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Antibacterial Conductinf Cotton W Si Modified PPy
Antibacterial Conductinf Cotton W Si Modified PPy
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antibacterial conductive DOI: 10.1177/1528083720906808
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cotton fabrics via
silane-modified
polypyrrole
Abstract
In this study, silane-modified polypyrrole (PPy) was coated onto cotton fabrics through
a conventional “in situ polymerization” method. And by chlorination with NaClO solu-
tion, we obtained antimicrobial conductive PPy/Si–Cl–cotton fabrics. The PPy/Si–Cl–
cotton fabrics were characterized by scanning electron microscopy, energy-dispersive
spectroscopy, X-ray photoelectron spectroscopy, Fourier-transform infrared and ther-
mogravimetric analysis. Also, the electrical conductivity property, antibacterial proper-
ty, and ultraviolet light stability of the coated fabrics were tested. The PPy/Si–Cl–cotton
fabrics showed antimicrobial and electrical conductivity properties when the chlorina-
tion time was up to 30 s. The chlorine content was 0.30 wt% and the resistance was
26.79 kX/cm. The PPy/Si–Cl–cotton fabrics (Clþ% 0.30) showed excellent antibacterial
properties against 100% Staphylococcus aureus and 100% Escherichia coli O157:H7 were
inactivated within 1 min of contact. Due to the proportional relationship of the elec-
trical conductivity and chlorine content of the PPy/Si–Cl–cotton fabrics, the electrical
conductivity of the PPy/Si–Cl–cotton fabrics can be used for monitoring the antimicro-
bial activity.
1
Key Laboratory of Eco-textiles of Ministry of Education, College of Textiles and Clothing, Jiangnan University,
Wuxi, Jiangsu, PR China
2
Department of Poultry Science, Auburn University, Auburn, AL, USA
Corresponding author:
Xuehong Ren, Key Laboratory of Eco-textiles of Ministry of Education, College of Textiles and Clothing,
Jiangnan University, Wuxi, Jiangsu 214122, PR China.
Email: xhren@jiangnan.edu.cn
2 Journal of Industrial Textiles 0(0)
Keywords
Polypyrrole, cotton, antibacterial, conductivity
Introduction
Static electricity is a potentially harmful phenomenon of textile production and can
become a big issue for textiles operation and cause industrial losses and endanger
human life. To prevent electrostatics in textiles, it is necessary to provide anti-
electrostatic clothing for workers and people. Therefore, wearable conductive
materials are of great importance for the prevention. In addition, they are applied
in wearable displays [1,2], medical clothing [3], facilities [4], and military equip-
ments [5]. Wearable conductive textiles are primarily designed by integrating con-
ductive fillers, such as conductive polymers [6,7], metal [8–10], and carbon-based
materials [11–13] into soft-based templates.
The majority of traditional wearable conductive materials are made by coating
conductive polymers onto fabrics. In 1977, Park Y et al. [14] used AsF5 and I2 to
dope polyacetylene to endow it with electrical conductivity. Since then, the
research of conductive polymeric materials has been developed rapidly. Many
polymers, such as polyacetylene, polyaniline, polypyrrole (PPy), polythiophene,
and polyindole, were found to possess conductive activities. Among conductive
polymers, PPy is considered as one of the most useful conductive polymers due to
its low cost, high electrical conductivity, and good chemical stability. It has been
widely used for gas sensors and biosensors [15,16]. Cotton fabrics draw much
attention in anti-electrostatic research and are widely used to make anti-
electrostatic clothing due to its cheap cost, comfort, light weight, high porosity,
large surface area, and good reactivity. Lu et al. [17] used cationic surfactant to
enhance the electrical conductive property of PPy-coated cotton fabrics. Khajavi
and Berendjchi [18] reported the formation of PPy films on pristine and precation-
ized cotton samples using admicellar polymerization by increasing the adsorption
of sodium dodecyl sulfate (SDS) on cotton fabric, enhancing the conductivity of
these samples up to 49%. Nautiyal et al. [19] coated PPy onto carbon steel using
electrochemical synthesis, and the coating showed great anti-corrosion and excel-
lent biocidal properties.
However, cotton fabrics are good media and carriers for microbial growth, such
as bacteria, fungi, and viruses, under suitable environment due to its hydrophilic
property retaining moisture, oxygen, and nutrients [20]. Cotton fabric has strong
hydrophilic property. Through surface modification of cotton fabric, its hydro-
phobicity can be improved [21–24]. It is important to produce PPy-coated cotton
with antibacterial property. The simple way of making antibacterial PPy-coated
fabrics is to add metal such as silver. However, high cost, poor softness, and
fastness limit their industrial production. Based on the structure of PPy
(Figure 1), PPy can be regarded as a polymeric N-halamine precursor since the
Xiao et al. 3
N–H bonds on the rings of PPy could be transformed into N–Cl bonds upon
chlorination. N-halamines are very effective biocides in inactivation of bacteria.
N-halamines compounds contain N–X covalent bonds, formed by amine, amide,
or imide group [25,26]. When N-halamines compounds are exposed to sodium
hypochlorite (NaClO) solution, the N–H bonds are transformed into N–Cl,
which have a good killing bacteria effect [27,28].
In this study, silane-modified PPy was prepared and coated onto cotton fabrics
by chemical oxidative polymerization. The morphology, elemental composition,
electrical conductivity, and thermal property of the coated fabrics were investigat-
ed. The relationship between electrical conductivity and chlorine content of the
PPy/Si–Cl–cotton fabrics was also explored. The PPy/Si–cotton fabrics after chlo-
rination were evaluated for their biocidal efficacies against Staphylococcus aureus
and Escherichia coli O157:H7.
Experiment
Materials
100% bleached cotton fabric was provided by Zhejiang Guandong Printing &
Dyeing Company, Zhejiang. Pyrrole monomer (Py, 98%) was purchased from
J&K Chemicals (Shanghai, China), and distilled under reduced pressure before
use. 3-Amino-propyltriethoxysilane (C9H23NO3Si) (98%) was purchased from
J&K Chemicals (Shanghai, China). Ammonium persulfate ((NH4)2S2O8, APS),
hydrochloric acid (HCl), NaClO, and ethyl alcohol (CH3CH2OH) were from
Sinopharm Chemical Reagent Co., Ltd, Shanghai. These chemicals were used
without further purification and all solutions were prepared with deionized water.
Instruments
Scanning electron micrographs were obtained using a SU-1510 scanning electron
microscope (SEM, Hitachi, Tokyo, Japan) at 5 kV accelerating voltage. The
S-4800 energy-dispersive X-ray spectroscopy (EDS, Hitachi, Tokyo, Japan) was
used to analyze the chemical compositions of samples. X-ray photoelectron spec-
troscopy (XPS) was performed on an ESCALAB 250Xi (Thermo Fisher, USA).
4 Journal of Industrial Textiles 0(0)
The Fourier transform infrared (FTIR) spectra were recorded by a Nicolet Nexus
470 spectrometer (Nicolet Instrument Corporation, Madison, WI) in the optical
range of 500–4000 cm1 by averaging 32 scans at a resolution of 4 cm1. The
resistance of the coated fabrics was measured by SZT-2 A four-point probe
tester (Thongchuang, Suzhou, China). UV-blocking property of the samples was
measured using a YG (B) 912E UV spectrophotometer (Shimadzu Co., Ltd.,
China). Thermogravimetric analysis (TGA) was carried out using a TGA unit
(TA Instruments, USA). A 5-mg sample was heated from 35 C to 600 C at a
heating rate of 10 C min1 under nitrogen atmosphere with 40 mL min1 flow rate.
N V 35:45
Clþ % ¼ 100 (1)
W2
where Clþ (wt%) is the weight percent of oxidative chlorine on the coated cotton
samples, N and V are the normality (eq/L) and volume (L) of the titrant sodium
thiosulfate, respectively, and W (g) is the weight of the coated cotton samples.
Xiao et al. 5
where E(k) is the solar irradiance (Wm2nm1), e(k) the erythema action spec-
trum, Dk the wavelength interval (nm), and T(k) the spectral transmittance of the
samples.
Antimicrobial test
PPy/Si–cotton fabric swatches and PPy/Si–Cl–cotton fabric swatches were chal-
lenged with S. aureus (ATCC 6538) and E. coli O157:H7 (ATCC 43895) using a
modified AATCC Test Method 100-2004. An aliquot of 25 lL bacterial suspension
in pH 7 phosphate buffer was added to one swatch, and another identical swatch
was placed on it. A sterile weight was placed on the top of the samples to ensure
the contact between the bacterial suspension and the swatches. After contact time
from 1 min to 30 min, each sample was transferred to a tube containing 5.0 mL of
sterile 0.02 N sodium thiosulfate to remove all oxidative chlorine. A 10-fold serial
dilution was applied to all quenched solutions with pH 7, 100 mM phosphate
buffer, and each dilution was plated on Trypticase soy agar plates. The plates
were incubated at 37 C for 24 h. The bacterial colonies were enumerated and
recorded for biocidal efficacy analysis.
6 Journal of Industrial Textiles 0(0)
Figure 2. SEM images of uncoated cotton fabrics and PPy/Si-cotton fabrics: (a) uncoated cotton
fabrics 10 k, (b) uncoated cotton fabrics 2 k, 2 k; (c) PPy/Si-cotton fabrics 2 k, (d) PPy/Si-
cotton fabrics 10 k, (e) PPy/Si-cotton fabrics 30 k.
Xiao et al. 7
and chlorine. The mass ratio of nitrogen to carbon of PPy/Si–cotton was lower
than that of pure PPy. The presence of silicon was due to 3-aminopropyltriethox-
ysilane in the coating solution. In addition, the presence of chlorine confirmed the
doping of hydrochloric acid into PPy coating. The presence of sulphur demon-
strated that APS was an oxidizing agent in PPy/Si system. Compared between
Figure 3(a) and (b), the weight percent of chlorine increased after chlorination.
In order to determine the elemental composition of the samples, XPS analysis
was applied to characterize the chemical state of the samples. In Figure 4(A),
binding energy of uncoated cotton, PPy/Si–cotton, and PPy/Si–Cl–cotton are
shown. Compared with uncoated cotton, new peaks at binding energies of
400.7 eV, 200.8 eV, 151.9 eV, and 100.9 eV were observed, corresponding to N,
Cl, S, and Si elements, respectively. After chlorination, the peak of chlorine at
200.78 eV could decompose into four contributions including 197.8, 200.2, 201.2,
and 202.3 eV, attributing to Cl 2p3/2, Cl 2p1/2, N–Cl 2p3/2, and N–Cl 2p1/2,
which revealed that N–H was successfully converted to a N–Cl bond [34].
Figure 5 shows the FTIR spectra of uncoated cotton fabrics and PPy/Si–cotton
fabrics. In Figure 5(a), the peak at 3303 cm1 is assigned to the characteristic broad
band for the O–H group of cellulose and a peak around 2906 cm1 can be
Figure 3. EDS of PPy/Si-cotton fabrics (a), PPy/Si-Cl-cotton fabrics (b) and pure PPy (c).
8 Journal of Industrial Textiles 0(0)
Figure 4. XPS spectra (A), Cl 2p fitting spectra (B): (a) cotton fabrics; (b) PPy/Si–cotton fabrics;
(c) PPy/Si–Cl–cotton fabrics.
Figure 5. FTIR spectra of uncoated cotton fabrics (a) and PPy/Si–cotton fabrics (b).
Figure 6. Chlorine content of PPy/Si–Cl–cotton with different chlorinated time (a) and resis-
tance of PPy/Si–Cl–cotton with different chlorine content (b).
1454 cm1 is assigned to five-membered ring stretching and the free C–N stretching
vibration of Py rings [36,37]. The band at 1072 cm1 is ascribed to Si–O between 3-
aminopropyltriethoxysilane and cotton fabrics [38,39]. The peak at 778 cm1 is
attributed to N–H inplane deformation vibration which is attributed to the N–H
bonds in PPy and 3-aminopropyltriethoxysilane [40]. All the peaks above con-
firmed the attachment of PPy/Si to cotton fabrics.
Table 1. UV protection properties and air permeability of the coated cotton fabrics.
Cotton 4 149.93
PPy/Si–cotton 382 72.47
PPy/Si–Cl–cotton (Clþ% 0.19) 319 73.05
PPy/Si–Cl–cotton (Clþ% 0.30) 307 74.52
PPy/Si–Cl–cotton (Clþ% 0.42) 271 79.01
PPy/Si–Cl–cotton (Clþ% 0.66) 175 88.88
PPy/Si–Cl–cotton (Clþ% 0.81) 134 90.87
fabrics can be used to monitor the electrical signals in order to keep its high
antimicrobial efficacy and good electrical conductivity.
Thermal analysis
TGA and DTG curves of uncoated cotton, PPy/Si–cotton, and PPy/Si–Cl–cotton
are shown in Figure 7. The weight loss below 200 C (Figure 7(a)) was due to the
removal of absorbed water [44]. In comparison, a lower weight loss temperature is
observed for PPy/Si–coated cotton fabrics than that of untreated fabric due to
doping acid accelerating decomposition of the composites. The presence of PPy
and 3-aminopropyltriethoxysilane enhanced the thermal stability of cotton fabrics
and increased the amount of char residues. Cotton fabrics displayed the onset of
degradation (9% mass loss) at 310 C and reached 11% char yield of the mass at
600 C. The decomposition of PPy/Si–cotton and PPy/Si–Cl–cotton fabrics started
Xiao et al. 11
Figure 7. TGA (a) and DTG (b) curves for uncoated cotton, PPy/Si–cotton fabrics and PPy/Si–
Cl–cotton fabrics (Clþ wt% 0.30).
TGA: thermogravimetric analysis; DTG: derivative thermogravimetric.
at 263 C and 246 C and provided a higher char yield of 35% and 37% at 600 C,
respectively. It can be seen in Figure 7(b) that the uncoated cotton fabrics had the
fastest decomposition rate at 378 C. The PPy/Si–cotton and PPy/Si–Cl–cotton
fabrics had maximum decomposition rate at 364 C and 368 C, respectively. The
maximum decomposition rate of the coated cotton fabrics was lower than
uncoated cotton fabrics. The results illustrated that the PPy/Si coatings might be
able to advance the second decomposition stage of the coated cotton fabrics and
cause the increase of char residue. In addition, there was nitrogen containing
components in PPy, which formed a gas protective layer on the fabric surface.
3-Aminopropyltriethoxysilane coated on cotton produced siliceous char layer
which acts as a barrier to heat, fuel, and oxygen transfer, protecting the underlying
cotton fabrics from fire spread and prevented further oxidative degradation of
cotton fabrics [45]. Compared with PPy/Si–cotton, PPy/Si–Cl–cotton had a
decomposition started at 190 C and continued up to 270 C, which was close to
the decomposition of the N–Cl bonds [46].
Tensile strength
In order to evaluate the effect of the coating and chlorination on the mechanical
property of the coated cotton fabrics, the tensile strengths in warp and weft direc-
tions of uncoated cotton and coated cotton with and without chlorination were
tested. Figure 8 shows that uncoated cotton fabric has an average breaking
strength of 734 N in the warp and 325 N in the weft directions. After coating
with PPy/Si, 27% and 16% of breaking strength was lost in the warp and weft
directions, respectively, which might be due to the breaking of glycoside bonds in
cellulose caused by the acidic polymerization reaction system. The chlorination
treatment has a small effect on the breaking strength of the PPy/Si–Cl–cotton
12 Journal of Industrial Textiles 0(0)
fabrics. The breaking strength after chlorination was almost the same as before
chlorination in the warp direction, and 10.3% of breaking strength was lost after
chlorination in the weft direction compared to PPy/Si–cotton fabrics.
Antibacterial efficacy
The PPy/Si–cotton and PPy/Si–Cl–cotton fabrics were challenged with S. aureus
(Gram positive) at 1.07 106 CFU/sample and E. coli O157:H7 (Gram negative) at
1.47 106 CFU/sample, with the biocidal efficacy data are presented in Table 2. As
the control sample, unchlorinated PPy/Si–cotton showed small reductions for both
bacteria, which were 0.84 log and 0.49 log reductions for S. aureus and E. coli
O157:H7, respectively, after 30 min contact time due some the adhesion of bacteria
onto the surface of cotton fabrics. The PPy/Si–Cl–cotton fabrics with 0.30% active
chlorine could completely inactivate all inoculated S. aureus (6.03 log) and E. coli
O157:H7 (6.17 log) after 1 min contact. The results show that PPy/Si–Cl–cotton
fabrics have a great potential for using as antibacterial products in different appli-
cations. After chlorination, the hydrogens of the N–H bonds were substituted by
chlorines, and PPy/Si–Cl transferred the active chlorines to the bacterial cells, kills
them upon contact. After inactivating bacteria, the biocidal function could be lost
since active chlorines were consumed. The lost chlorines could be regained with
diluted bleach solution to reinstall the antibacterial function. It has been found
that the chlorine content of the PPy/Si–Cl–cotton fabrics is negatively related to
the electrical conductivity. Therefore, the electrical resistance of PPy/Si–Cl–cotton
can be used as an indicator of the chlorine content for monitoring the antibacterial
efficacy.
Xiao et al. 13
Bacterial reduction
Conclusions
The PPy/Si–cotton fabrics were successfully prepared by a chemical polymeriza-
tion method and exhibited good electrical conductivity with the resistance of
0.86 kX/cm. After exposure to 10 wt% NaClO solution, the PPy/Si–Cl–cotton
fabrics were endowed an antibacterial function. The PPy/Si–Cl–cotton fabrics
(0.30% Clþ, wt%, 26.79 kX/cm resistance) showed excellent antibacterial efficacy
against S. aureus and E. coli O157:H7, and were able to inactivate 100% inocu-
lated S. aureus (6.03 log) and E coli O157:H7 (6.17 log) within 1 min of contact
time. This reported method for preparing antimicrobial/conductive coatings on
cotton fabrics is simple, green and highly effective. It has a great potential appli-
cation of low-cost and high-performance multifunctional coatings in textiles to
manufacture antielectrostatic clothing and wearable conductive materials.
Funding
The author(s) disclosed receipt of the following financial support for the research, author-
ship, and/or publication of this article: This study was supported by the research funds from
the Project for Jiangsu Scientific and Technological Innovation Team, and the Fundamental
Research Funds for the Central Universities (No. JUSRP51722B), the national first-class
discipline program of Light Industry Technology and Engineering (LITE2018-2), and 111
Projects (B17021).
ORCID iD
Xuehong Ren https://orcid.org/0000-0002-1682-9062
14 Journal of Industrial Textiles 0(0)
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