for dyeing
xxvi S.No Symbol/Abbreviation Full form
25 HT-HP High temperature high pressure
26 % v/v % Volume/Volume
27 l Microliter
28 µg/ml Microgram/milliliter
29 % w/vol % Weight/Volume
30 mg/l Milligram/litre
31 g/mole Gram/mole
32 g/l Gram per litre
33 eV Electron volt
34 KV Kilo volt
35 Min Minutes
36 DOE Design of experiments
37 RSM Response surface methodology
38 PJ Potato juice
39 DPPH 2.2- diphenyl-1-picryl-hydrazil
40 D.I water Deionized water
41 ISO International organization for standardization 42 AATCC American Association of Textile Chemists and
Colorists
43 ASTM American Society for Testing and Materials
44 TLC Thin layer chromatography
45 NMR Nuclear magnetic resonance
46 IR Infrared
47 CFU Colony forming units
48 K/S Colour value
49 L* Lightness or darkness
50 a* Redness or greenness
xxvii S.No Symbol/Abbreviation Full form
51 b* Blueness or yellowness
52 ANOVA Analysis of variance
53 XRD X-ray diffraction
54 FT-IR Fourier transform infrared spectroscopy 55 S. aureus Staphylococcus aureus
56 E.coli Escherichia coli
57 B.mori Bombyx mori
58 RSA Radical scavenging activity
59 UV-Vis Ultraviolet/visible
60 DLS Dynamic light scattering
61 TEM Transmission electron microscopy
62 ICP-MS Inductively coupled plasma mass spectrometry
63 µm Micrometer
64 Nm Nanometer
65 Gf Gram force
66 gm/m2 Gram per metre square
67 kDa Kilo Dalton
68 DNA Deoxyribonucleic acid
69 ATP Adenosine triphosphate
70 DMF N-N-dimethyl formamide
71 PVP Polyvinyl pyrrolidone
72 PMVE Poly methyl vinyl ether
73 SDS Sodium dodecyl sulphate
74 CTAB Cetyl trimethyl ammonium bromide
75 SNSE Sulfur nano-silver ethanol
76 SPR Surface plasmon resonance
77 PCS Photon correlation spectroscopy
xxviii S.No Symbol/Abbreviation Full form
78 QELS Quasi elastic light scattering
79 SEM Scanning electron microscopy
80 EDX Energy-dispersive X-ray spectroscopy
81 TOF-SIMS Time of flight secondary ion mass spectroscopy
82 LMIG Liquid metal ion gun
83 UHV Ultra high vacuum
84 YI Yellowness Index
85 M Mole
86 mM Milli mole
87 ppm Parts per million
88 Ag Silver
89 TPI Twist per inch
90 Epc Ends per cm
91 PPc Picks per cm
92 T.B Tris hydroxymethyl aminomethane buffer
93 MCT/VS Monochlorotriazine/Vinyl sulphone
94 S.D Standard deviation
95 MLR Material to liquor ratio
96 S.E Standard error
97 C.V Coefficient of variation
98 TGases Transglutaminases
99 DMDHEU Dimethyl dihydroxy ethylene urea
100 Rpm Revolutions per minute
101 7A Relaxation cycle
102 5A Felting cycle
103 RH Relative humidity
