Seminar entitled" Surface modification of woollen textiles" presented in Department of Textiles and Apparel designing, College of Community Science, UASD by Manpreet Kaur and Dr. Geeta Mahale

1. BIO-FINISHING OF WOOLLEN
TEXTILES
PRESENTED BY:
Manpreet Kaur and Dr. Geeta Mahale
1

2. 2
Bio-finishing
Using enzymes
Using biopolymers Using plant
extracts
Enzymes is specialized high
molecular weight protein
produced within an organism,
which is capable of catalyzing
specific chemical reactions.
Sources: Vegetable source
• Bacterial source
• Animal source
Ex: Amylase. Pectinase,
Lacasse, Cellulase, protease
etc.
• Synthesized by living
organism
• Suitable and renewable
materials
• Suitable alternative to
chemical based finishing
agents
• Derived from different
source
(Agricultural feed stock and
marine food resources)
Ex. Chitosan, Starch,
Polysaccarides,(cyclodextrins),
Sericin, alginate etc.
Ex. Pomegranate peel
Walnut husk
Aloe vera
Neem
Banana sap
Flowers
Fruits etc.
Biological way of giving
wet treatments to textiles

3. 3
Wool
• Renewable natural source
• Low energy requirement for production
3
Functional
finishes on
wool
Shrink resistance
Insect resistance
Flame resistance
Antibacterial
Dyeing

4. Surface modification
It is an act of modifying the surface of a material by physical, chemical
or biological characteristics different from the ones originally found on
the surface of a material.
Purpose of surface modification
10-11-2022 4
• Increasing the bioactivities
• Improve adhesion property
• Improve biocompatibility
• Create permanent wettability, Improve the hydrophobicity, dyability
• Soft feel

5. 5
Enzyme mechanism

6. 6
Application of chitosan in wool processing

7. 7
Research studies
Enzymatic
finishing
Biopolymer
treatment
Herbal
extracts

8. Quality improvement of Wool Fabric using Protease Enzyme
To find out the effect of protease enzyme on the physical and
colourfastness properties of the woollen fabric
1
Pooja et al. (2014)
8

9. Methodology
10-11-2022 9
Raw
Materials
Pretreatment
of woolen
fabrics
Enzyme
Treatment
Scouring
• Liquid soap (Ezee)
: 0.5 % (o.w.f)
• M:L : 1:50
• Temperature:40ºC
• Time duration : 30
min
• Alkaline protease : 1,
2, 3, 4 and 5 %(o.w.f)
• M:L : 1:20
• Temperature : 40ºC
• Time : 60 minutes
• pH : 8.5
• Coarse woollen
(woven) fabric
• Alkaline
Protease
Enzyme
Testing
For
Physical
Properties
• Absorbency
• Fabric tensile test
• Weight loss
• Pilling resistance
• Fabric drape
• Hand of fabric
• SEM

10. 10
S.No TEST TEST STANDARD
1 Absorbency AATCC:79-2010
2 Fabric tensile test IS:1969(Part 2):2010/ISO 13934-2:1999
3 Weight loss ASTM d 2720-94 (2012)
4 Pilling resistance IS:10971(Part 1):2011/ISO/2945-2:2000
5 Fabric drape ASTM D-737-04 (2012)
6 Hand of fabric AATCC: EP 5
Table 1 Testing For physical properties

11. 11
SI
No.
Types of
treatment
Conc. of
Protease
enzyme
Hand of fabric Weight
loss
(%)
Absorbency
(time taken in
seconds)
Fabric tensile
strength
Fabric
drape
Pilling(ra
ting)
Softness Smoothness Warp Weft
1 Control - 2 2 - 60 42 40 0.85 5(no
pilling)
2 Scoured - 2 3 0.52 45 40 36 0.75 5
3
Protease
treated
1 3 3 1.47 42 34 35 0.67 5
2 3 4 2.73 38 32 37 0.65 4-5
3 4 4 4.10 35 33 36 0.64 4
4 5 5 5.36 33 32 32 0.48 4
5 5 4 6.31 31 31 32 0.61 3
Table 2. Effect of various concentrations of Proteases enzyme treatment on physical properties of
woollen fabric

12. • Improved physical properties including hand,
drapability, absorbency
• Tensile strength decreased slightly
• 4 g/l enzyme concentration showed best results
12
CONCLUSION

13. Effects of cutinase on the enzymatic shrink-resist finishing of wool fabrics
To investigate the application of cutinase in the wool bio anti-
felting finishing to improve the wettability and shrink-
resistance of wool fabrics
1
Wang et al. 2015
13

14. MATERIALS AND METHODS
Fabric Worsted wool fabric
Enzyme Cutinase, protease
Treatment methods
Pretreatments of wool fabrics
with cutinase or hydrogen peroxide
Protease treatment of wool fabrics
Cutinase
solution
10 U/g
fabric
MLR 25:1
Temp. 600C
Time 4h
pH 8
H2O2 20 g/L
pH 9
Temp. 500C
Time 1h
Protease 250 U/g
pH 8.5
MLR 25:1
Temp 550C
Time 1h
14
Cutinase: plant
pathogenic fungi
Rinsing and drying

15. Testing procedure
Wettability (AATCC Test Method 39-1980)
Weight loss WL(%) = 100 × A − B/A
A= Wt. of untreated wool fabric, B=
pretreated wool fabric
Tensile strength Tensile strength tester(ISO 5081)
Felting shrinkage IWS Test Method 31
FT-IR ATR FT-IR spectrophotometer
Scanning electron microscopy
(SEM)
FEI Quanta- 200 Scanning electron
microscope
15

16. Samples Wetting (time/min) Contact angle (◦)
a b a b
Control (pretreated without
cutinase)
>30 18.5 134.83 123.15
Pretreated with cutinase 7.9 1.3 92.04 66.82
Pretreated with H2O2
21.2 11.5 127.33 98.14
16
a: no protease treatment b: protease-treated
Table 1 Wettability of wool fabrics treated with cutinase and protease
RESULTS AND DISCUSSION

17. Fig.1 Weight loss of wool fabrics after protease treatments (a) Control
(b) pretreated with cutinase (c) pretreated with hydrogen peroxide
17
6.3
6.9
3%

18. Fig. 2 Tensile strength of wool fabrics before and after protease treatments
(a)Control (b) pretreated with cutinase (c) pretreated with hydrogen peroxide
18

19. Fig. 4 FT-IR ATR spectra of wool fiber keratin over range 1000–1400 cm−1
(a) Control (b) pretreated with cutinase (c) pretreated with hydrogen peroxide
19

20. Fig. 5 Percentages of area shrinkage of wool fabrics before and after
protease treatment (a) Control (b) pretreated with cutinase (c) pretreated
with hydrogen peroxide
20

21. Fig. 6 SEM images of protease-treated wool fabrics
(a) Control (b) pretreated with cutinase (c) pretreated with hydrogen peroxide
21

22. CONCLUSION
• Weight loss of the sample treated with cutinase was similar to
that of the fabric treated with hydrogen peroxide
• The combination of cutinase and protease treatment improved
the shrink resistance of the wool fabrics mainly due to the
enhancement of the wettability
22

23. Surface functionalization of wool via microbial-trans glutaminase
and bentonite as bio-nano-mordant to achieve multi objective
wool and improve dye ability with madder
To improve the dye ability of wool by using bio-nano-mordant
Pour et al. (2020)
2
23

24. • Scoured and un-dyed
wool fabric(195g/m2)
• Bentonite nanoclay
• Transglutaminase
(TG)
• Maddar roots powder
Concentrations: 5%,
10%, 20%
MLR: 1:40
Temperature:370C
pH: 9-10
Materials: Extraction process of dye Enzymatic treatment
A temperature of dye solution
was raised up to the boiling
point and retained in boiling
for 60 min
Cooling for 24h
Filtertaion
MATERIALS AND METHODS
A powder was prepared
and dissolved in distilled
water to form a solution
24

25. Fig. 8 Schematic illustration of the wool treatment and dyeing process
25
25
50:1

26. 26
Fig. 9 Schematic representation of proposed mechanism for treated wool by
enzyme and bentonite

27. Fig. 10 Images of untreated wool (a) and treated wool with m-TGase (b)
bentonite (c), and m-TGase-bentonite(d)
RESULTS AND DISCUSSION
27

28. Fig 12 FTIR spectrums of untreated and treated wool with enzyme,
bentonite and enzyme-bentonite
28

29. Compounds Percentage
(%)
L* a* b* C* h*
Untreated 50 56.56 19.10 17.18 25.69 41.97
Enzyme 5% Clay 3 39.66 27.95 26.13 38.26 43.07
Clay 5 40.58 30.64 28.65 41.94 43.08
Clay 10 42.34 29.16 26.43 39.36 42.20
Enzyme 10% Clay 3 40.66 29.92 26.60 40.04 41.63
Clay 5 40.73 29.50 26.80 39.85 42.26
Clay 10 41.66 27.38 23.84 36.30 41.05
Enzyme 20% Clay 3 41.87 27.51 22.82 35.75 39.67
Clay 5 42.09 29.90 23.45 38.00 38.10
Clay 10 43.94 28.96 22.18 36.48 37.44
Table 2 CIE L* a* b* C* h* values of wool dyed with Madder using, m-TGase
and Clay
30

30. Fig. 15 K/S values of wool dyed with
Madder using, m-TGase and Clay
Fig. 16 ΔE values of wool dyed with Madder
using, m-TGase and Clay
31

31. Fig. 18 Colour of dyed wool: (a) untreated wool; treated wool with: (b) 5% m-TGase and
3% Clay, (c) 5% m-TGase and 5% Clay, (d) 5% m-TGase and10% Clay, (e) 10% m-TGase and
3% Clay, (f) 10% m-TGase and 5% Clay, (g) 10% m-TGase and 10% Clay, (h) 20% m-TGase
and3% Clay, (i) 20% m-TGase and 5% Clay, and (j) 20% m-TGase and 10% Clay 32

32. CONCLUSION
• Treatment of wool with 5% owf of m-TGase and 5% owf of
bentonite promoted dyeability and absorbed more madder dye
• Highest K/S value
33

33. 34
BIO-POLYMER TREATEMENT

34. Multifunctional finishing of wool fabrics by chitosan UV-grafting: An approach
To improve dyeability and thermal properties of wool fabrics by
using chitosan
Periolatto et. al (2013)
3
35

35. 36
Materials: Knitted wool fabric(mass/unit 292g/m2)
Low viscosity chitosan: 75-85% deacetylation degree
• Oxidative treatment by H2O2
• Telon turquoise blue M5-G 85% Acid blue(low affinity towards wool)
Dilution of chitosan by acetic acid and
spread on the fabric
Impregnation conditions: 1min, 1h
or 24 h at 250C or 500C
Drying, Curing
Medium pressure mercury lamp
under nitrogen atmosphere
Fabric finishing
Polymer add-on(%)=w-w0/w0×100
W= weight of grafting fabric
w0=Weight of original fabric
Dyeing parameters:
• 1% dye (owf)
• MLR: 1:50,pH:4, 850C

36. 37
Characterization of treated samples
• Antimicrobial activity: ASTM E2149-01 method using E.coli and s. aureous
• Dye exhaustion: Spechtrophotometer
• Wash durability : UNI-EN ISO 105 C01 using either ECE detergent standard or
Tween 20 (5 washing cycles)
• Antifelting: Woolmark Test TM31
• Thermal resistance (Rct), expressed in m2◦C/W, and water vapor resistance (Ret),
expressed in m2 Pa/W, of fabrics : (ISO 11092 standard) by Sweating Guarded
Hotplate (SGHP)
• Water vapour permeability(imt)=S× R ct/ (Ret where S= 60Pa/0C, imt=0-5
• Surface morphology: SEM(Scanning electron microscope)

37. Impregnation
time and
temperature
Chitosan
add-on (%)
Without oxidative
pretreatment
With oxidative
pretreatment
E. coli
(%)
S. aureus
(%)
E. coli
(%)
S. aureus
(%)
1 min, 25◦C 2 21 - 62 -
24 h, 25◦C 2 25 - 56 -
1 h, 50◦C 2 30 - 67 50
1 h, 50◦C 4 87 44 - -
1 h, 50◦C 8 88 - - -
1 h, 50◦C 12 77 - - -
Table 5 Microorganism reduction of chitosan treated wool fabrics: influence of
impregnation, chitosan add-on and oxidative pretreatment
38

38. Fig. 19 Dyeing tests with Telon Turquoise on wool: (a) untreated; (b) with 2% chitosan add-
on without oxidative pretreatment; (c) after oxidative pretreatment alone; (d)
with 2% chitosan add-on after oxidative pretreatment
39

39. Fig. 20 Color strength of wool samples dyed with Telon Turquoise: untreated (NT)
after oxidative pretreatment alone (OX), with 2% chitosan add-on without oxidative
pretreatment (CH), with 2% chitosan add-on after oxidative pretreatment (OX + CH)
40

40. Untreated 2% Chitosan not
pre-oxidized
Pre-oxidized only Pre-oxidized +
2% chitosan
Value St. dev. Value St.
dev.
Value St. dev. Value St. dev.
L 62.69 1.47 57.86 1.68 63.07 1.54 53.14 1.21
C 29.46 1.78 32.65 2.13 29.25 1.00 36.64 0.55
H 205.15 1.01 208.99 0.64 190.48 2.35 208.44 0.53
Table 6 Color measurements on wool dyed with Telon Turquoise
41

41. Fig. 21 SEM images of chitosan treated wool, 2% add-on: (a) unwashed and (b)
washed with ECE detergent (magnification ratio 400×)
42

42. Sample Sample Relaxation
dimensional
change (%)
Total
shrinkage (%)
Cross direction Untreated 0 -1.0
Treated -1.5 -2.9
Longitudinal
direction
Untreated -13.5 -16.9
Treated -1.2 -3.0
Sample Rct (m2◦C/W) Ret (m2 Pa/W) imt
Untreated 0.0304 ± 0.0011 3.51 ± 0.08 0.52
Treated 0.0477 ± 0.0051 5.13 ± 0.26 0.56
Table 7 Relaxation dimensional change and total shrinkage on untreated and 2% chitosan
treated wool fabrics
Table 8 Comfort properties, evaluated by Skin Model, on untreated and 2% chitosan
treated wool fabrics
43
• According to Skin model of Hohenstein Institute, 5 breathability levels were
established for textiles: if Ret<6(extreme breathability)
• 6<Ret<13(good breathability)
• 14<Ret<20(normal breathability)
• 21<30<30(low breathability)
• Ret>30(negligible breathabilty)

43. CONCLUSION
• Eco-friendly method to confer a multifunctional finishing to wool
fabrics
• Good antimicrobial activity (67% reduction of E. coli and 50%
of S. aureus)
• Maximum reduction of felting after washing
44

44. Wheat starch, gum arabic and chitosan biopolymer treatment
of wool fabric for improved shrink resistance finishing
To impart shrink resistance finish to wool fabric
Rani et al.(2020)
4
45

45. Materials: Woven wool fabric (146g/m2)
Dye Source: Madder root powder
Scouring: 1% Sodium carbonate and 2% wetting agent (Ultravon JU)
Bioploymer treatment: Gum arabic, chitosan, wheat starch, glacial acetic
acid, citric acid, sodium dihydrogen orthophosphate(catalyst)
MATERIALS AND METHODS
Citric acid: cross linking agent
Sodium dihydrogen orthophosphate: Catalyst(6%on the weight
of biopolymer solution)
10min
Schematic illustration of the biopolymer treatment on wool fabric 46

46. Characterization
• FTIR: (FTIR Spectrophotometer)
• SEM: (field emission scanning electron microscopy) FE-SEM
• Moisture content (ASTM D1576–13)
• Tensile and friction properties: ASTM D5035 and ASTMD 3108
• Bending length: Stiffness tester (ASTMD1388)
• Flexural rigidity: w х c3х 9.80 х 10-3 W= fabric weight, c= bending length
• Bending modulus: 12 G / t3 T= fabric thickness, G= bending modulus
• Colour strength: Colour spectrophotometer
• Shrinkage measurement: (launderometer) ISO 6330
47

47. Possible reaction mechanism of interaction between wool and biopolymers 48

48. Fig. 22FE-SEM images at ×5000
magnification of (a) untreated wool (b)
gum Arabic (c) chitosan and (d) wheat
starch biopolymer treated wool fiber
samples
Fig. 23 FE-SEM images at ×10,000
magnification of (a) untreated wool (b)
gum Arabic (c) chitosan and (d) wheat
starch biopolymer treated wool fiber
samples
RESULTS AND DISCUSSION
49

49. Fig. 25 FTIR spectra of (a) gum arabic (b) chitosan and (c) wheat starch biopolymers
50
-OH -COO
-COO
-C-O-C
C=O,-NH, -CH3, -CH2, -C-O-C
-OH, C-O-H, C-O, C-C, -CH2

50. Fig. 26 FTIR spectra of (a) untreated and wool fabric coated with (b) gum Arabic, (C)
chitosan and (d) wheat starch biopolymers 51
-OH
-OH
-NH

51. Fabric name Basis weight
(g/m2)
Thickness
(mm)
Moisture
Content (%)
Moisture
Regain (%)
Untreated 163 0.63 13.36 15.42
Gum Arabic 179⁎ 0.73⁎ 13.48 15.58
Chitosan 164 0.67⁎ 13.27 15.31
Wheat
starch
174⁎ 0.69⁎ 13.55 15.67
Fabric
name
Tensile stress
(MPa)
Strain (%) Tensile modulus
(MPa)
Coefficient of friction
Dynamic Static
Untreated 11.79 23.36 135.37 0.762 0.763
Gum Arabic 11.04 22.42 142.41 0.799⁎ 0.803⁎
Chitosan 13.03⁎ 23.58 161.73⁎ 0.800⁎ 0.802⁎
Wheat
starch
11.86 23.36 136.72 0.790⁎ 0.791⁎
Table 9 Effect of biopolymer treatment on structural and moisture properties of wool fabric
Table 10 Effect of biopolymer treatment on tensile and frictional properties of wool
fabric
52

52. Fabric
name
Bending length
(mm)
Flexural rigidity
(mN.mm)
Bending modulus
(kN/m2)
Untreated 20.8 14.42 692.41
Gum Arabic 20.9 14.65 703.26
Chitosan 23.5⁎ 20.78⁎ 997.40⁎
Wheat
starch
20.3 13.41 997.40⁎
Fabric
name
Yellowness Whiteness Dyeing performance
L* a* b* dE K/S
Untreated 17.16 54.01 32.60 22.40 24.02 0.00 24.39
Gum Arabic 20.86 47.97 30.23 22.29 23.38 1.91 26.48
Chitosan 21.54 46.25 31.27 23.52 24.80 2.46 26.04
Wheat
starch
18.02 52.00 31.37 22.28 23.55 1.32 25.33
Table 12 Yellowness and whiteness measurement of untreated and biopolymer treated
fabrics before dyeing and color coordinates after dyeing under similar conditions
Table 11 Effect of biopolymers treatment on bending properties of wool fabric
53

53. Fig. 28 Area shrinkage for application of biopolymer treatment
55

54. CONCLUSION
• Sustainable treatment
• No significant change in tensile and bending properties of fabric
in case of gum arabic and wheat starch coating
• Color strength improved
• Among all the biopolymers, wheat starch at 0.5% concentration
was found most effective for least shrinkage
56

55. Adsorption and Flame Retardant Properties of
Bio-BasedPhytic Acidon Wool Fabric
To know the effect of phytic acid on adsorption and flame
retardence properties on wool fabric
Cheng et al.(2016)
5
57

56. MATERIALS AND METHODS
Materials:
• Scoured woven wool fabric
• Phytic acid(70%) aqueous solution
• Sodium hydroxide
Phytic acid: biobased phosphorous containing
compound
• “Green molecule” found in plant tissues
such as beans, cereal grains and oil seeds
• consists of six negatively charged phosphate
groups
58

57. Experiments of the adsorption of PA (phytic acid)
2. Effect of Temp. on the
adsorption of PA
pH was adjusted to
1.2,2.1,3.0,4.1 by addition
of 1M NaOH
Wool fabric immersed in
solution of 120% owf at
300c
Temperature was raised to
900c at a rate of 20C/min
1. Effect of pH on the
adsorption of PA
Wool fabric immersed in
solution of 120% owf at
300c
Temperature was raised to
50-980c at a rate of 20C/min,
Time=60min(holding time)
3. Equilibrium adsorption
of PA
Concentarions: (10- 200%owf)
at 900C, pH=1.2
4. Building up property
Concentarions: (10
200%owf) at 300C, pH=1.2
Temperature was raised to
900c at a rate of 20C/min for
60 min 59
pH: 1.2
900C

58. Adsorptions of PA Shimadzu UV-1800 UV-Vis spectrophotometer
Exhaustion (%)=100 (m0 -m1)/m0
m0 = Quantities of PA before treatment
m1= Quantities of PA after treatment
Weight gain Weight gain (%)= 100 х (W2-W1)/W1
W1: Weight before treatment
W2:Weight after treatment
LOI test GB/T 5454-1997 (equivalent to ASTM Standard Method D2863)
with the FTT0080 oxygen index apparatus
Vertical burning test GB/T 5455-2014 (equivalent to ASTM Standard Method D6413)
with the YG 815B automatic vertical flammability cabinet
Measurements
Vertical burning test
LOI test
60

59. PCFC test FTT0001 microscale combustion calorimetry (Fire Testing
Technology Ltd., East Grinstead, UK) according to ASTM
Standard Method D7309
TG Analysis Diamond TG/DTA SII thermal analyzer
FT-IR Spectra Nicolet5700 FT-IR spectrometer
SEM Observation TM3030 tabletop scanning electron microscope
ICP-OES ICAP 6300 DUO (Thermo Fisher Scientific Inc., Waltham,
MA, USA) with argon plasma at the wavelength of 178.284
nm
Whiteness Index WSB-2 digital whiteness meter
Mechanical
Performance
Tensile strength: ISO 13934-1-2013 with the Instron 3365
tester
Durability to Washing WashTec–P fastness tester
Pyrolysis combustion
flow calorimetry
ICP-OES
(Inductively coupled plasma
- optical emission
spectrometry) 61

60. RESULTS AND DISCUSSION
62

61. Fig. 29Effect of pH on the uptake of PA by
wool
Fig. 30 Effect of temperature on the
uptake of PA by wool
63

62. Fig. 31 Influence of initial PA
concentration on its uptake by wool
Fig. 32 Weight gain and LOI of the
wool fabrics treated with PA
64

63. Fig. 33 Char length (a) and photographs (b) of the treated wool fabrics after
vertical burning tests
65
B1 Classification: char length≤15cm
B2 Classification: char length ≤20 cm,
B3classification: no special requirement.(GB8624-2012)

64. 66
Table 13 PCFC parameters for the wool fabrics treated with PA.
HRC= Heat release capacity
pHRR = peak heat release
THR= Total heat release
Tmax= Maximum heat release

65. Fig. 34 TG curves of wool fabrics under air (a,b)and nitrogen (c,d)
67
a
b

66. Fig. 35 FT-IR spectra of (a) PA and (b) wool fabrics
68

67. Fig. 36 SEM micrographs of wool fibers (a,b) and char residues (c)
69

68. Fig.37 P(phosphorous) content of wool fibers and corresponding
char residues determined using ICP-OES
70

69. Fig. 39 P content of wool fibers determined
using SEM-EDS
Fig. 40 Whiteness of the wool fabrics treated
with PA
71

70. Fig. 41 Stress-strain curves of the
untreated and treated wool fabrics
Fig. 42 LOI of the treated wool
fabric after laundering
72

71. CONCLUSION
• PA (Phytic acid)has been proven to be a potential flame
retardent agent because of its high char-forming ability
• Provides an opportunity for producing FR wool fabrics
using a green FR reagent
73

72. Environmental friendly bioactive finishing of wool textiles
using the tannin-rich extracts of Chinese tallow (Sapium
sebiferum L.) waste/ fallen leaves
To impart bioactive finishing to wool by using tannin-rich waste
leaves extract of Chinese tallow through simple adsorption
technique
Zhou et al. 2019
6
74

73. • Materials: 100% pure knitted wool fabric
• Chinese tallow leaves powder
• Camphor green leaves (chlorophyll extract for biomordanting)
• Ferrous sulfate, potassium aluminium sulfate, sodium carbonate, hydrogen
chloride, aluminium chloride, sodium nitrite, ABTS(2,20-Azino-bis(3
ethylbenzothiazoline-6-sulphonic acid)
• Folin –Ciocalteu reagent
MATERIALS
METHODS
Extraction under simple water
bath conditions using UV-Visible
absorption method
0.5g of CT leaves powder , MLR:100:1, pH: 1-8,Temp:
40-1000C, Time interval: 40-120 min
Effect of substrate concentration on the extraction
efficiency of CT colorants
0.1-0.5g / 50 ml of water
Effect of the solvent system under different ethanol-water
(Organic-aqueous) ratio of 70:30, 50:50, and 30:70 was also
conducted
Centrifuged at 10,000rpm
for 15 min to collect the
supernatent
75
Filteration
Evaporation at room temp.

74. Dye component characterization and thermal stability
Analysis of dye extraction: UV–visible spectrophotometer
TGA: TG 209 F3 Tarsus thermal analyzer
DSC: DSC 25 thermal instrument
Antioxidant property of CT leaves : ABTS assay
TPC Folin-Ciocalteu reagent procedure in terms of gallic acid equivalents
Dye(40mg)+ gallic acid (0.2-2 mg/ml)+ Folin-Ciocalteu reagent (0.5ml)+10ml
1.5 ml of 20% Na2CO3 , heating at 400C
15 min
Dyeing with and without mordants: Optimizing dyeing variables, pH(1-8), Temp.
(50-900C), Dye concentration(10-50%owf), Time: 30-90 min
Premordanting: 5% each of ferrous sulphate, alum and chlorophyll extract to alter
the functional properties
76
755nm

75. 77
Colour measurement and fastness properties: Datacolr 650 TM
spectrophotometer
Wash fastness: Digi Wash-SSTMISO 105- C06:1994
Dry and Wet rub fastness : Digi CROCK™ (Crockmeter) as per ISO
105/X12:2001
Functional properties:
Sun protection(UV): YG912E Textile antiultraviolet Performance tester(EU:
13758-2001)
Antioxidant: ABTS assay
Antibacterial: Optical density measurement of incubated culture at 595nm

76. Procedure for ABTS solution
ABTS (1.74gm) + 0.67 g potassium
persulphate+ 1000ml water
Different concentrations of CT leaves
extract ranging between(0.15-0.5mg/ml)
mixed with 5ml of diluted ABTS
Absorbance at 734mm
C= absorbance value of control (ascorbic)
S= absorbance value of sample
78

77. Fig. 43 Chemical components of C. tallow leaves extract
79

78. Fig. 44 UV–Visible spectra of Chinese tallow dye solution
80
Results and discussion

79. Fig.45 Optimization of extraction parameters of CT natural dye (a) pH (b) temperature
(c) CT dose/amount (d) time
81

80. Fig. 46 Effect of different ethanol-aqueous ratio on extraction capacity
82

81. Fig. 47 FT-IR spectra of extracted dye.
S. No. Chemical
constituents
Amount per 1 mg
extract
1 Phenolics (Tannins) 0.59
2 Flavonoids 0.69
Table 13 Total phenolic and flavonoid content present in extracted dye powder
83

82. Fig. 48 Thermal stability of extracted dye (a) TG
84

83. Fig. 49Optimization of dyeing variables using reflectance spectroscopy (K/S) (a)
pH (b) Temperature (c) Dye concentration (d) Time 85

84. Fig. 51 Antioxidant properties CT leaves
Fig. 52Antioxidant properties wool
fabric dyed with extracted CT dye
86

85. Fig. 53 Percentage inhibition of dyed wool fabric on different bacterial strains
87

86. S. No. Sample Transmittance UPF
values
Grading
T(UV) A T(UV) B
1 Original Wool fabric 11.15 6.34 12.46 Bad
2 Un-mordanted 3.70 2.30 33.70 Very good
3 FeSO4. 5H2O 2.38 1.95 42.59 Excellent
4 KAl(SO4)2 2.82 2.00 40.60 Excellent
5 Chlorophyll extract
(CE)
2.88 2.23 37.45 Very good
Table 14 Anti-UV properties of wool fabric dyed with 50.0% (o.w.f.) CT extract
88

87. CONCLUSION
• Higher ethanol/water ratio(70:30) in conjunction with small
amounts of alkali and acid gave better extraction results
• FTIR: tannin functional groups
• Two metal mordants and one biomordant: enhanced the shade
palette(dark black to dark yellow)
• Excellent UV properties, antioxidant and antibacterial: bioactive
sutures, bandages, wound dresseingd
89

88. Enhanced insect-resistance, UV protection, and antibacterial and
antioxidant properties exhibited by wool fabric treated with
polyphenols extracted from mango seed kernel and feijoa peel
To impart multifunctional property to wool fabric
Hassan 2019
7
90

89. Materials: Plain woven wool fabric)
Mango and feijoa fruits
• 2,2 Azino-bis (3 ethylbenzothiazoline-6- sulphinic acid) diammonium salt (ABTS),
citric acid, disodium hydrogen phosphate
Extraction of PPs from mango seeds and feijoa peels
Bottles were shaken a 220rpm at
500C for 90min
Powederd feijoa peel was dispersed
in 80% acteone and 20% water
Filteration and concentration by
rotary evaporator
Freeze drying(PP-2)
Centifugation at 4000rpm, 5 min,
room temperture
Kernel powder(50g)+water at a
consistency of 10%
Supernatents removed by decanting
Freeze drying
Yellowing brown color mango
seed powder(PP-3)
Tannic acid(PP-1)
91

90. Treatment of wool with PPs
Pre-dissolved PPs, 5g/l sodium sulphate
(lavellng agent)+water
Wool fabric wrapped on a perforated
carrier was introduced into the vessel
for 15 min at 980C
Rinsing and drying of fabric at 600C for
30 min
• Assesment of antibacterial activity: AATCC method 147-1998 by parallel streak method
• Assesment of insect resist performance: Tineola bisselliella by following the wools of
New Zealand Test Method 25: ISO 3998-1977
• Antioxidant activity: ABTS decolourisation assay
Surface characteristics
• Surface morphology: SEM
• Contact angle: KSV contact angle measurement
• Surface resistance: Surface/ volume resistance
meter
92

91. Chemical structures of components of mango seed kernel and feijoa peel extracts
93

92. Fig. 54 FTIR spectra of PP-1, PP-2, and PP3
94

93. Fig. 55 Effect of treatment pH on the UV transmission of wool fabrics treated with various
PPs. 95

94. Fig. 56 Effect of concentrations of PP-1, PP-2,
and PP-3 on the UV transmission of wool
fabrics treated with various PPs
Fig. 57 Effect of treatment pH and
the applied dosage of PPson the
surface resistance of the treated wool
fabric
96

95. PP-2
PP-1
PP-3
Untreated
Fig. 58 Antibacterial performance of wool fabric treated with polyphenols extracted from various
plants against various bacteria

96. Table 15 Bioassay of wool fabric treated with various PPs against Tineola bisseliella
98

97. Fig. 59 Surface morphologies of untreated (a) and wool fabrics treated with 5% owf PP-
1 (b) PP-2 (c) and PP-3 (d)
99

98. Sample ID 0 s 30 s 60 s 90 s 120 s
Untreated 121±90.5 117.0± 0.3 114.7 ± 0.7 112.0 ±1.1 110.5 ± 1.3
PP-1 96.3 ±1.8 88.8 ± 1.4 57.8 ±1.5 46.0 ± 1.1 28.1 ± 0.9
PP-2 121.3± 1.2 101.7 ± 0.7 79.2 ± 1.1 39.9 ± 0.8 0
PP-3 117.3 ±2.2 30.3 1.5 0 0 0
Table 16 Dynamic contact angle of surfaces of untreated and treated wool fabrics
100
Fig. 60 Optical images of
shape of droplets of water at
various times

99. Fig. 60 Effect of applied dosage of PP on the antioxidant activity of wool fabric
treated with various PPs
101

100. CONCLUSION
• PPs extracted from mango seed kernel (PP-3) not only work as an
antibacterial agent but also can replace synthetic pyrethroids used
in wool industry as an insecticide
• treatment with PP-3 also enhanced UV radiation protection ability
of wool fabric and also made the fabric antistatic, antioxidant, and
hydrophilic
102

101. Economically viable UV-protective and antioxidant
finishing of wool fabric dyed with Tagetes erecta flower
extract: Valorization of marigold
To impart multifunctional property to wool fabric by waste
utilization
Shabbir et al. 2020
8
103

102. MATERIALS AND METHODS
Dyestuff, chemicals
and textile substrate
Caretenoid colorant’s
extraction
Mordanting and
dyeing
Color characteristics
Fastness properties
UV protection
Powdered marigold flowers dyestuff, ABTS (2,2′-Azino-
bis (3-ethylbenzothiazoline-6-sulphonic acid) ammonium
salt) Alum, ferrous sulphate, stannous chloride
ML: 1:20, Temp: 900C, Time 45min(repeated three times)
3 metal mordants(Alum(10%owf), Iron sulphate(5%owf),Tin
chloride(1%owf)) at 900C for 60min
MLR: 1:40, Ph=7, Time: 60min,Temp.= 900C
HunterLab UltraScan PRO reflectance spectrophotometer
ISO 105-B02:1994
Labsphere UV-1000F ultraviolet transmittance analyzer
Antioxidant activity
Antioxidant activity =A control-A sample/A controlх100, where
A contro=initial absorbance of ABTS+, A sample=absorbance of
remaining ABTS·+
104

103. S. No. Wool Sample L* a* b* c* h°
1 5% MG 66.89 2.09 33.67 33.73 86.45
2 10% MG 58.78 1.79 36.01 36.06 87.16
3 15% MG 56.18 1.40 36.44 36.47 87.79
4 20% MG 54.32 1.39 35.30 35.33 87.74
5 Al+20% MG 53.03 7.74 48.15 48.77 80.86
6 Fe+20% MG 55.41 6.18 34.24 34.79 79.77
7 Sn+20% MG 59.18 5.86 38.81 39.25 81.42
Table 17 Color characteristics of dyed wool (MG=Marigold)
RESULTS AND DISCUSSION
105

104. Fig. 61 Color strength (K/S) variation with the effect of (a) Dye concentration, (b)
metallic mordants 106

105. Fig. 62 % UV transmittance in the region of 250–450 nm range (a) Dye conc. variation,
(b) Metallic mordants variation
107

106. Fig. 63 UV protection in terms of UPF with the
effect of dye concentration and metallic
mordants
Wool Sample T(UV-A)% T(UV-B)% UPF Rating
Undyed 22.39 13.58 <15 Bad
5% MG 3.43 2.53 25–39 Very good
10% MG 1.95 1.74 50+ Excellent
15% MG 1.76 1.68 50+ Excellent
20% MG 1.80 1.77 50+ Excellent
Al+20% MG 1.68 1.67 50+ Excellent
Fe+20% MG 1.48 1.51 50+ Excellent
Sn+20% MG 2.22 2.22 40-50+ Excellent
Table 18 Dye conc. and mordants effect on UV protection parameters(MG=Marigold)
108

107. Fig. 64 Antioxidant activity of Marigold dyed wool fabric samples
109

108. CONCLUSION
• Ecofriendly and waste utilization approach
• Application of metallic mordants improved the UPF value
• Coloration, UV protection, and antioxidant properties are
quite high and very low concentration of dye (even 5%owf)
succesfully imparted durable functionalities
110

109. Use of pomegranate peels and walnut green husks as the green
antimicrobial agents to reduce the consumption of inorganic
nanoparticles on wool yarns
To determine the antimicrobial activity of wool yarns by in situ
synthesis of nanoparticles
Kiakhani et al. (2020)
9
111

110. MATERIALS AND METHODS
Wool yarns(200Tex)
Pomegranate peels and Walnut green husks
Dried at 400C , particle size b/w 0.2 and 0.4mm
AgNO3(99.8), ZnO(99.9%), Cu2O(97%)
Washing the wool samples (MLR: 1:40, 600C, 30min)
Wool treatment with Ag/Cu2O/ZnO Nps
Aueous solution (0.1,0.15,0.20%owf), 30ml water, citric acid(4%owf)
Sodium hypophosphite(4%owf) at pH(4)
Wool samples(1g) immersed in the solution, shaking rate 120rpm, 500C, 2h
Rinsing and drying 112

111. Dyeing method
Solvent extraction at 900C,
90min, MLR: 1:40
Raw and pretreated wool
dyed with different
concentrations(5-100%owf),
pH(3,5,7),60 min, 600C
Rinsing and drying
Testing
Color strength Gretag Macbeth spectrophotometer
Dyeing fastness properties ISO 105 C06 C2S:1994 (E)
Antimicrobial test AATCC 100-2004
Characterization
Surface crystallinity Siemens D5000 X-ray
diffractometer
Surface morphology LEO 1455VP scanning
electron microscope
(SEM
113
X-ray diffractometer

112. In situ formation of metal nanoparticles on wool fibers
114

113. Fig. 66 XRD spectra of (a) original wool fabric, (b) wool treated by Ag, (c) wool
treated by Zn, (d) wool treated by Cu, (e) wool treated by Ag/Zn, (f) wool treated by
Ag/Cu, (g) wool treated by Cu/Zn
230
115

114. Fig. 67 SEM images of wool fibers (a) untreated/raw, (b) treated with Ag salt, (c)
treated with Zn salt, (d) treated with Cu salt, (e) treated with Ag þ Zn salts, (f) treated
with Ag þ Cu salts, (g) treated with Cu þ Zn salts. 116

115. Sample code Max. Load at Break (N) Elongation at Break (%)
Wool 166.29 41.70
Wool-Ag 169.15 42.63
Wool-Cu 169.20 42.28
Wool-Zn 169.24 42.14
Wool-Ag/Cu 169.12 42.56
Wool-Ag/Zn 169.06 42.17
Wool-Cu/Zn 169.08 42.31
Table 19 Physical properties of the raw and treated wool yarns
117

116. Fig. 68 Effect of (a) initial dye concentration, (b) temperature, (c) time, (d) pH on the
color strength of wool yarns
30% 1000C
60min
118

117. Dye Pre-
treated
with
Before dyeing process After dyeing process
L* a* b* K/S DE* L* a* b* K/S DE*
Pomegranate peel
- 62.82 5.91 17.78 7.78 0.00 62.82 5.91 17.78 7.78 0.00
Ag 54.48 4.52 19.74 8.07 8.67 46.59 9.14 31.59 14.40 21.55
Ag-Zn 55.59 5.27 21.60 8.31 8.20 44.80 8.90 30.16 14.64 22.06
Ag-Cu 47.98 1.97 22.68 13.47 16.11 57.24 7.42 24.45 8.33 8.82
Zn 57.71 4.57 19.74 7.57 5.63 63.75 5.79 25.47 7.46 7.74
Zn-Cu 52.27 1.69 24.28 10.87 13.09 49.70 1.36 24.60 13.38 115.47
Cu 52.66 1.21 23.08 10.21 12.38 49.38 2.27 25.75 14.07 16.04
Green Walnut husks
- 37.65 8.32 17.78 11.21 0.00 37.65 8.32 17.78 11.21 0.00
Ag 39.95 8.33 18.91 10.36 2.56 34.27 9.41 20.92 16.37 4.74
Ag-Zn 41.76 7.00 18.95 18.10 4.49 35.76 8.83 19.55 13.55 2.63
Zn 43.38 6.40 19.93 9.68 6.41 36.05 6.82 16.25 12.35 2.67
Ag-Cu 41.84 8.20 18.11 8.49 4.20 36.22 8.72 16.09 11.58 2.24
Zn-Cu 42.02 6.98 18.68 9.55 4.65 35.55 7.03 16.23 12.79 2.91
Cu 35.20 11.00 25.54 9.96 8.56 35.91 7.03 16.23 12.49 2.66
Table 20 Color coordinates for the treated and untreated samples before and after dyeing with the
natural dyes
119

118. Sample %(o.w.f.) Antibacterial activity (%)
Un-dyed samples Pomegranate peels Green Walnut husk
E. coli S.aureus E. coli S.aureus E. coli S.aureus
Wool-Ag - - - 70.65 64.72 63.33 55.19
0.1 16.21 12.60 74.07 67.24 68.14 62.81
0.15 86.38 79.43 99.80 99.64 98.27 97.25
0.20 100 100 100 100 100 100
WoolAg/Zn 0.1 14.08 10.70 72.48 65.86 64.21 60.46
0.15 75.72 70.38 96.27 91.42 92.57 88.75
0.20 100 100 100 100 100 100
Wool-Ag/Cu 0.1 15.19 13.82 73.82 70.89 65.33 69.49
0.15 68.43 65.45 99.92 99.56 99.80 98.22
0.20 100 100 100 100 100 100
Wool-Zn 0.1 10.44 7.17 74.28 63.48 65.74 56.24
0.15 42.36 37.92 80.06 68.23 71.18 60.54
0.20 60.87 58.43 88.47 75.12 75.60 67.58
Wool-Zn/Cu 0.1 12.73 50.27 78.18 71.48 67.42 58.60
0.15 62.49 58.33 96.77 89.37 94.88 86.37
0.20 73.52 68.73 98.12 91.24 96.46 89.52
Table 21 Antibacterial properties of the wool samples treated with various inorganic salts and
dyed with the natural dyes against E. coli (gram-negative) and S.aureus (grampositive) bacteria
120

119. Sample Washing cycle Antibacterial activity (%)
Un-dyed samples Pomegranate peels Green Walnut husk
E. coli S.aureus E. coli S.aureus E. coli S.aureus
Wool-Ag 1 86.38 79.43 99.80 99.64 98.27 97.25
5 82.14 75.22 96.25 96.70 95.62 94.30
10 75.16 70.85 92.86 92.55 92.48 91.17
WoolAg/Zn 1 75.72 70.38 96.27 91.42 92.57 88.75
5 70.28 65.38 93.50 88.19 88.45 85.64
10 66.42 61.42 89.87 84.66 82.63 81.42
Wool-Ag/Cu 1 68.43 65.45 99.92 99.56 99.80 98.22
5 64.02 61.23 96.53 95.69 96.33 94.70
10 59.76 56.49 93.31 93.20 92.48 91.66
Wool-Zn 1 42.36 37.92 80.06 68.23 71.18 60.54
5 36.54 34.20 77.25 65.08 68.33 56.38
10 32.41 28.68 73.04 62.39 64.75 52.50
Wool-Zn/Cu 1 62.49 58.33 96.77 89.37 94.88 86.37
5 57.30 54.41 92.48 86.28 91.22 83.01
10 51.98 48.07 89.36 82.96 88.76 79.46
Wool-Cu 1 65.50 61.17 96.62 94.46 94.65 92.54
5 61.78 56.30 92.96 91.07 91.72 88.20
10 56.64 52.79 89.00 88.85 87.86 84.36
Table 22 Antimicrobial activity to washing durability
121

120. CONCLUSION
• Environmemt friendly approach for in situ formation of NPs
on the surface of wool fibres
• Improved color strength, fastness and antibacterial
properties of wool yarn
• Optimum conditions: initial dye concentration(30% owf, pH
5, 1000C, 60min)
122

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