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Antibacterial Finishes for Textiles
using Herbal Sources
by
Shameembanu A. ByadgiShameembanu A. Byadgi
2
3
Introduction
 The rapid growth in technical textiles and their end-uses has generated
many opportunities for the application of innovative finishes
 Novel finishes of high added value for apparel fabrics are also greatly
appreciated by a more discerning and demanding consumer market
 Antimicrobial textiles with improved functionality find a variety of applications
such as health and hygiene products, specially the garments worn close to
the skin and several medical applications, such as infection control and barrier
material
 Although, the synthetic antimicrobial agents are very effective against a range
of microbes and give a durable effect on textiles, they are a cause of
concern due to the associated side effects on humans and environment
 There is a great demand for antimicrobial textiles based on eco- friendly
agents which not only help to reduce effectively the ill effects associated
due to microbial growth on textile material but also comply with statutory
requirements imposed by regulating agencies
4
Antibacterial finish
 The plant products comprise the major segment among all the natural
antibacterial agents
 Healing power of some of the plant materials has been used since
ancient times
 Relatively small percentage (1-10%) of these is used as food by both humans
and other animal species
 Plants produce secondary metabolites which serve as plant defense
mechanisms against predation by microorganisms, insects and herbivores
 Some compounds such as terpenoids give plants their odours; others (quinones
and tannins) are responsible for plant pigment
 Many compounds are responsible for plant flavour (terpenoid capsaicin from
chilli peppers)
5
Necessity of Antibacterial Finishes
1. To avoid cross infection by pathogenic microorganisms
2. To control the infestation by microbes
3. To arrest metabolism in microbes in order to reduce the formation of odour
4. To safeguard the textile products from staining, discoloration and quality
deterioration
6
Requirements for Antimicrobial Finish
Durability to washing, dry cleaning and hot pressing;
Selective activity to undesirable microorganisms;
Should not produce harmful effects to the manufacturer, user and the
environment;
Should comply with the statutory requirements of regulating agencies;
Compatibility with the chemical processes;
Easy method of application;
No deterioration of fabric quality;
Resistant to body fluids; and
Resistant to disinfections/sterilization
7
Natural antibacterial agents for textiles
 Neem extract
 Aloevera
 Sericin
 Chitosan
 Tea tree
 Tulsi leaves
 Clove oil
 Cinnamon
 Pomegranate rind
 Eucalyptus
 Periwinkle
 Henna leaves
8
Antibacterial finishing methodologies
 Exhaust technique
 Pad-dry-cure method
 Coating technique
 Spray technique
 Microencapsulation
 Nanoencapsulation
9
Methods for improving the durability of the finish
1. Solubilisation of the active substances in/on the fibre
2. Treating the fibre with resin or cross-linking agents
3. Micro encapsulation of the antimicrobial agents with the fibre matrix
4. Coating the fibre surface
5. Chemical modification of the fibre by covalent bond formation
6. Use of graft polymers, homo polymers and/or co-polymerization on to the
fibre
10
Evaluation of Antibacterial Activity
QualitativeQualitative QuantitativeQuantitative
Bacterial reduction method
(AATCC 100-2004)
Bacterial reduction method
(AATCC 100-2004)
Parallel streak method
(AATCC 147-2004)
Parallel streak method
(AATCC 147-2004)
Agar diffusion plate test
(ISO 20645)
Agar diffusion plate test
(ISO 20645)
11
Parallel streak method
(AATCC 147-2004)
12
Calculations and results
 Examine the incubated plates for interruptions of growth along the streaks of
inoculum beneath the specimen and for a clear zone of inhibition beyond the
edge
 The average width of zone of inhibition along a streak on either side of test
specimen is calculated by
W = T – D / 2
W = width of clear zone of inhibition (mm)
T = total diameter of test specimen and clear zone (mm)
D = diameter of test specimen (mm)
13
Antibacterial effect
Growth Description Assessment
No growth Zone of inhibition is seen Diffusible antibacterial
activity
No growth under the
fabric
No zone of inhibition Bacteriostatic antibacterial
activity
Growth under the
fabric
No inhibition zone Antibacterial activity is
absent
14
Agar diffusion plate test
(ISO 20645)
15
Calculations and results
 Examine the incubated plates for absence or presence of bacterial growth in the
contact zone between agar & specimen and inhibition zone around the specimen
H = D – d / 2
H = width of inhibition zone (mm)
D = total diameter of test specimen and inhibition zone (mm)
d = diameter of test specimen (mm)
 Examine the contact zones under the specimen for bacterial growth
16
Antibacterial effect
Inhibition zone (mm)
Mean value
Growth Description Assessment
> 1 None Inhibition exceeding 1 mm, no
growth
Good effect
1 - 0 None Inhibition zone up to 1mm, no
growth
0 None No inhibition zone, no growth
0 Slight No inhibition zone, only some
restricted colonies, growth
nearly totally suppressed
Limit of
efficacy
0 Moderate No inhibition zone, compare to
control growth reduced to half
Insufficient
effect
0 Heavy No inhibition zone, compare to
the control no growth
reduction or only slightly
reduced growth
17
Bacterial reduction method
(AATCC 100-2004)
18
Calculations and results
 Report bacterial counts as the number of bacteria per sample
 Percent reduction of bacteria by the specimen treatment is calculated by
R = [(B – A)/ B] x 100
R = percent reduction
A = no. of bacteria recovered from inoculated treated test specimen swatches in
the
bottle incubated over desired contact
B = no. of bacteria recovered from inoculated treated test specimen swatches in
the
bottle immediately after inoculation
Antimicrobial activity of cotton fabric treated with Quercus
infectoria extract
Gupta and Laha, 2007
New Delhi, India
Objective
To study the antimicrobial properties of cotton fabric treated with QI
extract against selected bacterial species that cause infections in hospitals and
unpleasant odour on textiles
19
Methodology
Plain weave cotton fabric 107 g/m2
weight, 40 ends/cm and 35 picks/cm
Application of QI extract
Samples were rinsed with cold water, soaped with 0.5 g/L non-ionic detergent
(Lissapol N) and dried
MLR 1:30 at 60ºC and neutral pH
Pretreatment with alum (1 & 5% owf) at 80ºC and later treated with QI for 45 mins
Post mordanting of QI treated samples with copper sulphate (1 & 5% owf)
20
21
Scoured cotton was also treated with 0.5% (owf) Fabshield (commercial
antimicrobial agent) at 50ºC and 4.5 pH for 20 min followed by curing at
130-135ºC
Wash fastness (ISO II test)
Wash durability for retention of antimicrobial finish after single and 5 launderings
22
Assessment of antibacterial activity
Qualitative : Parallel streak method (AATCC 147-1993)
Quantitative : Agar plate method (AATCC 100-1993)
Microbial inhibition was determined by the reduction in number of colony
forming units (CFU)
Reduction in microbial colonies = B – A x 100
B
where A = CFU/ml for treated sample after 24h incubation
B = CFU/ml for untreated sample incubated under identical conditions
Table 1. Effect of dye and mordant on antimicrobial activity of treated cotton
fabric
+ = growth under fabric Nil = no growth under fabric
Results and DiscussionResults and Discussion
Cotton fabric
Growth Zone of inhibition (mm)
E. coli B. subtilis E. coli B. subtilis
Control + + 0 0
Fabshield treated Nil Nil 0 0
Treated with
QI Nil + 4.0 3.0
QI + 1% alum Nil + 1.0 0.5
QI + 5% alum Nil + 2.0 1.0
QI + 1% CuSO4 Nil Nil 1.5 0
QI + 5% CuSO4 Nil + 1.5 1.5
23
Figure 1. Parallel streak test on cotton against S. aureus
[(a) control and (b) sample treated with QI]
Figure 2. Antimicrobial activity of cotton fabric
treated with QI against E. coli
Figure 3. Antimicrobial activity of cotton
fabric treated with QI on B. subtilis 24
a b
Table 2. Retention of antimicrobial activity by treated cotton after sample
launderings
Bacteria Cotton fabric
After single laundering After 5 launderings
Reduction
in cfu %
Activity
retention (%)
Reduction
in cfu %
Activity
retention (%)
B. subtilis Control Nil Nil Nil Nil
Treated with
QI 33 55 0 0
QI + 5% alum 83 99.1 75 89.6
QI + 1% CuSO4 84.1 100 83 99.6
E. coli Control Nil Nil Nil Nil
Treated with
QI 55.6 65.4 61.1 62
QI + 5% alum 30.2 84.4 27.1 75.6
QI + 1% CuSO4 50.6 75.1 56.0 77.4
25
 12% QI extract (owf) was found to be effective concentration against
selected microbes
 The activity was greatly enhanced when 5% alum or 1% copper sulphate
was used as a mordant
 Studies on durability of the treatment showed that the QI treatment was not
durable to washing and the antimicrobial activity was lost completely after 5
launderings
 Mordanted samples showed 80-100% retention of activity even after 5
washes
Conclusion
26
Application of Prickly chaff (Achyranthes aspera Linn.)
leaves as herbal antimicrobial finish for cotton fabric used
in healthcare textiles
Thilagavathi and Kannaian, 2008
Tamil Nadu, India
Objective
To utilize methanolic extract of prickly chaff leaves to develop
microbial resistant cotton fabric for healthcare textiles
27
Methodology
28
Extraction process
Grinding of dried leaves into very small units
Extracted of active constituents by methanolic extraction method and sonication
Shade drying of prickly chaff leaves @ 38-40ºC till the moisture reduces to
14%
Table 3. Box and Behnken method for optimization of process parameters
Test No. Extract conc. (%) Temperature (ºC) Citric acid conc. (%)
1 3 40 8
2 7 40 8
3 3 60 8
4 7 60 8
5 3 50 7
6 7 50 7
7 3 50 9
8 7 50 9
9 5 40 7
10 5 60 7
11 5 40 9
12 5 60 9
13 5 50 8
14 5 50 8
15 5 50 8
29
30
Results and DiscussionResults and Discussion
Table 4. Antimicrobial efficacy of the treated samples based on Box and
Behnken experiments
Test No.
Agar diffusion test
Zone of inhibition (mm)
Parallel streak test
Zone of inhibition (mm)
Challenge test
Bacterial reduction (%)
S. aureus E. coli S. aureus E. coli S. aureus E. coli
1 49 21 4.5 2.5 97.83 56.58
2 47 16 4.2 0 96.99 45.00
3 41 16 4.6 1.5 60.00 25.00
4 43 20 4.1 1.6 95.89 26.36
5 39 16 3.5 1.4 93.34 45.25
6 37 17 3.0 0 92.70 56.56
7 31 15 4.9 1.5 96.63 72.00
8 32 25 3.2 2.0 65.05 73.00
9 43 26 3.1 0 92.82 56.00
10 45 18 4.5 1.2 98.45 45.00
11 43 17 2.5 1.5 98.65 69.23
12 42 27 2.6 0 55.43 45.12
13 40 20 3.5 1.0 92.74 56.56
14 40 20 3.5 1.0 92.74 56.56
15 40 20 3.5 1.0 92.74 56.56
31
Conclusion
 The fabric samples treated with methanolic extract of prickly chaff leaves
applied by pad-dry-cure method possessed better antimicrobial activity
against Staphylococcus aureus and Escherichia coli
 Hence, the treated cotton fabric can be used for healthcare textiles
32
Experimental study on antimicrobial activity of cotton
fabric treated with aloe gel extract from Aloe vera plant for
controlling the Staphylococcus aureus (bacterium)
Jothi, 2009
Ethiopia
Objective
To develop an ecofriendly natural herbal finish from A. vera extracts
for various textile applications
33
Methodology
34
Fabric Bleached cotton fabric with 28 ends/cm, 25 picks/cm, plain
weave and 40 x 40 Ne count
Chemicals Citric acid and methanol
Aloe gel Antimicrobial agent [1, 2,3,4 and 5gpl]
35
Extraction process
36
Application of antimicrobial finish
37
Assessment of antibacterial activity
Shake flask method (ATCC 6538)
Bacterial reduction was determined by using the formula
Reduction in microbial colonies = A – B x 100
A
where A = Number of colonies before shaking
B = Number of colonies after 1 hour shaking
Hohenstein modified test method – challenge test
The finished samples were washed using a standard detergent (2% owf) and
sodium carbonate (1% owf) at 60°C. The antimicrobial activity was assessed after
50 washes
Results and DiscussionResults and Discussion
Figure 4. Antimicrobial efficiency of Aloe
gel treated sample (Agar Diffusion Test)
Figure 5. Antimicrobial activity of untreated
sample 38
Table 6. Quantitative analysis test results
Sl.
No.
Bacteria
Finishing agent conc.
(gpl)
%of bacteria reduction
after treatment
1 Staphylococcus 1 97.00
2 97.90
3 98.10
4 98.40
5 99.10
95.5
96.0
96.5
97.0
97.5
98.0
98.5
99.0
99.5
54321
Finishing agent concentration (gpl)
Figure 6. Antimicrobial efficiency of
aloe gel treated sample against S. aureus
(Shake flask Method)
39
Table 7. Durability of antimicrobial effect of treated sample (5 gpl)
after 50 washes
Sl. No. Number of washes Antimicrobial effect (%)
1 10 99.70
2 20 99.30
3 30 99.10
4 40 98.40
5 50 98.00
40
Conclusion
 The specimens treated with the solution containing 5gpl aloe gel showed
excellent antimicrobial activity
 The treated sample showed high reduction rate in the number of colonies
grown and a clear zone of bacteria inhibition
 Finish durability to washing of antimicrobial property of the aloe gel treated
sample was 98% after 50 washing
 The finding of the study suggested that the treated fabrics can be used for
textile application
41
Dyeability and Antimicrobial Properties of Cotton Fabrics
finished with Punica granatum extracts
Rajendran et al., 2011
India
Objective
To investigate the antibacterial functionality of cotton fabric dyed
using Punica granatum rind extract
42
Methodology
43
Extraction process
Aqueous extraction Ethanol extraction
Add 10g P. granatum rind powder to
100ml distilled water
Filtered through Whatmann No. 1 filter
paper
The filterate was stored at 4ºC
Add 20g powder to 100 ml ethanol and
kept @ room temperature for 48 hrs
Filtered to obtain a clear filterate
Filterate was condensed through a rotary
vacuum evaporator @ 60ºC for 30 min
44
Assessment of antibacterial activity
Qualitative : Disc diffusion method (SN 195920-1992) and parallel streak
method (AATCC 147-2004)
Quantitative : Percentage reduction method (AATCC 100-2004)
% reduction = A - B x 100
B
A = surviving cells (CFU/ml) for control (blank cotton fabric)
B = surviving cells (CFU/ml) for test samples (natural dyed cotton fabric)
Wash durability test
AATCC-100 test
5% neutral soap for 20 mins
2, 4, 6, 8 & 10 launderings
Table 8. Preliminary assessment of antimicrobial activity of natural dye
Results and DiscussionResults and Discussion
Sl.
No.
P. granatum
extracts
Antibacterial activity
(Zone of inhibition in mm)
E. coli S. aureus
1. Aqueous 8 14
2. Ethanol 10 17
45
Qualitative antimicrobial assessment
(a) (b)
Figure 7. Agar diffusion method of (1) P. granatum treated fabric (2) Untreated sample against
(a) E. coli and (b) S. aureus
(a) (b)
Figure 8. Parallel streak method of P. granatum treated fabric against (a) E. coli and (b) S. aureus
46
Quantitative assessment
Table 9. Antibacterial activity of treated fabric by percentage reduction test
Test organisms
Survival cells (CFU/ml)
% bacterial
reduction
Control
fabric
Treated
fabric
Staphylococcus aureus 9.5 x 106
0.4 x 106
95.7
Escherichia coli 9.5 x 106
1 x 106
89.4
Wash durability
Figure 9. Wash durability test
47
Conclusion
 The fabric dyed with P. granatum rind extracts displayed excellent
antibacterial activity against both the test organisms
 The results demonstrated that utilizing extracted natural colourants as
dyeing materials significantly facilitate in obtaining quality fabrics having
dyeability and antibacterial properties
 The method of extraction and application of dyestuff from natural
colourants may help to optimize the technical aspects of natural dyeing
process
48
Antibacterial efficacy analysis of Punica granatum L. leaf,
rind and Terminalia chebula fruit extract treated cotton
fabric against five most common human pathogenic bacteria
Rathinamoorthy et al., 2011
Tamil Nadu, India
Objective
To develop an ecofriendly natural antimicrobial finish from plant
extracts for textile application
49
Methodology
50
Extraction process
Fresh leaves & rind of Punica granatum L and Terminalia chebula fruits
Shade dried and made into fine powder
10 gm of powder of each was soaked in methanol for 24 hours to obtain 10%
concentrated solution
The extracts were filtered
51
Application of finish
Results and DiscussionResults and Discussion
Table 10. Zone of inhibition of treated textile material for different strains
(methanol extract)
Sl. No. Bacteria
Zone of inhibition (mm)
Control
P. granatum
leaf extract
P. granatum
rind extract
T. chebula
fruit extract
1 Staphylococcus aureus - 30 28 38
2 Escherichia coli - 28 26 33
3 Klebsiella pneumonia - 26 25 36
4 Proteus vulgaris - 32 32 34
5 Salmonella typhi - 30 28 32
52
Table 11. Zone of inhibition of treated textile material for different strains
(water extract)
Sl.
No.
Bacteria
Zone of inhibition (mm)
Control
P. granatum
leaf extract
P. granatum
rind extract
T. chebula fruit
extract
1 Staphylococcus aureus - 32 35 34
2 Escherichia coli - 31 34 32
3 Klebsiella pneumonia - 27 29 34
4 Proteus vulgaris - 38 34 34
5 Salmonella typhi - 30 33 32
53
Table 12. Percentage of bacterial reduction by Hohensteins modified
challenge test for methanol extract
Bacterial
strains Sample ‘0’ contact hour
‘24’ contact
hour
%
reduction
S. aureus P. granatum leaf 244 x 10-5
122 x 10-2
99.95
P. granatum rind 220 x 10-4
110 x 10-2
99.50
T. Chebula fruit 224 x 10-3
142 x 10-4
99.36
E. coli P. granatum leaf 136 x 10-4
124 x 10-3
90.88
P. granatum rind 140 x 10-3
121 x 10-3
85.00
T. Chebula fruit 104 x 10-3
196 x 10-2
98.11
54
Table 13. Durability evaluation of treated samples by agar diffusion method
Sources Bacterial strains 5 wash
Inhibition zone (mm)
10 wash
Inhibition zone (mm)
P. granatum rind Staphylococcus aureus - -
Escherichia coli 22 -
Klebsiella pneumonia 26 24
Proteus vulgaris - -
Salmonella typhi - -
P. granatum leaf Staphylococcus aureus 22 -
Escherichia coli 26 21
Klebsiella pneumonia - -
Proteus vulgaris 24 -
Salmonella typhi - -
T. chebula fruit Staphylococcus aureus 28 25
Escherichia coli 24 24
Klebsiella pneumonia 36 26
Proteus vulgaris 26 24
Salmonella typhi - -
55
Table 14. Durability test by quantitative measurement
Bacterial strains Sample ‘0’ contact hr ‘24’ contact hr % reduction
S. aureus P. granatum leaf Control - - No reduction
5 wash - - No reduction
10 wash - - No reduction
P. granatum rind Control - - No reduction
5 wash - - No reduction
10 wash - - No reduction
T. chebula Control - - No reduction
5 wash - - No reduction
10 wash - - No reduction
E. coli P. granatum leaf Control - - No reduction
5 wash 272 x 10-5
128 x 10-5
52.94
10 wash - - No reduction
P. granatum rind Control - - No reduction
5 wash 212 x 10-4
540 x 10-3
74.52
10 wash - - No reduction
T. chebula Control - - No reduction
5 wash 160 x 10-3
230 x 10-2
85.62
10 wash - - No reduction
56
Conclusion
 Agar diffusion test indicated that both water and methanol extract treated
textile material exhibited 27-38 mm of inhibition zone
 Challenge test results indicated that both Punica granatum L leaf and rind
extract treated samples had 99% of bacterial reduction against S. aureus
 In case of E. coli, P. granatum L leaf treated sample showed 87% and the
rind extract treated material showed 79% of bacterial reduction
 T. chebula extract treated material showed higher percentage of reduction for
both S. aureus (99.3%) and E. coli (98.1%)
 The wash durability result indicated that, the effectiveness of the treatment
reduced with the increase in washing cycle
57
Effect of Laundering on Herbal Finish of Cotton
Hooda et al., 2013
Haryana, India
Objective
To develop an eco-friendly herbal antimicrobial finish from Aloe vera
leaves for textile application
58
Methodology
59
Fabric 100 % cotton fabric (unbleached and unfinished); fabric count
of 56 x 44 and GSM - 286
Chemicals Citric acid, acetic acid and methanol
Preparation of Aloe vera extract
Fresh mature green leaves of Aloe vera were collected, washed, weighed
Hot air oven @ 40ºC
Fine powder and weighed
Extraction by maceration process using methanol
Drying
Grind
60
The sample was immersed in Aloe vera extract (3 & 5 g/l) for 30 minutes with
MLR 1:20
Dried at 80ºC for 3 minutes and cured at 120ºC for 2 minutes on a lab model
curing chamber
Padded on a pneumatic padding mangle at a pressure of 2.5 psi, dried at 80°C
and cured at 120 °C
Application of antibacterial finish
61
Determination of Add-on (%)
Add-on (%) = W2−W1 ×100
W1
W1:Weight of fabric before treatment (g)
W2:Weight of fabric after treatment (g)
Determination of Bacterial Population AATCC-100 test method
Durability of Finish to Washing
ISO: 6330-1984E using Launder-o-meter
Results and DiscussionResults and Discussion
Table 15. Weight add-on (%) of Aloe vera treatment on treated cotton fabric
Application
method
Conc.
(g/l)
Weight per unit area of cotton g/m2
)
Aloe vera application
Grey fabric Scoured fabric
g/m2
% g/m2
%
Pad-dry-cure
method
3 309.66 6.17 308.33 6.64
5 320.66 9.94 318.66 10.21
C.D. 2.22 5.67
62
Table 16. Bacterial reduction of Aloe vera treated grey and scoured cotton
fabric by quantitative method
Application
method
Conc.
(g/l)
Bacterial reduction in Aloe vera treated cotton fabric
Grey fabric Scoured fabric
10-2
10-3
10-4
Mean
(103
)
%
reduction
10-2
10-3
10-4
Mean
(103
)
%
reduction
Control Confluent lawn of growth
Pad-dry-cure
method
3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69
5 >300 69 12 9.5 68.50 13 Nil Nil 4.3 96.70
63
Table 17. Wash durability of finish in terms of bacterial reduction percentage
of Aloe vera treated cotton fabric
Method of
application
Bacterial reduction in Aloe vera treated cotton fabric (%)
Pad-dry-cure method
Grey fabric Scoured fabric
Dilutions 10-2
10-3
10-4
Mean
(103
)
%
reduction
10-2
10-3
10-4
Mean
(103
)
%
reduction
Wash
cycles
Conc.
(g/l)
Control Confluent lawn of growth
0 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69
5 >300 69 12 9.45 68.50 13 Nil Nil 4.3 96.70
5 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69
5 >300 69 12 9.45 68.50 13 Nil Nil 4.3 96.70
10 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69
5 >300 69 12 9.45 68.50 13 Nil Nil 4.3 96.70
15 3 >300 103 22 16.15 46.17 24 Nil Nil 8.0 96.67
5 >300 75 17 12.25 59.17 15 Nil Nil 5.0 96.67
20 3 >300 111 35 23.05 23.17 29 2 2 83.0 71.38
5 >300 82 28 18.1 39.67 19 1 1 43.0 77.37
64
Conclusion
 Finished fabric showed very good antibacterial activity as compared to
controlled fabric
 Aloe vera treated scoured fabric exhibited excellent antimicrobial activity
than Aloe vera treated grey fabric
 Wash durability test also revealed that the finish was able to withstand upto
20 washes in case of Aloe vera treated scoured sample
65
Antibacterial and Physical Properties of Knitted Cotton
Fabrics Treated with Antibacterial Finishes
Ureyen et al., 2010
Objective
To investigate the effect of antibacterial application on physical
properties of knitted fabric and the laundering durability of the applied agents
66
Methodology
67
Turkish cotton knitted on circular knitting machine with a fabric weight
of 170 g/m2
and subjected to scouring, bleaching, dyeing
Table 22.Treatment Recipes
Finishing process Recipe Exhausting process
Bleaching + scouring 1 g/L wetting agent
1 g/L scouring agent
3 g/L NaOH
3 g/L H2O2
95°C for 25 min
Neutralization with acid at
70°C
Anti-peroxide at 40°C
Reactive Dyeing 0.005% Remazol Yellow 3RS-A
(C.I. Reactive Yellow 176)
0.0114% Remazol Red 3BS-A
(C.I. Reactive Red 239)
20 g/L Sodium chloride
5 g/L Sodium carbonate
0.8 mL/L sequestering agent
Neutralization with 0.5 mL/L
Acetic acid
Washing: 0.5 g/L soap
Total time: 160 min
68
Antibacterial finishing
Rapid P-A1 model laboratory vertical padder for impregnation and an
Atac GK4 model laboratory stenter for curing
Table 23.Notations and Concentrations of Antibacterial Agents
Antibacterial agents
Notation Type Concentrations
A Organic antimicrobial agent (Triclosan) 60 g/L (pH 4-5)
B Silver and TiO2 5 g/L (pH 5-6)
C Quaternary ammonium salt
(3-trimethoxysilylpropyldimethyloctadecyl
ammonium chloride)
35 g/L (pH 6)
D Silver compound 28.5 g/L (pH 4-5)
Laundering
BS ENISO 26330 standard using Wascator laundering machine with
4 g/L soap for 40 wash cycles
69
Table 24.Test Instruments and Standards
Tests Instruments Standards
Antibacterial - JIS-L 1902:2002
Fabric weight James Heal Circular Fabric
Sample Cutter
ISO 3801
Pilling James H. Heal Nu Martindale
Abrasion and Pilling Tester
ISO 12945-2
Air permeability Textest AG FX 3300 ISO 9237
Bursting strength James H. Heal TruBurst Tester ISO 13938-2
Colour efficiency Minolta CM 3600 d
spectrophotometer
-
Results and DiscussionResults and Discussion
Fig. 12. Mean values of fabric weight results
(NW: Non-Washed, WC: Washing Cycles)
70
Figure 13. Mean values of pilling test results
(NW: Non-Washed, WC: Washing Cycles)
71
Table 18. Mean values of air permeability test results
Sl. No. Particulars
Air permeability (L/m2
/s)
Wash cycles
0 10 20 30 40
1 NW greige fabric 742.91
2 Agent A 553.75 1162.50 1254.55 1396.67 1443.33
3 Agent B 1039.56 1183.64 1192.73 1256.67 1151.67
4 Agent C 609.67 1253.55 1260.53 1343.33 1310.83
5 Agent D 940.18 1220.00 1256.33 1347.27 1241.87
72
Table 19. Mean values of bursting strength test
results
Sl. No. Particulars
Bursting strength (kPa)
Wash cycles
0 10 20 30 40
1 NW greige
fabric
749.86
2 Agent A 787.56 543.40 629.00 607.25 609.20
3 Agent B 590.48 564.84 626.25 586.60 621.32
4 Agent C 687.06 604.46 585.40 588.28 599.88
5 Agent D 616.06 558.16 590.54 558.68 610.14
73
Table 20. Mean values of colour efficiency
Sl. No. Particulars
Colour efficiency (K/S)
Wash cycles
0 10 20 30 40
1 NW greige fabric 0.154
2 Agent A 0.141 0.176 0.277 0.293 0.253
3 Agent B 0.141 0.213 0.232 0.256 0.236
4 Agent C 0.145 0.165 0.221 0.252 0.216
5 Agent D 0.161 0.213 0.223 0.249 0.239
74
Table 21. Antibacterial activity of the treated samples
Sl. No. Particulars
Reduction in bacteria (CFU)
Wash cycles
0 10 20 30 40
1 Agent A 3.70 2.91 3.60 3.63 3.05
2 Agent B 4.78 3.36 3.55 3.50 3.44
3 Agent C 2.26 1.91 1.35 0.32 0.68
4 Agent D 3.50 3.44 3.05 2.93 3.06
75
Conclusion
 The study concluded that fabrics shrunk due to the wet process of antibacterial
treatments, causing a difference in the fabric weights
 Due to the content of the antibacterial agents, pilling, air permeability and
bursting strength of treated samples was lower than that of the untreated
samples, except for the fabrics treated with agent A
 Antibacterial finishing did not affect the colour efficiency of the dyed fabrics
 Laundering affected the colour efficiency of the samples
 Agent B gave the best antibacterial performance, while agent C gave the worst
 The antibacterial activity of agents A, B, and D decreased slightly after several
washings, while that of agent C decreased dramatically
76
Antimicrobial efficiency of Vitex negundo leaf extracts
Mohanraj et al., 2012
Sathyamangalam, India
Objective
 To study the antimicrobial effectiveness of Vitex negundo leaf extracts on
cotton fabric treated by exhaustion and microencapsulation
 To assess the durability of the finish against standard wash cycles and
synthetic perspiration
77
Methodology
78
Fresh nochi (V. negundo) leaves were collected and shade dried within a
temperature range of 37-40ºC
ground and sieved
Nochi leaf powder (25g) was mixed
with 250mL water, boiled for 30 min
and filtered using nylon fabric
10g of nochi leaf powder was extracted in
soxhlet apparatus with 150mL methanol
for 24h
Microencapsulation Nochi leaf extract as core material and
acacia gum as wall material
The microcapsules were freeze dried
79
Samples were treated with herbal extract using 8% citric acid as cross linking
agent by pad-dry-cure method
Padded through padding mangle and dried at 60ºC for 5 min
Application of antibacterial finish
Microencapsulation
80
Evaluation of fabrics
Flexural rigidity ASTM D1388-96, using Shirley fabric stiffness
tester
Antimicrobial activity Agar diffusion method specified in AATCC TM
100
Wash durability Laundrometer at a speed of 40 rpm with ISO 3 test
method
Fastness to perspiration AATCC TM 15-2002
Results and DiscussionResults and Discussion
Table 22. Effect of finishing treatment on flexural rigidity of samples
Samples treated with
Flexural rigidity
(mg cm)
Methanol extract
Warp 35.54
Weft 31.07
Water extract
Warp 36.26
Weft 31.04
Microcapsules
Warp 37.92
Weft 32.37
81
(a) (b)
(c) (d)
Figure 11. Antimicrobial activity of samples treated with padding mangle
(a – S. aureus & b – E. coli) and microcapsules (c – S. aureus & d – E. coli)
82
Table 23. Effect of washing on antimicrobial efficacy of fabric samples
Sample
treatment
Zero wash 5 wash 10 wash 15 wash
S.
aureus
E. coli S.
aureus
E. coli S.
aureus
E. coli S.
aureus
E. coli
Methanol extract 13 12 7 7 5 3 2 2
Water extract 15 14 9 7 6 5 1 1
Microcapsules 7 8 7 6 5 5 5 3
Table 24. Perspiration fastness of samples treated with V. negundo extracts
Leaf extracts
Fabric samples treated with V. negundo extracts
Alkaline perspiration Acidic perspiration
Water extract 4/5 4
Methanol extract 4 3/4
Microencapsulated 5 4/5
83
Conclusion
 Acidic perspiration resulted in slight decrease in the fastness (antimicrobial
activity) of the samples compared to alkaline perspiration
 The extracts of Vitex negundo could be used for bactericidal and
bacteriostat applications on different textile materials
84
85

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Antibacterial finishes

  • 1. 1
  • 2. Antibacterial Finishes for Textiles using Herbal Sources by Shameembanu A. ByadgiShameembanu A. Byadgi 2
  • 3. 3 Introduction  The rapid growth in technical textiles and their end-uses has generated many opportunities for the application of innovative finishes  Novel finishes of high added value for apparel fabrics are also greatly appreciated by a more discerning and demanding consumer market  Antimicrobial textiles with improved functionality find a variety of applications such as health and hygiene products, specially the garments worn close to the skin and several medical applications, such as infection control and barrier material  Although, the synthetic antimicrobial agents are very effective against a range of microbes and give a durable effect on textiles, they are a cause of concern due to the associated side effects on humans and environment  There is a great demand for antimicrobial textiles based on eco- friendly agents which not only help to reduce effectively the ill effects associated due to microbial growth on textile material but also comply with statutory requirements imposed by regulating agencies
  • 4. 4 Antibacterial finish  The plant products comprise the major segment among all the natural antibacterial agents  Healing power of some of the plant materials has been used since ancient times  Relatively small percentage (1-10%) of these is used as food by both humans and other animal species  Plants produce secondary metabolites which serve as plant defense mechanisms against predation by microorganisms, insects and herbivores  Some compounds such as terpenoids give plants their odours; others (quinones and tannins) are responsible for plant pigment  Many compounds are responsible for plant flavour (terpenoid capsaicin from chilli peppers)
  • 5. 5 Necessity of Antibacterial Finishes 1. To avoid cross infection by pathogenic microorganisms 2. To control the infestation by microbes 3. To arrest metabolism in microbes in order to reduce the formation of odour 4. To safeguard the textile products from staining, discoloration and quality deterioration
  • 6. 6 Requirements for Antimicrobial Finish Durability to washing, dry cleaning and hot pressing; Selective activity to undesirable microorganisms; Should not produce harmful effects to the manufacturer, user and the environment; Should comply with the statutory requirements of regulating agencies; Compatibility with the chemical processes; Easy method of application; No deterioration of fabric quality; Resistant to body fluids; and Resistant to disinfections/sterilization
  • 7. 7 Natural antibacterial agents for textiles  Neem extract  Aloevera  Sericin  Chitosan  Tea tree  Tulsi leaves  Clove oil  Cinnamon  Pomegranate rind  Eucalyptus  Periwinkle  Henna leaves
  • 8. 8 Antibacterial finishing methodologies  Exhaust technique  Pad-dry-cure method  Coating technique  Spray technique  Microencapsulation  Nanoencapsulation
  • 9. 9 Methods for improving the durability of the finish 1. Solubilisation of the active substances in/on the fibre 2. Treating the fibre with resin or cross-linking agents 3. Micro encapsulation of the antimicrobial agents with the fibre matrix 4. Coating the fibre surface 5. Chemical modification of the fibre by covalent bond formation 6. Use of graft polymers, homo polymers and/or co-polymerization on to the fibre
  • 10. 10 Evaluation of Antibacterial Activity QualitativeQualitative QuantitativeQuantitative Bacterial reduction method (AATCC 100-2004) Bacterial reduction method (AATCC 100-2004) Parallel streak method (AATCC 147-2004) Parallel streak method (AATCC 147-2004) Agar diffusion plate test (ISO 20645) Agar diffusion plate test (ISO 20645)
  • 12. 12 Calculations and results  Examine the incubated plates for interruptions of growth along the streaks of inoculum beneath the specimen and for a clear zone of inhibition beyond the edge  The average width of zone of inhibition along a streak on either side of test specimen is calculated by W = T – D / 2 W = width of clear zone of inhibition (mm) T = total diameter of test specimen and clear zone (mm) D = diameter of test specimen (mm)
  • 13. 13 Antibacterial effect Growth Description Assessment No growth Zone of inhibition is seen Diffusible antibacterial activity No growth under the fabric No zone of inhibition Bacteriostatic antibacterial activity Growth under the fabric No inhibition zone Antibacterial activity is absent
  • 14. 14 Agar diffusion plate test (ISO 20645)
  • 15. 15 Calculations and results  Examine the incubated plates for absence or presence of bacterial growth in the contact zone between agar & specimen and inhibition zone around the specimen H = D – d / 2 H = width of inhibition zone (mm) D = total diameter of test specimen and inhibition zone (mm) d = diameter of test specimen (mm)  Examine the contact zones under the specimen for bacterial growth
  • 16. 16 Antibacterial effect Inhibition zone (mm) Mean value Growth Description Assessment > 1 None Inhibition exceeding 1 mm, no growth Good effect 1 - 0 None Inhibition zone up to 1mm, no growth 0 None No inhibition zone, no growth 0 Slight No inhibition zone, only some restricted colonies, growth nearly totally suppressed Limit of efficacy 0 Moderate No inhibition zone, compare to control growth reduced to half Insufficient effect 0 Heavy No inhibition zone, compare to the control no growth reduction or only slightly reduced growth
  • 18. 18 Calculations and results  Report bacterial counts as the number of bacteria per sample  Percent reduction of bacteria by the specimen treatment is calculated by R = [(B – A)/ B] x 100 R = percent reduction A = no. of bacteria recovered from inoculated treated test specimen swatches in the bottle incubated over desired contact B = no. of bacteria recovered from inoculated treated test specimen swatches in the bottle immediately after inoculation
  • 19. Antimicrobial activity of cotton fabric treated with Quercus infectoria extract Gupta and Laha, 2007 New Delhi, India Objective To study the antimicrobial properties of cotton fabric treated with QI extract against selected bacterial species that cause infections in hospitals and unpleasant odour on textiles 19
  • 20. Methodology Plain weave cotton fabric 107 g/m2 weight, 40 ends/cm and 35 picks/cm Application of QI extract Samples were rinsed with cold water, soaped with 0.5 g/L non-ionic detergent (Lissapol N) and dried MLR 1:30 at 60ºC and neutral pH Pretreatment with alum (1 & 5% owf) at 80ºC and later treated with QI for 45 mins Post mordanting of QI treated samples with copper sulphate (1 & 5% owf) 20
  • 21. 21 Scoured cotton was also treated with 0.5% (owf) Fabshield (commercial antimicrobial agent) at 50ºC and 4.5 pH for 20 min followed by curing at 130-135ºC Wash fastness (ISO II test) Wash durability for retention of antimicrobial finish after single and 5 launderings
  • 22. 22 Assessment of antibacterial activity Qualitative : Parallel streak method (AATCC 147-1993) Quantitative : Agar plate method (AATCC 100-1993) Microbial inhibition was determined by the reduction in number of colony forming units (CFU) Reduction in microbial colonies = B – A x 100 B where A = CFU/ml for treated sample after 24h incubation B = CFU/ml for untreated sample incubated under identical conditions
  • 23. Table 1. Effect of dye and mordant on antimicrobial activity of treated cotton fabric + = growth under fabric Nil = no growth under fabric Results and DiscussionResults and Discussion Cotton fabric Growth Zone of inhibition (mm) E. coli B. subtilis E. coli B. subtilis Control + + 0 0 Fabshield treated Nil Nil 0 0 Treated with QI Nil + 4.0 3.0 QI + 1% alum Nil + 1.0 0.5 QI + 5% alum Nil + 2.0 1.0 QI + 1% CuSO4 Nil Nil 1.5 0 QI + 5% CuSO4 Nil + 1.5 1.5 23
  • 24. Figure 1. Parallel streak test on cotton against S. aureus [(a) control and (b) sample treated with QI] Figure 2. Antimicrobial activity of cotton fabric treated with QI against E. coli Figure 3. Antimicrobial activity of cotton fabric treated with QI on B. subtilis 24 a b
  • 25. Table 2. Retention of antimicrobial activity by treated cotton after sample launderings Bacteria Cotton fabric After single laundering After 5 launderings Reduction in cfu % Activity retention (%) Reduction in cfu % Activity retention (%) B. subtilis Control Nil Nil Nil Nil Treated with QI 33 55 0 0 QI + 5% alum 83 99.1 75 89.6 QI + 1% CuSO4 84.1 100 83 99.6 E. coli Control Nil Nil Nil Nil Treated with QI 55.6 65.4 61.1 62 QI + 5% alum 30.2 84.4 27.1 75.6 QI + 1% CuSO4 50.6 75.1 56.0 77.4 25
  • 26.  12% QI extract (owf) was found to be effective concentration against selected microbes  The activity was greatly enhanced when 5% alum or 1% copper sulphate was used as a mordant  Studies on durability of the treatment showed that the QI treatment was not durable to washing and the antimicrobial activity was lost completely after 5 launderings  Mordanted samples showed 80-100% retention of activity even after 5 washes Conclusion 26
  • 27. Application of Prickly chaff (Achyranthes aspera Linn.) leaves as herbal antimicrobial finish for cotton fabric used in healthcare textiles Thilagavathi and Kannaian, 2008 Tamil Nadu, India Objective To utilize methanolic extract of prickly chaff leaves to develop microbial resistant cotton fabric for healthcare textiles 27
  • 28. Methodology 28 Extraction process Grinding of dried leaves into very small units Extracted of active constituents by methanolic extraction method and sonication Shade drying of prickly chaff leaves @ 38-40ºC till the moisture reduces to 14%
  • 29. Table 3. Box and Behnken method for optimization of process parameters Test No. Extract conc. (%) Temperature (ºC) Citric acid conc. (%) 1 3 40 8 2 7 40 8 3 3 60 8 4 7 60 8 5 3 50 7 6 7 50 7 7 3 50 9 8 7 50 9 9 5 40 7 10 5 60 7 11 5 40 9 12 5 60 9 13 5 50 8 14 5 50 8 15 5 50 8 29
  • 30. 30
  • 31. Results and DiscussionResults and Discussion Table 4. Antimicrobial efficacy of the treated samples based on Box and Behnken experiments Test No. Agar diffusion test Zone of inhibition (mm) Parallel streak test Zone of inhibition (mm) Challenge test Bacterial reduction (%) S. aureus E. coli S. aureus E. coli S. aureus E. coli 1 49 21 4.5 2.5 97.83 56.58 2 47 16 4.2 0 96.99 45.00 3 41 16 4.6 1.5 60.00 25.00 4 43 20 4.1 1.6 95.89 26.36 5 39 16 3.5 1.4 93.34 45.25 6 37 17 3.0 0 92.70 56.56 7 31 15 4.9 1.5 96.63 72.00 8 32 25 3.2 2.0 65.05 73.00 9 43 26 3.1 0 92.82 56.00 10 45 18 4.5 1.2 98.45 45.00 11 43 17 2.5 1.5 98.65 69.23 12 42 27 2.6 0 55.43 45.12 13 40 20 3.5 1.0 92.74 56.56 14 40 20 3.5 1.0 92.74 56.56 15 40 20 3.5 1.0 92.74 56.56 31
  • 32. Conclusion  The fabric samples treated with methanolic extract of prickly chaff leaves applied by pad-dry-cure method possessed better antimicrobial activity against Staphylococcus aureus and Escherichia coli  Hence, the treated cotton fabric can be used for healthcare textiles 32
  • 33. Experimental study on antimicrobial activity of cotton fabric treated with aloe gel extract from Aloe vera plant for controlling the Staphylococcus aureus (bacterium) Jothi, 2009 Ethiopia Objective To develop an ecofriendly natural herbal finish from A. vera extracts for various textile applications 33
  • 34. Methodology 34 Fabric Bleached cotton fabric with 28 ends/cm, 25 picks/cm, plain weave and 40 x 40 Ne count Chemicals Citric acid and methanol Aloe gel Antimicrobial agent [1, 2,3,4 and 5gpl]
  • 37. 37 Assessment of antibacterial activity Shake flask method (ATCC 6538) Bacterial reduction was determined by using the formula Reduction in microbial colonies = A – B x 100 A where A = Number of colonies before shaking B = Number of colonies after 1 hour shaking Hohenstein modified test method – challenge test The finished samples were washed using a standard detergent (2% owf) and sodium carbonate (1% owf) at 60°C. The antimicrobial activity was assessed after 50 washes
  • 38. Results and DiscussionResults and Discussion Figure 4. Antimicrobial efficiency of Aloe gel treated sample (Agar Diffusion Test) Figure 5. Antimicrobial activity of untreated sample 38
  • 39. Table 6. Quantitative analysis test results Sl. No. Bacteria Finishing agent conc. (gpl) %of bacteria reduction after treatment 1 Staphylococcus 1 97.00 2 97.90 3 98.10 4 98.40 5 99.10 95.5 96.0 96.5 97.0 97.5 98.0 98.5 99.0 99.5 54321 Finishing agent concentration (gpl) Figure 6. Antimicrobial efficiency of aloe gel treated sample against S. aureus (Shake flask Method) 39
  • 40. Table 7. Durability of antimicrobial effect of treated sample (5 gpl) after 50 washes Sl. No. Number of washes Antimicrobial effect (%) 1 10 99.70 2 20 99.30 3 30 99.10 4 40 98.40 5 50 98.00 40
  • 41. Conclusion  The specimens treated with the solution containing 5gpl aloe gel showed excellent antimicrobial activity  The treated sample showed high reduction rate in the number of colonies grown and a clear zone of bacteria inhibition  Finish durability to washing of antimicrobial property of the aloe gel treated sample was 98% after 50 washing  The finding of the study suggested that the treated fabrics can be used for textile application 41
  • 42. Dyeability and Antimicrobial Properties of Cotton Fabrics finished with Punica granatum extracts Rajendran et al., 2011 India Objective To investigate the antibacterial functionality of cotton fabric dyed using Punica granatum rind extract 42
  • 43. Methodology 43 Extraction process Aqueous extraction Ethanol extraction Add 10g P. granatum rind powder to 100ml distilled water Filtered through Whatmann No. 1 filter paper The filterate was stored at 4ºC Add 20g powder to 100 ml ethanol and kept @ room temperature for 48 hrs Filtered to obtain a clear filterate Filterate was condensed through a rotary vacuum evaporator @ 60ºC for 30 min
  • 44. 44 Assessment of antibacterial activity Qualitative : Disc diffusion method (SN 195920-1992) and parallel streak method (AATCC 147-2004) Quantitative : Percentage reduction method (AATCC 100-2004) % reduction = A - B x 100 B A = surviving cells (CFU/ml) for control (blank cotton fabric) B = surviving cells (CFU/ml) for test samples (natural dyed cotton fabric) Wash durability test AATCC-100 test 5% neutral soap for 20 mins 2, 4, 6, 8 & 10 launderings
  • 45. Table 8. Preliminary assessment of antimicrobial activity of natural dye Results and DiscussionResults and Discussion Sl. No. P. granatum extracts Antibacterial activity (Zone of inhibition in mm) E. coli S. aureus 1. Aqueous 8 14 2. Ethanol 10 17 45
  • 46. Qualitative antimicrobial assessment (a) (b) Figure 7. Agar diffusion method of (1) P. granatum treated fabric (2) Untreated sample against (a) E. coli and (b) S. aureus (a) (b) Figure 8. Parallel streak method of P. granatum treated fabric against (a) E. coli and (b) S. aureus 46
  • 47. Quantitative assessment Table 9. Antibacterial activity of treated fabric by percentage reduction test Test organisms Survival cells (CFU/ml) % bacterial reduction Control fabric Treated fabric Staphylococcus aureus 9.5 x 106 0.4 x 106 95.7 Escherichia coli 9.5 x 106 1 x 106 89.4 Wash durability Figure 9. Wash durability test 47
  • 48. Conclusion  The fabric dyed with P. granatum rind extracts displayed excellent antibacterial activity against both the test organisms  The results demonstrated that utilizing extracted natural colourants as dyeing materials significantly facilitate in obtaining quality fabrics having dyeability and antibacterial properties  The method of extraction and application of dyestuff from natural colourants may help to optimize the technical aspects of natural dyeing process 48
  • 49. Antibacterial efficacy analysis of Punica granatum L. leaf, rind and Terminalia chebula fruit extract treated cotton fabric against five most common human pathogenic bacteria Rathinamoorthy et al., 2011 Tamil Nadu, India Objective To develop an ecofriendly natural antimicrobial finish from plant extracts for textile application 49
  • 50. Methodology 50 Extraction process Fresh leaves & rind of Punica granatum L and Terminalia chebula fruits Shade dried and made into fine powder 10 gm of powder of each was soaked in methanol for 24 hours to obtain 10% concentrated solution The extracts were filtered
  • 52. Results and DiscussionResults and Discussion Table 10. Zone of inhibition of treated textile material for different strains (methanol extract) Sl. No. Bacteria Zone of inhibition (mm) Control P. granatum leaf extract P. granatum rind extract T. chebula fruit extract 1 Staphylococcus aureus - 30 28 38 2 Escherichia coli - 28 26 33 3 Klebsiella pneumonia - 26 25 36 4 Proteus vulgaris - 32 32 34 5 Salmonella typhi - 30 28 32 52
  • 53. Table 11. Zone of inhibition of treated textile material for different strains (water extract) Sl. No. Bacteria Zone of inhibition (mm) Control P. granatum leaf extract P. granatum rind extract T. chebula fruit extract 1 Staphylococcus aureus - 32 35 34 2 Escherichia coli - 31 34 32 3 Klebsiella pneumonia - 27 29 34 4 Proteus vulgaris - 38 34 34 5 Salmonella typhi - 30 33 32 53
  • 54. Table 12. Percentage of bacterial reduction by Hohensteins modified challenge test for methanol extract Bacterial strains Sample ‘0’ contact hour ‘24’ contact hour % reduction S. aureus P. granatum leaf 244 x 10-5 122 x 10-2 99.95 P. granatum rind 220 x 10-4 110 x 10-2 99.50 T. Chebula fruit 224 x 10-3 142 x 10-4 99.36 E. coli P. granatum leaf 136 x 10-4 124 x 10-3 90.88 P. granatum rind 140 x 10-3 121 x 10-3 85.00 T. Chebula fruit 104 x 10-3 196 x 10-2 98.11 54
  • 55. Table 13. Durability evaluation of treated samples by agar diffusion method Sources Bacterial strains 5 wash Inhibition zone (mm) 10 wash Inhibition zone (mm) P. granatum rind Staphylococcus aureus - - Escherichia coli 22 - Klebsiella pneumonia 26 24 Proteus vulgaris - - Salmonella typhi - - P. granatum leaf Staphylococcus aureus 22 - Escherichia coli 26 21 Klebsiella pneumonia - - Proteus vulgaris 24 - Salmonella typhi - - T. chebula fruit Staphylococcus aureus 28 25 Escherichia coli 24 24 Klebsiella pneumonia 36 26 Proteus vulgaris 26 24 Salmonella typhi - - 55
  • 56. Table 14. Durability test by quantitative measurement Bacterial strains Sample ‘0’ contact hr ‘24’ contact hr % reduction S. aureus P. granatum leaf Control - - No reduction 5 wash - - No reduction 10 wash - - No reduction P. granatum rind Control - - No reduction 5 wash - - No reduction 10 wash - - No reduction T. chebula Control - - No reduction 5 wash - - No reduction 10 wash - - No reduction E. coli P. granatum leaf Control - - No reduction 5 wash 272 x 10-5 128 x 10-5 52.94 10 wash - - No reduction P. granatum rind Control - - No reduction 5 wash 212 x 10-4 540 x 10-3 74.52 10 wash - - No reduction T. chebula Control - - No reduction 5 wash 160 x 10-3 230 x 10-2 85.62 10 wash - - No reduction 56
  • 57. Conclusion  Agar diffusion test indicated that both water and methanol extract treated textile material exhibited 27-38 mm of inhibition zone  Challenge test results indicated that both Punica granatum L leaf and rind extract treated samples had 99% of bacterial reduction against S. aureus  In case of E. coli, P. granatum L leaf treated sample showed 87% and the rind extract treated material showed 79% of bacterial reduction  T. chebula extract treated material showed higher percentage of reduction for both S. aureus (99.3%) and E. coli (98.1%)  The wash durability result indicated that, the effectiveness of the treatment reduced with the increase in washing cycle 57
  • 58. Effect of Laundering on Herbal Finish of Cotton Hooda et al., 2013 Haryana, India Objective To develop an eco-friendly herbal antimicrobial finish from Aloe vera leaves for textile application 58
  • 59. Methodology 59 Fabric 100 % cotton fabric (unbleached and unfinished); fabric count of 56 x 44 and GSM - 286 Chemicals Citric acid, acetic acid and methanol Preparation of Aloe vera extract Fresh mature green leaves of Aloe vera were collected, washed, weighed Hot air oven @ 40ºC Fine powder and weighed Extraction by maceration process using methanol Drying Grind
  • 60. 60 The sample was immersed in Aloe vera extract (3 & 5 g/l) for 30 minutes with MLR 1:20 Dried at 80ºC for 3 minutes and cured at 120ºC for 2 minutes on a lab model curing chamber Padded on a pneumatic padding mangle at a pressure of 2.5 psi, dried at 80°C and cured at 120 °C Application of antibacterial finish
  • 61. 61 Determination of Add-on (%) Add-on (%) = W2−W1 ×100 W1 W1:Weight of fabric before treatment (g) W2:Weight of fabric after treatment (g) Determination of Bacterial Population AATCC-100 test method Durability of Finish to Washing ISO: 6330-1984E using Launder-o-meter
  • 62. Results and DiscussionResults and Discussion Table 15. Weight add-on (%) of Aloe vera treatment on treated cotton fabric Application method Conc. (g/l) Weight per unit area of cotton g/m2 ) Aloe vera application Grey fabric Scoured fabric g/m2 % g/m2 % Pad-dry-cure method 3 309.66 6.17 308.33 6.64 5 320.66 9.94 318.66 10.21 C.D. 2.22 5.67 62
  • 63. Table 16. Bacterial reduction of Aloe vera treated grey and scoured cotton fabric by quantitative method Application method Conc. (g/l) Bacterial reduction in Aloe vera treated cotton fabric Grey fabric Scoured fabric 10-2 10-3 10-4 Mean (103 ) % reduction 10-2 10-3 10-4 Mean (103 ) % reduction Control Confluent lawn of growth Pad-dry-cure method 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69 5 >300 69 12 9.5 68.50 13 Nil Nil 4.3 96.70 63
  • 64. Table 17. Wash durability of finish in terms of bacterial reduction percentage of Aloe vera treated cotton fabric Method of application Bacterial reduction in Aloe vera treated cotton fabric (%) Pad-dry-cure method Grey fabric Scoured fabric Dilutions 10-2 10-3 10-4 Mean (103 ) % reduction 10-2 10-3 10-4 Mean (103 ) % reduction Wash cycles Conc. (g/l) Control Confluent lawn of growth 0 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69 5 >300 69 12 9.45 68.50 13 Nil Nil 4.3 96.70 5 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69 5 >300 69 12 9.45 68.50 13 Nil Nil 4.3 96.70 10 3 >300 98 19 14.4 52.00 19 Nil Nil 6.3 96.69 5 >300 69 12 9.45 68.50 13 Nil Nil 4.3 96.70 15 3 >300 103 22 16.15 46.17 24 Nil Nil 8.0 96.67 5 >300 75 17 12.25 59.17 15 Nil Nil 5.0 96.67 20 3 >300 111 35 23.05 23.17 29 2 2 83.0 71.38 5 >300 82 28 18.1 39.67 19 1 1 43.0 77.37 64
  • 65. Conclusion  Finished fabric showed very good antibacterial activity as compared to controlled fabric  Aloe vera treated scoured fabric exhibited excellent antimicrobial activity than Aloe vera treated grey fabric  Wash durability test also revealed that the finish was able to withstand upto 20 washes in case of Aloe vera treated scoured sample 65
  • 66. Antibacterial and Physical Properties of Knitted Cotton Fabrics Treated with Antibacterial Finishes Ureyen et al., 2010 Objective To investigate the effect of antibacterial application on physical properties of knitted fabric and the laundering durability of the applied agents 66
  • 67. Methodology 67 Turkish cotton knitted on circular knitting machine with a fabric weight of 170 g/m2 and subjected to scouring, bleaching, dyeing Table 22.Treatment Recipes Finishing process Recipe Exhausting process Bleaching + scouring 1 g/L wetting agent 1 g/L scouring agent 3 g/L NaOH 3 g/L H2O2 95°C for 25 min Neutralization with acid at 70°C Anti-peroxide at 40°C Reactive Dyeing 0.005% Remazol Yellow 3RS-A (C.I. Reactive Yellow 176) 0.0114% Remazol Red 3BS-A (C.I. Reactive Red 239) 20 g/L Sodium chloride 5 g/L Sodium carbonate 0.8 mL/L sequestering agent Neutralization with 0.5 mL/L Acetic acid Washing: 0.5 g/L soap Total time: 160 min
  • 68. 68 Antibacterial finishing Rapid P-A1 model laboratory vertical padder for impregnation and an Atac GK4 model laboratory stenter for curing Table 23.Notations and Concentrations of Antibacterial Agents Antibacterial agents Notation Type Concentrations A Organic antimicrobial agent (Triclosan) 60 g/L (pH 4-5) B Silver and TiO2 5 g/L (pH 5-6) C Quaternary ammonium salt (3-trimethoxysilylpropyldimethyloctadecyl ammonium chloride) 35 g/L (pH 6) D Silver compound 28.5 g/L (pH 4-5) Laundering BS ENISO 26330 standard using Wascator laundering machine with 4 g/L soap for 40 wash cycles
  • 69. 69 Table 24.Test Instruments and Standards Tests Instruments Standards Antibacterial - JIS-L 1902:2002 Fabric weight James Heal Circular Fabric Sample Cutter ISO 3801 Pilling James H. Heal Nu Martindale Abrasion and Pilling Tester ISO 12945-2 Air permeability Textest AG FX 3300 ISO 9237 Bursting strength James H. Heal TruBurst Tester ISO 13938-2 Colour efficiency Minolta CM 3600 d spectrophotometer -
  • 70. Results and DiscussionResults and Discussion Fig. 12. Mean values of fabric weight results (NW: Non-Washed, WC: Washing Cycles) 70
  • 71. Figure 13. Mean values of pilling test results (NW: Non-Washed, WC: Washing Cycles) 71
  • 72. Table 18. Mean values of air permeability test results Sl. No. Particulars Air permeability (L/m2 /s) Wash cycles 0 10 20 30 40 1 NW greige fabric 742.91 2 Agent A 553.75 1162.50 1254.55 1396.67 1443.33 3 Agent B 1039.56 1183.64 1192.73 1256.67 1151.67 4 Agent C 609.67 1253.55 1260.53 1343.33 1310.83 5 Agent D 940.18 1220.00 1256.33 1347.27 1241.87 72
  • 73. Table 19. Mean values of bursting strength test results Sl. No. Particulars Bursting strength (kPa) Wash cycles 0 10 20 30 40 1 NW greige fabric 749.86 2 Agent A 787.56 543.40 629.00 607.25 609.20 3 Agent B 590.48 564.84 626.25 586.60 621.32 4 Agent C 687.06 604.46 585.40 588.28 599.88 5 Agent D 616.06 558.16 590.54 558.68 610.14 73
  • 74. Table 20. Mean values of colour efficiency Sl. No. Particulars Colour efficiency (K/S) Wash cycles 0 10 20 30 40 1 NW greige fabric 0.154 2 Agent A 0.141 0.176 0.277 0.293 0.253 3 Agent B 0.141 0.213 0.232 0.256 0.236 4 Agent C 0.145 0.165 0.221 0.252 0.216 5 Agent D 0.161 0.213 0.223 0.249 0.239 74
  • 75. Table 21. Antibacterial activity of the treated samples Sl. No. Particulars Reduction in bacteria (CFU) Wash cycles 0 10 20 30 40 1 Agent A 3.70 2.91 3.60 3.63 3.05 2 Agent B 4.78 3.36 3.55 3.50 3.44 3 Agent C 2.26 1.91 1.35 0.32 0.68 4 Agent D 3.50 3.44 3.05 2.93 3.06 75
  • 76. Conclusion  The study concluded that fabrics shrunk due to the wet process of antibacterial treatments, causing a difference in the fabric weights  Due to the content of the antibacterial agents, pilling, air permeability and bursting strength of treated samples was lower than that of the untreated samples, except for the fabrics treated with agent A  Antibacterial finishing did not affect the colour efficiency of the dyed fabrics  Laundering affected the colour efficiency of the samples  Agent B gave the best antibacterial performance, while agent C gave the worst  The antibacterial activity of agents A, B, and D decreased slightly after several washings, while that of agent C decreased dramatically 76
  • 77. Antimicrobial efficiency of Vitex negundo leaf extracts Mohanraj et al., 2012 Sathyamangalam, India Objective  To study the antimicrobial effectiveness of Vitex negundo leaf extracts on cotton fabric treated by exhaustion and microencapsulation  To assess the durability of the finish against standard wash cycles and synthetic perspiration 77
  • 78. Methodology 78 Fresh nochi (V. negundo) leaves were collected and shade dried within a temperature range of 37-40ºC ground and sieved Nochi leaf powder (25g) was mixed with 250mL water, boiled for 30 min and filtered using nylon fabric 10g of nochi leaf powder was extracted in soxhlet apparatus with 150mL methanol for 24h Microencapsulation Nochi leaf extract as core material and acacia gum as wall material The microcapsules were freeze dried
  • 79. 79 Samples were treated with herbal extract using 8% citric acid as cross linking agent by pad-dry-cure method Padded through padding mangle and dried at 60ºC for 5 min Application of antibacterial finish Microencapsulation
  • 80. 80 Evaluation of fabrics Flexural rigidity ASTM D1388-96, using Shirley fabric stiffness tester Antimicrobial activity Agar diffusion method specified in AATCC TM 100 Wash durability Laundrometer at a speed of 40 rpm with ISO 3 test method Fastness to perspiration AATCC TM 15-2002
  • 81. Results and DiscussionResults and Discussion Table 22. Effect of finishing treatment on flexural rigidity of samples Samples treated with Flexural rigidity (mg cm) Methanol extract Warp 35.54 Weft 31.07 Water extract Warp 36.26 Weft 31.04 Microcapsules Warp 37.92 Weft 32.37 81
  • 82. (a) (b) (c) (d) Figure 11. Antimicrobial activity of samples treated with padding mangle (a – S. aureus & b – E. coli) and microcapsules (c – S. aureus & d – E. coli) 82
  • 83. Table 23. Effect of washing on antimicrobial efficacy of fabric samples Sample treatment Zero wash 5 wash 10 wash 15 wash S. aureus E. coli S. aureus E. coli S. aureus E. coli S. aureus E. coli Methanol extract 13 12 7 7 5 3 2 2 Water extract 15 14 9 7 6 5 1 1 Microcapsules 7 8 7 6 5 5 5 3 Table 24. Perspiration fastness of samples treated with V. negundo extracts Leaf extracts Fabric samples treated with V. negundo extracts Alkaline perspiration Acidic perspiration Water extract 4/5 4 Methanol extract 4 3/4 Microencapsulated 5 4/5 83
  • 84. Conclusion  Acidic perspiration resulted in slight decrease in the fastness (antimicrobial activity) of the samples compared to alkaline perspiration  The extracts of Vitex negundo could be used for bactericidal and bacteriostat applications on different textile materials 84
  • 85. 85