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Textile Science and Clothing Technology

Subramanian Senthilkannan Muthu

Editor

Textiles and
Clothing
Sustainability
Nanotextiles and Sustainability
Textile Science and Clothing Technology

Series editor
Subramanian Senthilkannan Muthu, SGS Hong Kong Limited, Hong Kong,
Hong Kong
More information about this series at http://www.springer.com/series/13111
Subramanian Senthilkannan Muthu
Editor

Textiles and Clothing

Sustainability
Nanotextiles and Sustainability

123
Editor
Subramanian Senthilkannan Muthu
Environmental Services Manager-Asia
SGS Hong Kong Limited
Hong Kong
Hong Kong

ISSN 2197-9863 ISSN 2197-9871 (electronic)

Textile Science and Clothing Technology
ISBN 978-981-10-2187-9 ISBN 978-981-10-2188-6 (eBook)
DOI 10.1007/978-981-10-2188-6

Library of Congress Control Number: 2016946934

© Springer Science+Business Media Singapore 2017

This work is subject to copyright. All rights are reserved by the Publisher, whether the whole or part
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The use of general descriptive names, registered names, trademarks, service marks, etc. in this
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The publisher, the authors and the editors are safe to assume that the advice and information in this
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Printed on acid-free paper

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The registered company is Springer Science+Business Media Singapore Pte Ltd.
Contents

Advances in Nanotextile Finishes—An Approach Towards

Sustainability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
N. Gokarneshan, P.T. Chandrasekar and L. Suvitha
Nanochemicals and Effluent Treatment in Textile Industries. . . . . . . . . . 57
P. Senthil Kumar, Abishek S. Narayan and Abhishek Dutta
Insights into the Functional Finishing of Textile Materials
Using Nanotechnology. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
Shahid-ul-Islam, Mohd Shabbir and Faqeer Mohammad

v
Advances in Nanotextile Finishes—An
Approach Towards Sustainability

N. Gokarneshan, P.T. Chandrasekar and L. Suvitha

Abstract The chapter critically surveys the recent development trends in nan-
otextile finishes. Garments for special needs comprising of the functional aspects
such as protective, medical treatment and care, have been considered through
treatment with silver nanoparticles and have been related to sustainability. The
micro- and nanoencapsulation of 100 % cotton denim fabric using three herbal
extracts have been studied for antimicrobial efficiency, resulting in improvement in
durability and good resistance to microbes over 30 industrial washes. The synthesis,
characterization, and application of nanochitosan on cotton fabric has been studied,
and the treated fabrics were evaluated for appearance, tensile, absorbency, stiffness,
dyeing behaviour, wrinkle recovery, and antibacterial properties. Polyester fabric
has been treated with nanosized dispersed dye particles without carrier, using
ultrasound. This has been used for optimizing the parameters for the preparation of
the printing paste. Attempt has been made to improve the handle property of jute
polyester-blended yarn to produce union fabric with cotton yarn, intended for
winter garment. The findings indicate that nano–micropolysiloxane-based finishing
exhibit better improvement in the surface morphology, handling, and recovery
property of the fabric as compared with other finishing combinations. Viscose
fabrics have been modified to improve the attraction for metal oxides such as
aluminium, zinc, or titanium in order to impart antimicrobial activity against two
types of microorganisms. Nanosafe textile using the extracts of yellow papaya peel
has been developed by extracellular synthesis of highly stable silver nanoparticles.
Cotton fabrics with smart properties have been developed by functional finishing
with stimuli-responsive nanogel using a combination of biopolymer and synthetic

N. Gokarneshan (&)
P.T. Chandrasekar
L. Suvitha

Department of Textile Technology, Park College of Engineering and Technology,
Coimbatore, Tamil Nadu, India
e-mail: [email protected]

© Springer Science+Business Media Singapore 2017 1

S.S. Muthu (ed.), Textiles and Clothing Sustainability,
Textile Science and Clothing Technology,
DOI 10.1007/978-981-10-2188-6_1
2 N. Gokarneshan et al.

polymer in the synthesis of nanogel. The findings reveal that the application of
nanogel as a smart finishing system affects the intrinsic cotton properties and also
improves the common textile quality by providing new features of stimuli
responsiveness. Above all these, the newer concepts of the nanotextile finishes
discussed in the chapter promise enhancement in the existing properties of textile
materials, increase durability, promote ecofriendliness and economy, and thus pave
the way towards achieving better sustainability.

Keywords Chitosan Disperse dye Viscose

Nanogel
Silver particles



Nanoencapsulation Nanopolysiloxane

1 Introduction

The new millennium has witnessed significant research works around the globe in the
area of nanotextile finishing (Gokarneshan et al. 2013). A number of innovative
approaches have been attempted during the recent years and tend to exploit the
functional properties and tailor the fabrics to suit specific requirements. Some of the
efforts have been directed towards improvement in antibacterial efficacy of the fabrics
so treated (Gokarneshan et al. 2012). When considering garments for special needs,
three aspects have been considered, namely, protective, treatment, and caring. Efforts
have been directed to improve the comfort and functionality of these groups clothing
with nanotechnology by assessing all of these concerns and comparing the benefits of
nanotechnology with its disadvantages (Ebrahim and Mansour 2013). Application of
antimicrobial finishes using natural materials has been the popular trend, which
promotes natural and ecofriendly lifestyle. Attempt has been made through the use of
plant extracts containing active substances on fabrics, so as to maker them microbial
resistant (Sumithra and Vasugi Raaja 2012). The textile wet processing operations are
going through a stage of green revolution, wherein many types of conventional and
non-eco-friendly chemicals are being replaced by natural-based products that are safe
to environment and health during manufacturing and usage. The synthesis and
characterization of nanochitosan on cotton fabric has been studied. The
nanochitosan-treated fabrics are then tested for appearance, tensile, absorbency,
stiffness, dyeing behaviour, wrinkle recovery, and antibacterial properties
(Chattopadhyay and Inamdar 2013). In an interesting study, a nanoparticle-sized
disperse dye treated with ultrasound has been applied on polyester fabric without
using a carrier. The dyeing and process parameters considered include K/S values,
dye particle size, dye exposure to ultrasound waves, printing paste pH, steaming
conditions of prints, morphological study using SEM and TEM of dye particles, and
fastness properties of the prints (Osman and Khairy 2013). Even though jute fibre has
unique properties such as roughness, coarseness, and stiffness, it can cause problems
during fabric formation and performance of final product as well, rendering it
unsuitable for apparel. Hence efforts have been taken to improve the handle property
of jute fabric through application of nanopolysiloxane-based finishing both in
Advances in Nanotextile Finishes—An Approach Towards Sustainability 3

individual as well as in combination with other finishing chemicals by conventional

pad-dry-cure method (Lakshmanan et al. 2014). Textile fabrics are generally sub-
jected to repeated laundering during their lifetime, and hence the washing durability
of nanometal-treated fabric is of significant importance. In this context, attempt has
been made to prepare permanent antimicrobial viscose fabrics by fixation of propi-
onic acid groups at lower temperature (below 100 °C), as active centres, onto the
cellulosic polymeric chain. The added carboxylic groups are believed to act as
favourable centres for some oxides such as titanium oxide, zinc oxide, or aluminium
oxide nanoparticles. The efficiency of the antimicrobial activity, considering the
permanent performance against selected microorganisms onto modified textile, has
also been evaluated (El-Sayeed et al. 2015). Cotton fabrics have been functionally
finished with stimuli-responsive nanogel comprising of biopolymer chitosan and a
synthetic polymer so as to obtain smart properties (Bashari et al. 2015). The above
approaches enable a more effective way of nanofinishing of textile materials and hold
the prospects of greater viability coupled with sustainability, since they address the
concerns related to the field of application of nanotechnology in textiles. The chapter
focuses on the advantages of the newer methods of nanotextile finishing which hold
the prospects of wider areas of applications.

2 Treatment of Nanomaterials on Garments

for Special Needs

2.1 Overview

The mechanical and physical properties of cotton fabrics can be modified to meet
special needs garments, by application of nanosilver finishes. Accordingly fabrics
have been subjected to the nanosilver finishing process with 5 different solution
concentrations of 100, 200, 300, 400 and 500 ppm. It has been found that
nanosilver finishing minimized the air and water vapour permeability of the fabric,
which could be due to the nanosilver particles that fill the fabric pores. The wrinkle
recovery angle of the nanofinished fabrics has decreased in both directions due to
the generation of links on the fabric by nanosilver particles (Ebrahim and
Mansour 2013). Yarn swelling phenomena happens during the finishing process in
cotton fabrics which means increment of occupied space by fibres and yarns and
thus rise in the fabric thickness; owing to integration of fibres and yarns by the
nanosilver particles, the breaking elongations of fabrics in both warp and weft
directions were inclined to applying the nanosilver finishing process, and applying
the nanosilver finishing process led to formation of links on the fabric, and con-
sequently bending rigidity of the fabrics was increased in both warp and weft
directions. Finally, it has been observed that there has been a decrease in most of the
physical and chemical properties of cotton fabrics by increasing the concentration
of the solution to 500 ppm.
4 N. Gokarneshan et al.

2.2 Related Aspects

Despite the fact that the application of nanoparticles to textile materials is gaining
popularity owing to their novel physicochemical properties and their potential
applications, some of them are toxic or ineffective and renders them unsuitable for
applications in medicine, filters, and textiles and for the exclusion of pollution. To
quote some examples
(a) Improving the water-repellent property of the fabric by creating nanowhiskers
(hydrocarbons which are 1/1000 size of typical cotton fibres) on the fabric
(b) Creating antistatic properties of textile which can be provided by TiO2, ZnO,
antimony-doped tin oxide (ATO), and silane nanosol, increasing the surface
energy and thereby providing a very high particle retention to filters by the
usage of nanofibrous webs on them
(c) Using nanotitanium dioxide and nanosilica to advance the wrinkle resistance
of cotton and silk respectively, employing nanosized TiO2 and ZnO in order to
absorb and scatter UV radiation more effectively regarding the larger surface
area and blocking ability of so-called particles
(d) Covering the cotton fibres in a fuzz of minute whiskers and creating fewer
points of contact of dirt, thus the fabric has been rendered super-hydrophobic,
and the self-cleaning property can be developed in this way.
Eventually, antibacterial properties can be imparted by using nanosized silver,
titanium dioxide, and zinc oxide (Wong et al. 2006a; Anna et al. 2007; Parthasarathi
2008). The nanosilver particles are given a greater focus, as they have an extremely
large relative surface area, and so their contact with bacteria or fungi is increased,
thereby resulting in great improvement in their bactericidal and fungicidal
effectiveness.
Cotton is generally used in the production of textiles for sport and leisure
activities owing to its outstanding moisture absorption ability. Since cotton is moist,
it is susceptible to bacterial attack. There is a characteristic odour in decomposed
products of body secretions (Gorensek and Recel 2007). In recent research, a good
antibacterial effect of nanosized silver colloidal solution on polymer and textile
fabrics was shown (Lee and Jeong 2005; Yeo et al. 2003). It has been intended to
not only study the synthesis of silver nanoparticles used in microwave radiation as a
heating source but also investigate the role of nanotechnology in improving sus-
tainability cotton fabrics and the relationship between the physical and mechanical
properties and the content of nanosized silver on cotton fabric. Generally, this
utilization can be categorized into two main areas: firstly, application of nanofibres
and, secondly, application of nanoparticles in different domains. Here some of these
applications can be named. Some examples are the use of polymeric nanofibres and
their composites in drug delivery systems, tissue engineering, reinforcement of
some composites, transistors, capacitors, and so on (Hatiboglu 2006; Huanga et al.
2003; Tan and Lim 2006).
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Advances in Nanotextile Finishes—An Approach Towards Sustainability 5

2.3 Technical Details

100 % plain woven cotton fabrics have been used. For investigating the influence of
nanosilver finishes on the physical and mechanical properties of the fabric, six
different fabrics have been tested (Ebrahim and Mansour 2013). Finished fabrics
have been compared with unfinished fabrics. The finishing has been done with five
different solution concentrations, so as to identify a trend in changes. Fabrics have
been soaked in 50 °C suspensions with five distinct concentrations of nanosilver
particles for 30 min and then dried in the open air (known as ‘exhausting finish-
ing’). The physical and mechanical properties including air permeability (A.P),
wrinkle recovery (W.R), water vapour permeability (W.V.P), thickness (T),
breaking strength (B.S), breaking elongation (B.E), and bending rigidity (B.R) have
been measured as a testing procedure (Ansari and Maleki 2007).

3 Physical and Mechanical Properties

3.1 Air Permeability

The test results of air permeability are shown in Fig. 1. A severe drop in the air
permeability property can be clearly observed by applying nanosilver finish on the
fabric, and also a gradual fall by increasing the solution concentration (Ebrahim and
Mansour 2013) is observed. This occurs due to the reduced fabric pores, which have
been padded by nanosilver particles. As the nanoparticles are very small, increasing
the concentration does not significantly influence the air permeability property.

3.2 Wrinkle Recovery

The test results of wrinkle recovery in the warp and weft directions are depicted in
Figs. 2 and 3. There is a high angle of recovery in the warp direction in sample A,

Fig. 1 Air permeability of fabrics (Ebrahim and Mansour 2013)

6 N. Gokarneshan et al.

Fig. 2 Wrinkle recovery

angle of fabrics in weft
direction (Ebrahim and
Mansour 2013)

Fig. 3 Wrinkle recovery

angle of fabrics in warp
direction (Ebrahim and
Mansour 2013)

and it goes down gradually in sample E and then rises again in the sample F.
A downward trend in wrinkle recovery is observed due to the links which have been
created by nanosilver particles on the fabric, but the created links decrease upon
increasing solution concentration to 500 ppm. In the case of Fabric A, the recovery
angle in the weft direction is high, and there has been a moderate drop in this value
for the other samples. However, no regular trend is seen, and it is due to the
unevenness in finishing (Ebrahim and Mansour 2013).

3.3 Water Vapour Permeability (WVP)

The water vapour permeability percentage of the fabrics is depicted in Fig. 4. It can
be generally concluded that WVP% of nanofinished fabrics are lower than the
unfinished one. The explanation relating to air permeability holds valid in this case
too. The highest value of WVP% is found in Fabric A, while the lowest is in
Fabric F. The irregularity arises due to the unevenness of finishing process
(Ebrahim and Mansour 2013).

Fig. 4 Water vapour permeability of fabrics (Ebrahim and Mansour 2013)

Advances in Nanotextile Finishes—An Approach Towards Sustainability 7

Fig. 5 Thickness of fabrics (Ebrahim and Mansour 2013)

3.4 Thickness

Figure 5 depicts the thickness values of the fabrics. It is evident that the thickness
values of nanofinished fabrics are more than those of the unfinished fabric. The
higher thickness values of the nanofinished fabrics are due to the yarn swelling
phenomena that occur during the finishing process (Ebrahim and Mansour 2013).
However, increasing solution concentration to 500 ppm resulted in a severe fall,
which occurs due to decreasing of yarn swelling.

4 Influence of Nanosilver Finish on Mechanical Properties

4.1 Breaking Strength

Figure 6 shows the breaking strength of the fabrics in the warp direction. The
lowest breaking strength has been exhibited by Fabric F and the highest by
Fabric C. The general trend seen is that the breaking strength of nanofinished
fabrics is more than unfinished fabric due to the linkage formation between fibres
and yarns. However, the exact trend is not predictable. The breaking strength of the
fabrics in the weft direction is shown in Fig. 7 (Ebrahim and Mansour 2013).
Fabric D exhibits the highest breaking strength. However, there is no significant
difference between other fabrics.

4.2 Breaking Elongation

Figures 8 and 9 typify the breaking elongations of the fabrics in both warp and weft
directions. Significant differences can be seen in the breaking elongation of fabrics
between nanofinished and unfinished fabrics. The necessary difference arises due to
consolidation of fibres and yarns by the nanosilver particles (Ebrahim and Mansour
2013).
8 N. Gokarneshan et al.

Fig. 6 Breaking strength of

fabrics in weft direction
(Ebrahim and Mansour 2013)

Fig. 7 Breaking strength of

fabrics in warp direction
(Ebrahim and Mansour 2013)

Fig. 8 Breaking elongation

of fabrics in warp direction
(Ebrahim and Mansour 2013)

Fig. 9 Breaking elongation

of fabrics in weft direction
(Ebrahim and Mansour 2013)

4.3 Bending Rigidity

Figures 10 and 11 show the bending rigidity values of fabrics in the warp and weft
directions, respectively. Fabric A has bending rigidity of 71.2 (mgr cm) in the warp
direction and 72.5 (mgr cm) in the weft direction. In the case of Fabric E the bending
rigidity values started to increase, and they reached to 126 (mgr cm) in the warp
direction and 124 (mgr cm) in the weft direction (Ebrahim and Mansour 2013). This
gradual upward trend is caused by the links which was formed on the yarns and
Advances in Nanotextile Finishes—An Approach Towards Sustainability 9

Fig. 10 Bending rigidity of

fabrics in warp direction
(Ebrahim and Mansour 2013)

Fig. 11 Bending rigidity of

fabrics in weft direction
(Ebrahim and Mansour 2013)

fabrics by nanosilver finishing. In the case of Fabric F, an increase in solution

concentration to 500 ppm leads to a gradual fall, owing to decreasing form of links.

5 Micro- and Nanoencapsulation of Denim Fabrics

5.1 Overview

The use of herbal extracts (Ricinus communis, Senna auriculata and Euphorbia
hirta) holds good prospects as antimicrobial finishing on denim fabric. The finished
fabric exhibits maximum antibacterial activity against both Escherichia coli and
Staphylococcus aureus. The microencapsulation and nanoencapsulation techniques
increase the durability of the herbal finishing. The findings reveal antimicrobial
effect even for the washed fabrics against the standard strains (Sumithra and Vasugi
Raaja 2012).

5.2 Related Aspects

It is a well known fact that bacteria can grow and survive on fabrics commonly used
in healthcare environments for more than 90 days and hence contribute to the
transmission of diseases (Gaurav 2005; Subhash and Sarkar Ajoy 2010). The recent
trend has been the use of antimicrobial finishes using natural sources, which pro-
motes natural and ecofriendly lifestyle (Natarajan 2002). Attempt has been made
through application of plant extracts containing active substances, so as to explore
10 N. Gokarneshan et al.

the possibility of making the cloth microbial resistant (Sumithra and Vasugi Raaja
2012). These natural antimicrobial substances are not only ecofriendly but are also
taken from renewable sources (Gaurav 2005). Bacterial growth in textile materials
leads to the deterioration of fabric properties and produces foul smells, skins irri-
tation, and cross-infections (Subhash and Sarkar Ajoy 2010). Microbes are small
organisms that cannot be seen by the naked eye and include a variety of
microorganisms such as bacteria, algae, and fungi (Natarajan 2002). Encapsulation
involves covering small solid, liquid, or gaseous substrates by means of a polymeric
or inorganic shell. The resulting capsules or particles normally range from
micrometres to millimetres in size (Holme 2002).
The microencapsulation has multivaried applications that include controlled
release of the active components, particle coating, flavour stabilization, taste
masking, physical/chemical stabilization, improvement in shelf life, and prevention
of exposure of the active material to the surroundings (Bhoomika et al. 2007). Two
common technologies can be used to obtain such nanocapsules and microcapsules,
namely the interfacial polymerization of a monomer and the interfacial deposition
of a preformed polymer (Shilpa 2004). Denim has become very popular due to its
suitability for many occasions rather than merely complementing a rugged style,
and is also used irrespective of demographic differences (Srikanth 2010). The
durability of denim as only the warp yarns go through the dyeing process, while the
weft yarn is left natural without undergoing any chemical process. This is the
advantage of yarn-dyed fabric over piece-dyed fabric (Thies 2005). The denim wear
is gaining importance tremendously each year and has also increased its worldwide
market share unpredictably during the past few decades. The consumer needs have
been focussed towards the latest developments and new styles, and also there is
increased awareness of special finishes and process treatments given to the garment
to make them ecofriendly and user-friendly. The discussion herein focuses on
screening for the antimicrobial activity of the natural herbs and providing the denim
fabric with the antimicrobial finish from the screened herbal extracts. AATCC
methods are followed relating to the combinations and conditions.
Microencapsulation and nanoencapsulation methods have been used to increase the
washing durability of the antimicrobial finish provided from the herbal extracts.

5.3 Technical Details

For the application of antimicrobial finish, 100 % cotton denim fabric has been
used. The antimicrobial extract has been obtained using the herbs R. communis
(leaves), S. auriculata (leaves), and E. hirta (leaves, stem and flower). The collected
plants have been dried at a temperature range of 100–140 °C, as they cannot be
stored without drying, thereby preventing the breakdown of important compounds
and contamination by microorganisms (Sumithra and Vasugi Raaja 2012). The
fabric has been primarily washed with distilled water, air-dried, and then used for
herbal finishing. Dip technique has been used to finish the fabric with herbal extract.
Advances in Nanotextile Finishes—An Approach Towards Sustainability 11

The fabric has been immersed in the extract for 30 min, air-dried, and then used for
the antibacterial assessment using standard bacterial strains. The AATCC test
method has been used, and the herbal extracts having antibacterial activity have
been mixed during preliminary screening, in various combinations and conditions
used for their combined antibacterial property. The denim fabric with herbal extract
having the diameter of 23 mm was placed on the surface of medium and the plates
were kept for incubation at 37 °C for 24 h. The zone of inhibition formed around
the fabric during the end of incubation has been measured in mm and recorded.
Addition of sodium alginate with subsequent spraying into the calcium chloride
solution by sprayer resulted in formation of microcapsules containing herbal
extract. In order to harden the capsules, the droplets have been retained in the
calcium chloride solution for 15 min. The microcapsules were obtained by
decantation and followed by repeated washing with isopropyl alcohol and then
drying at 45 °C for 12 h. The microcapsules were applied on the fabric by
exhaustion method using 8 % citric acid (cross-linking agent). The fabric was kept
immersed in the solution (ML ratio 1:20) for 30 min at 50 °C in water bath. After
finishing, the fabric was removed, squeezed, and dried at 80 °C in the oven for
5 min and then cured at 120 °C for 2 min. The antibacterial activity of the
microcapsule-finished fabric was analysed by AATCC test method. The herbal
extracts prepared were encapsulated using bovine albumin fraction as the wall
material and the nanoparticles as the core material. The herbal extract-enclosed
bovine serum albumin protein was prepared by coacervation process followed by
cross-linking with glutaraldehyde. After glutaraldehyde treatment, for purification
the solution is put in rotary vacuum evaporator to remove the organic solvent, then
centrifuged at 4 °C at 10,000 rpm, suspended in 0.1 M phosphate buffer (pH 7.4),
and then lyophilized with mannitol (2 % w/v). The herbal extract was incubated
with the required protein solution (2 % w/v) for an hour at room temperature. The
pH of the solution was adjusted to 5.5 by IMHCL using digital pH meter. Then
ethanol was added to the solution in the ratio of 2:1 (v/v). The rate of ethanol
addition was carefully controlled at 1 mL per min. The coacervate so formed was
hardened with 25 % glutaraldehyde for 2 h to allow cross-linking of protein.
Organic solvents were then removed under reduced pressure by rotary vacuum
evaporator, and the resulting nanocapsules were purified by centrifugation
(10,000 rpm) at 4 °C. Pellets of nanocapsules thus obtained were then suspended in
phosphate buffer (pH 7.4; 0.1 M), and each sample was finally lyophilized with
mannitol (2 % w/v). The nanocapsules obtained were further dried by lyophiliza-
tion and then applied on the cotton fabric by exhaustion method using 8 % citric
acid as binder. The fabric was finished following the conditions M/L ratio 1:20,
binder (citric acid) 8 %, temperature 55 °C, and time 30 min. The AATCC test
method has been used to evaluate the antibacterial activity of the
nanocapsule-finished fabric. The denim fabric finished with microcapsules and
nanocapsules have been assessed for their wash durability and antibacterial activity
evaluated. The binding of microcapsules and alignment on to the fabric have been
confirmed by scanning electron microscopy.
12 N. Gokarneshan et al.

6 Determination of Antibacterial Activity of Finished

Fabric

The antibacterial activity has been evaluated for the finished fabric using AATCC test
method against E. coli and S. aureus. The zone of inhibition for the fabrics finished
with methanolic extract of R. communis, S. auriculata, and E. hirta is 0 (no bacterial
growth), 25, and 24 mm, respectively, for E. coli and 27, 30, and 29 mm, respec-
tively, for S. aureus. The methanolic extract of the herbs is able to impart antibacterial
efficacy to the finished fabric. Among the three herbs used, the methanolic extract of
S. auriculata is found to give maximum antibacterial activity in comparison with the
other two. The selected ratio of 1:3:2 of R. communis, S. auriculata, and E. hirta,
respectively, is found to be the best combination. The fabric so treated is found to be
strongly resistant to both Gram-positive and Gram-negative microorganisms. The
bacterial growth is prevented by the treated fabrics. The values of the inhibition zone
show that the herbal extracts prevent the bacterial growth under the fabric and also
leaches out and kills the bacteria. In the case of E. coli, the bacterial growth rate is
2.7 × 109 cfu/mL, and for S. aureus, it is 2.4 × 109 cfu/mL.
Antibacterial activity of ajwain seeds extract treated fabrics using qualitative and
quantitative methods has also been reported (Benita 1996). Antibacterial property
of extract alone clearly shows extended zone of inhibition (20–30 mm) for both
types of microorganism (Gram positive and Gram negative) when analysed by
AATCC (parallel streak method). Test results show that all treated fabrics have very
good antimicrobial property to both S. aureus and Klebsiella pneumoniae
microorganisms. The treated fabrics do not allow the growth of bacteria under the
test specimen. In all the cases, there is a good zone of inhibition ranging from 11.9
to 14.5 mm for S. aureus and from 6.9 to 7.1 mm for K. pneumoniae. It has been
shown that the extracts from basil, clove, guava, jambolan, lemon balm, pome-
granate, rosemary, and thyme exhibit antimicrobial activity to at least one of the
tested microorganisms (Barari et al. 2009). The highest activities are seen in the
extracts of clove and jambolan. In other words they are able to inhibit 9 (64.2 %)
and 8 (57.1 %) kinds of microorganisms of interest, respectively.

6.1 Microencapsulation of Herbal Extract

The effective herbal combination is microencapsulated using ionic gelatin technique

so as to increase the durability of the finished fabric. The antibacterial activity of the
finished fabric and the fabric after washes have been tested and the results are
presented in Table 1. It has been found that the microcapsules of the herbal
extract-finished denim fabric exhibit activity for the sample after 20 washes. They
exhibit potential for antimicrobial activity against S. aureus and E. coli. It is
observed that the microencapsulated herbal extracts possess a very good resistance
for microbes even after 15 washes. The antimicrobial efficiency has been defined in
Advances in Nanotextile Finishes—An Approach Towards Sustainability 13

Table 1 Antibacterial activity of the microcapsules and nanocapsule-finished fabrics (Sumithra

and Vasugi Raaja 2012)
Samples Zone of bacteriostasis Zone of inhibition
(mm) (mm)
Microcapsule Nanocapsule
E. coli S. aureus E. coli S. aureus
Finished fabric 24 33 30 35
Finished fabric after10 washes 0 30 29 33
Finished fabric after 20 washes 0 27 28 30
Finished fabric after 30 washes 0 0 28 25

terms of bacterial reduction percentage for directly applied and herbal microcap-
sules applied fabrics (Sanjay Vishwakarma et al. 2010). The herbal extracts applied
both directly and microencapsulated show better activity against S. aureus than
against E. coli.
Fabrics on which herbal extract has been directly applied do not exhibit much
activity after 10 washes, since the extracts are coated only on the surface without
any firm bonding and get removed by washing. This was ascertained when the
structure of microcapsules was studied by scanning electron microscopy using
image analysis technique. The antimicrobial efficacy by quantitative method in
terms of bacterial reduction and the wash durability of antimicrobial activity was
studied by agar diffusion method (AATCC 124). The fabrics show potential for
antimicrobial activity against S. aureus and E. coli. The microencapsulated herbal
extracts are highly resistant to microbes even after 15 washes. Hence, the herbal
extracts are nanoencapsulated so as to increase the durability of the fabric.

6.2 Nanoencapsulation of Herbal Extract

The exhaustion method has been used to apply the nanocapsules of the herbal
extracts on the denim fabric, and the antibacterial activity was evaluated for the
finished fabric and for the fabrics after washes (Table 1; Fig. 12). The results reveal
that the fabric finished with nanocapsules of herbal extracts is able to retain the

Fig. 12 Zones of inhibition of nanoencapsulated denim fabrics a for E. coli, b for S. aureus, c for
E. Coli after 10, 20 and 30 washes, and d for S. Aureus after 10, 20 and 30 washes (Sumithra and
Vasugi Raaja 2012)
14 N. Gokarneshan et al.

antimicrobial activity even after 40 industrial washes, hence providing long-term

durability to the finished fabric. Nanosized silver, titanium dioxide, and zinc oxide
have been used for imparting antibacterial properties (Pujari et al. 2010). The effect
of TiO2 nanoparticles concentration with and without using 4 % PUA binder on
antimicrobials on either screen printed or pigment-dyed silk fabric shows that the
use of PUA binder alone has no effect on the antimicrobial property. But upon
using TiO2 in either printing paste or in ink preparation, good results are observed
against E. coli and S. aureus. Moreover, printing yielded better results than obtained
in the case of dyeing.

6.3 SEM Investigation

Figures 13 and 14 depict the SEM images at various magnification levels of

nanocapsule-finished fabric and the fabrics after 10, 20, and 30 washes. It is clear
that the nanocapsules not only adhere on the surface, but also penetrate into the
interstices of the yarn and fabric. It shows that the nanocapsules are bonded well to
the fabric surface even after 30 washes.

7 Application of Synthesized Nanochitosan on Cotton

7.1 Overview

For the preparation of nanochitosan dispersion, ionotropic gelation with penta-

sodium tripolyphosphate has been used (Chattopadhyay and Inamdar 2013). The
following findings accrue with regard to application of nanochitosan on cotton fabric
(a) Nanochitosan-treated cotton fabric shows reasonably good appearance and
handle.
(b) There is improvement in fibre strength, which increases with the decrease in
particle size of nanochitosan.
(c) There is slight reduction in elongation-to-break with the scaling down of
particle size.
(d) Moisture-related property such as absorbency is affected; nevertheless, it is in
acceptable limit of tolerance.
(e) The dyeability of chitosan and nanochitosan-treated cotton fabric towards
direct dyes is improved significantly. The progress is sustained with reduction
in particle size. The effect is further enhanced after acidification of dye bath.
Fastness to washing is improved satisfactorily and fastness to rubbing slightly.
(f) Wrinkle recovery property is slightly improved and use of suitable
cross-linking agent is essential.
(g) Improved antibacterial activity is observed in combined treatment of
nanochitosan with nanosilver.
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Advances in Nanotextile Finishes—An Approach Towards Sustainability 15

Fig. 13 SEM photographs of nanocapsules finished fabrics under different magnifications

a ×250, b ×500, c ×1000 and d ×3000 (Sumithra and Vasugi Raaja 2012)

7.2 Related Aspects

The green technology is being given due attention for different wet processing
operations of textiles from initial preparatory processes to final finished fabrics.
Natural-based products are replacing many conventional non-ecofriendly chemicals
and are considered safe to environment and health during manufacturing and usage.
Applications of enzymes in preparatory and in biopolishing, natural dyes for
colouration, biopolymers, and their derivatives in fibre production and finishing
processes, etc., are some of them. During recent years, the biopolymer that has
drawn good attention is chitosan, which is derived from alkaline deacetylation of
16 N. Gokarneshan et al.

Fig. 14 SEM images of nanocapsule-finished fabrics after 10, 20, and 30 washes under different
magnifications a ×250, b ×500, c ×1000 and d ×3000 (Sumithra and Vasugi Raaja 2012)
Advances in Nanotextile Finishes—An Approach Towards Sustainability 17

chitin (Sathianarayanan et al. 2011). The precursor chitin is a nitrogen-containing

polysaccharide, which is second most abundant biopolymer after cellulose, dis-
tributed in the shells of crustaceans such as crabs, shrimps, and lobsters and in the
exoskeleton of marine zoo plankton, including coral, jellyfish, and squid pens. It is
totally ecofriendly and renewable (Tatiana et al. 2008; Thilagavathi et al. 2007).
Chemically, chitosan is a linear linked 2-amino-2-deoxy-β-D-glucan (i.e. β-D-glu-
cosamine) having the structure very much close to that of cellulose except the
hydroxyl group in C of cellulose is being replaced by amino group in chitosan.
Indeed, it is a copolymer of N-acetyl-glucosamine and glucosamine units. Being a
primary aliphatic amine, chitosan can be protonated by various acids (El-Molla
et al. 2011). In view of the many valuable inherent properties like antibacterial,
antifungal, antiviral, antacid, non-toxic, totally biodegradable, biocompatible with
animal and plant tissues, and film formation, fibre formation, and hydrogel for-
mation properties, chitosan holds promise in a number of applications like
biomedical, wastewater treatment, cosmetics, dentifrices, food, agriculture, pulp
and paper, and textile industries (Muzzarelli 1996; Hirano 2003; No and Meyers
1995).
The application potential of chitosan in textiles has been reviewed comprehen-
sively (Oktem 2003; Harish Prashant and Tharanathan 2007). Studies have revealed
that it can also be used as a dye-fixing agent, for shade and naps coverage, for
enhancing the fastness of dyed fabrics, as a binder in pigment printing, and as a
thickener in printing. By virtue of its bacteria-impeding property, chitosan can
prevent garments from developing bad odour (Giri Dev et al. 2005; Kean et al.
2005; Enescu 2008; Inamdar and Chattopadhyay 2006; Achwal 2000). An
improved wrinkle recovery of cotton fabric is reported on finishing cotton with
citric acid solution in presence of chitosan with minimum loss in tensile strength
due to citric acid treatment (Achwal 2003). It is found that complete inhibition of
E. coli and Hay bacillus bacteria is possible by treatment of cotton with 0.5 gpL
chitosan concentration (Hasebe 2001). Tiwari and Gharia (Eom 2003) attempted to
use chitosan as a thickener in printing paste. Performance of the prints with respect
to K/S, wash fastness, crock fastness, and hand are observed to be unsatisfactory.
Earlier studies have shown improved dyeability towards direct dyes of
chitosan-pretreated cotton fabric, and the degree of improvement was found to be a
function of molecular weight and concentration of chitosan (Knittel and
Schollmeyer 2002). The fastness to washing of direct dyes on chitosan-pretreated
fabric, however, was only slightly improved especially for the low molecular
weight chitosan applications. Chitosan-treated cotton fabric also showed a sub-
stantial dyeability towards acid dyes. But, the appearance and handling of the
treated fabric have been adversely affected. There has been decrease in the wrinkle
recovery property. Due to the rigid film deposition of chitosan on cotton fibre
surface, there is loss in inherent qualities of cotton fibres.
But it is necessary to improve above properties without changing the inherent
natural qualities of cotton. It is possible by achieving the maximum penetration of
polymer particles into fibre structure and increasing its effectiveness at lowest
possible concentration. The decrease in particle size or reducing the viscosity of its
18 N. Gokarneshan et al.

solution helps to improve the penetration of chitosan solution. Reduction in con-

centration of normal chitosan in solution, however, may reduce its effectiveness and
larger chain does not permit its entry into the yarn/cellulose structure. The only
possible way is to reduce the particle size, which, in addition to decrease in vis-
cosity, offers greater surface area and hence increases the effectiveness of chitosan.
It forms the basis of the nanotechnology concept. The potential applications of
nanochitosan are well demonstrated in medical field particularly in controlled drug
delivery systems (Chattopadhyay and Inamdar 2009; El-Tahlawy 1999; Zhang et al.
2003). But, their applications in textiles have not yet been well studied. The
practical application of such nanochitosan to textiles at shop floor level demands
suitable technology for the production of nanochitosan dispersions, characterization
and the analysis of stability of standing baths. Therefore, attempt has been made to
set a simple methodology to produce nanochitosan by ionotropic gelation with
pentasodium tripolyphosphate. Chitosans of different molecular weights are
obtained by controlled depolymerization of parent chitosan using nitrous acid
hydrolysis, and these products are subsequently used for the synthesis of
nanochitosan. The final results of many basic experiments after getting the con-
firmation of reproducibility are given herein. A representative concentration of
1gpL is, therefore, only reported and discussed here to make it as brief as possible
and to avoid presenting less important data. The influence of particle size on
different properties of nanochitosan-treated cotton fabric, like appearance, stiffness,
absorbency, dyeing behaviour, and wrinkle recovery, has been explained. SEM
images of nanochitosan-treated cotton fabric have also been analysed.

7.3 Technical Details

The following materials have been used

• 100 % cotton fabric ready for dyeing stage
• Certain class of direct dyes
• Chitosan (CHT1), having degree of deacetylation (DAC) 90 % and viscosity
22 cPs
• Dimethylol dihydroxy ethylene urea (DMDHEU) and other chemicals such as
sodium tripolyphosphate (TPP), acetic acid, sodium nitrite, sodium acetate
(anhydrous), and sodium hydroxide used were of analytical grade.
Chitosans with various molecular weight grades have been first obtained by
depolymerization of CHT1 by nitrous acid hydrolysis method, which have been
employed for the preparation of nanochitosan dispersions as described elsewhere
(Tiwari and Gharia 2003). In general, chitosan was dissolved in acetic acid solution,
and an optimized quantity of TPP was added drop-wise with rapid stirring (about
400 rpm) to obtain an opalescent solution. The sample was allowed to stand
overnight, filtered through sintered glass filter of porosity grade G3, and preserved
Advances in Nanotextile Finishes—An Approach Towards Sustainability 19

in refrigerator. The prepared nanochitosan was termed as CHT1 N (Chattopadhyay

and Inamdar 2013). The synthesized nanochitosan was applied to cotton fabric
within 24 h since the stability of nanochitosan gets adversely affected with time as
discussed earlier. The various grades of chitosan and nanochitosan have been
specified. A particle size analyser has been used to determine the particle size and
size distribution of the chitosan.
A two-dip–two-nip technique has been used to apply nanochitosan dispersion
(1 gpL) onto fabric, using a padding mangle with wet pickup of 70 %. After drying,
the fabric was cured in oven at 150 °C for 4 min. The sample was then washed in
the following sequence: rinse → alkali wash (soda ash 1 gpL, MLR 1:50) → hot
wash (twice) (85 °C/20 min) → cold wash → dry.
The following studies have been done
• SEM
• Evaluation of Indices
• Fabric Stiffness, Tenacity and Absorbency
• Crease Recovery Angle and Antimicrobial Activity.

7.4 Synthesis and Characterization of Nanochitosan

Chitosan possesses quite a long linear structure and has rigid conformation.
The CHTI (Parent chitosan sample 1) has a characteristic size of hydrodynamic
sphere of 4014 nm. The higher viscosity of the solution is due to the higher particle
size in the solution. Any molecular size chitosan can reduce the particle size to
nanolevel by ‘bottom-up’ approach (Patel and Jivani 2009). Due to its polycationic
nature, chitosan is subjected to ionic gelation with poly anions like pentasodium
tripolyphosphate (TPP), ethylene diamine tetra acetic acid (EDTA), resulting in
formation of nanoparticles. Such particles are stabilized by electrostatic hindrance
due to coulombic repulsion between particles of same ionic charges (Zhang et al.
2010; Trapani et al. 2009; Chattopadhyay and Inamdar 2010). Owing to faster ionic
reactions between chitosan and TPP, non-toxic nature of these components and ease
of operation, we adopted the gel ionization technique for the synthesis of
nanochitosan particles. The particle size distribution of CHT5 N, having particle
size of 110.74 nm, is given in Fig. 15. Scaling down the particle size of large
polymeric materials to nanolevel is a big challenge. It is clear from them present
study that the molecular weight (Table 1) has a great role in controlling the particle
size and by reducing the molecular weight we achieved about 110-nm particle size.
The study evidently shows that the particle size can be decreased below 100 nm by
conducting a trial with parent chitosan of low molecular weight (lesser than
10,000). This investigation would provide a platform for future work of such a type
and would serve basic information to the future researchers.
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