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Chapter

Cotton Based Cellulose

Nanocomposites: Synthesis and
Application
Patricia Jayshree Samuel Jacob

Abstract

Nanocellulose is a renewable natural biomaterial which has risen to prominence

due to its biodegradability and physiochemical properties making it a promising
candidate to replace non-biodegradable synthetic fibers. Due to its profound qualities,
nanocellulose extracted from cotton fibers have tremendous application potential
and have been intensively studied particularly in the generation of nanofillers and as
reinforcement components in polymer matrixes. Deposition of inorganic nanopar-
ticles on cotton fabric result in antimicrobial textiles with multifunctional use
particularly in manufacture of PPE and as filtration devices against environmental
pollutants and pathogens. This chapter compiles three main sections. The first section
gives an overview of the extent of work done in the creation and application potential
of cotton-based nanocomposites. The second section describes the in situ and ex situ
methods of nanoparticle deposition and self assembly on cotton fabrics to generate
multifunctional cotton-based nanocomposites with antimicrobial potential while the
final section describes the incorporation of cotton nanofibers in polymer matrices,
their reinforcing properties, as well as surface modification to assist their incorpora-
tion. Finally in the conclusion, a summary of the up-to-date challenges and progresses
is presented postulating the undiscovered arenas and future undertakings of this
venture.

Keywords: cotton nanostructures, cellulose nanocomposites, nanofibers,

nanocellulose, antimicrobial textiles, reinforcement fillers

1. Introduction

With the dawn of the age of nanotechnology, there has been an intense scurrying
and scavenging for nanomaterials with unique properties and specific molecular
arrangements that allow it to find application in specific niches inaccessible to
alternative forms. Nanostructured materials display unique physicochemical proper-
ties such as excellent electrical and thermal conductivity, solubility, porosity, surface
interactions, density, band gap and surface electronic charge resulting in exceptional
catalytic and optical activity and enhanced performance compared to their bulk
counterparts [1]. Presently, nanoscale devices have widespread application in cell tar-
geted therapeutic delivery, high resolution tissue imaging and in replacing damaged
1
Cotton

tissue [2]. In agriculture, nanomaterials are being used to enhance crop production
as nanofertilizers [3] and for crop protection as nanopesticides and nanobiosensors
[4]. These active ingredients are encapsulated in nanocapsules, micelles, gels, lipo-
somes, mesoporous silica nanoparticles or hollow nanoparticles to ensure controlled
release, better solubility and for active stablity in the long-term [5]. To compensate for
hazardous emissions to the environment, nanomaterials have been functionalized to
remove contaminants through adsorption [6], immobilization, photocatalytic degra-
dation, and electro-nanoremediation [7]. It is therefore undeniable that uncovering
novel multifunctional nanosized materials is an elaborate pursuit with promising
outcomes, yet filled with pressing concerns which are in dire need to be addressed.
One of the primary concerns of nanotechnology is the indiscriminate release
of hazardous nanowaste, generated during the manufacturing and processing of
engineered of nanomaterials, which could inevitably accumulate in the environment
and inevitably end up in the food chain [8]. This has roused an overdrive in the hunt
for sustainable nanomaterials from renewable bioresources such as cellulose, starch,
chitosan, gelatin, alginate and chitin which are biodegradable, leave minimal implica-
tions on health and the environment and could be retrieved as value added waste in
the production of a new generation of green nanomaterials [9].
Cellulose is a renewable feedstock with interesting properties such as biocompat-
ibility and biodegradability. It is found to be chemically inert, displays excellent stiff-
ness, high strength and dimensional stability, low density and easily functionalized
surface chemistry [10]. Lignocellulosic biomass such as wood and agricultural resi-
dues such as tree trunks, rice straw, sugarcane bagasse, coconut husks, oil palm empty
fruit bunches energy crops and grass are excellent feedstocks for green nanomaterials
derived from cellulose or nanocellulose. This natural biopolymer is abundantly avail-
able and can be used as renewable feedstock in the generation of sustainable nanoma-
terials [11]. Reconstruction of lignocellulosic biomass waste residues into value added
products such as nanostructures is an attractive, feasible option [12].
Cotton is an abundantly available fibrous crop grown for global commercial
production with over 95% cellulose in its plant structure. Cotton stalk which is an
overbearing agricultural residue generated in cotton-producing countries such as
India, USA, China, Brazil and Pakistan, represents a semi-wood raw material made
up of cellulose, hemicellulose, and lignin which could be utilized to fabricate value-
added nanocellulose, paving an excellent way to maximize the utilization of waste
[13]. Nanocellulose has exceptional properties such as high tensile strength, high
Young’s modulus, low weight, mechanical robustness, low coefficient of thermal
expansion, biodegradability, surface functionality and hydrophilicity, biocompatibil-
ity and lack of toxicity [14]. In recent times, nanocellulose is used in energy storage,
as aerogels, emulsion stabilizers, enzyme immobilization substrates, low-calorie
food additives, reinforcing fillers, pharmaceutical binder, biomimetic materials and
biosensors [15–17]. Nanocellulose derived from cotton feedstock can be broadly
categorized as cellulose nanocrystals (CNC) and nanofibrillated cellulose (NFC).
CNCs (as shown in Figure 1), also known as cellulose nanowhiskers or nanorods,
are short (<500 nm) and narrow (<40 nm) rod shaped, rigid crystalline structures
with diameters between 1 and 100 nm [18] with tremendous application potential in
regenerative medicine [19], optoelectronics [20], automotive polymers [21] and as
composite materials [22]. It is generated by eliminating the amorphous regions in cel-
lulose fibers using acid hydrolysis [23]. CNC have been extracted from cotton fibers
[24], processed cotton [25] and cotton linters [26], a byproduct of cotton processing.
NFC or cellulose nanofibers (as shown in Figure 2) are longer (< 3000 nm) and wider
2
Cotton Based Cellulose Nanocomposites: Synthesis and Application
DOI: [Link]

Figure 1.
TEM image depicting cotton-derived CNC.

Figure 2.
FESEM images of the cotton based NCFs.

(< 100 nm) fibers with low crystallinity obtained by the mechanical disintegration of
cotton biomasses using a high-speed ball grinder [27], ultrasonicator [28] or high-
pressure homogenization [29].
Nanocomposites are materials made up of 2 or more constituent phases with at
least 1 phase of nano-size particles (<100 nm) which creates a discontinuous phase
over a matrix of standard material [30]. This unique multiphase structure that is
reinforced by a stronger component of nanosized fillers [31] demonstrates greater
mechanical and tensile strength and increased capacity for thermal expansion and
3
Cotton

conductivity [32]. CNCs are interesting materials that could function as nano-
fillers owing to the abundance of the -OH groups, reactivity, high surface area,
mechanical, thermal and optical properties, even at low concentrations [33] which
enhances tensile strength and decreases elasticity due to the strong intermolecular
linkages such as covalent bonds, van der Waals forces, mechanical interlocking and
molecular entanglement between the fillers and its polymeric matrix [34]. Various
methods have been developed to generate cellulose nanocomposites which include
melt extrusion, ball milling, injection molding, compression molding, 3D printing,
layered assembly, electrospinning, among others [35, 36]. Cellulose nanocomposites
find vast application as packaging material, automotive and aerospace paints and
coatings, adhesives, hydrogels, nanobarriers, fire retardants, construction materials,
military defense and as emerging smart hybrids which display outstanding proper-
ties such as stretch ability, high mechanical strength, optical transparency, electrical
and thermal conductivity, porosity and high adsorption [37]. Cotton based cellulose
nanocomposites constructed with metals, metal oxides and non-metallic elements
have exhibited innovative features due to its synergetic effects which are unattainable
as pure nanomaterials [38]. Nanocomposites loaded with noble metal nanostructures
have antibacterial properties and are used in biomedicine, enzyme immobilization,
catalysis and as biosensors [39]. Rumi et al., 2021 observed that cotton-based CNC
display high crystallinity, tensile strength and stiffness making it an attractive engi-
neering nanomaterial for composite reinforcement [40]. In a separate study, Araujo
et al., 2018 found that biopolymer nanocomposites reinforced with hydrolyzed
cotton NFC extracted from cotton waste textiles resulted in a composite material
with greater tensile strength and thermal capacity compared to the pure biopolymer
[25]. Rafaella et al., 2019 constructed a cotton NFC/chitosan nanocomposite with
collagen like properties which demonstrated increased surface roughness, improved
cell adhesion, spreading and proliferation when used as scaffolds in tissue engineer-
ing [41]. Thus, surface modification of polymeric materials with cotton NFC for
substrates used as scaffolds in tissue engineering would result in functionalized
nanocomposites with novel physicochemical properties and large surface area which
allow numerous contact points between cells and the nanocomposite surfaces for
cell viability and growth. In a separate study, Li et al., (2013) generated cotton CNC
through electrospinning and functionalized it into composites by surface coating
it with CeO2 nanoparticles using the hydrothermal reaction. The resulting cotton
based cellulose nanocomposite demonstrated excellent UV-shielding and enhanced
photocatalytic properties making it of great value in medicine, military operations
and optoelectronics [42].
Multifunctional cotton-based nanomaterials have been inadvertently thrust
into the limelight with the recent Covid-19 pandemic through the design of vari-
ous nanosensor devices for viral detection, surface decontaminants, antiviral
compounds and nanocomposite fabrics which serve to prevent or annihilate the
SARS-CoV-2. In this aspect, cotton nanocomposites have been constructed as
nanosensors in the detection of the virus and as antimicrobial textiles for medical
PPE (personal protective equipment). Eissa and Zourob, (2021) fabricated a cotton
CNF-tipped electrochemical immunosensor as a one-step diagnostic tool for the
detection of SARS-CoV-2 viral antigen [43]. Textiles embedded with antimicrobial
nanoparticles such as Ag, ZnO and CuO have been tailored as a protective measure
in PPE’s for those on the frontline of defense against the SARS-CoV-2. An extensive
research resulting in the design and manufacture of antibacterial cotton-based
face mask embedded with CuO nanoparticles (CuONps) demonstrated that cotton
4
Cotton Based Cellulose Nanocomposites: Synthesis and Application
DOI: [Link]

could be reconstructed as an antimicrobial nanocomposite and used as a PPV

fabric to secure the protection of medical personnel embodying it [37]. In this
work, Perelshtein et al., 2016 functionalized cotton fabric with CuONps using
ultrasound-assisted deposition by an in-situ coating process on the surface of
the fabric. The resulting nanocomposite material retained excellent antibacterial
properties after 65 washing cycles at 75–92°C, making it an excellent material as a
reusable medical PPE [44]. In a separate study, Adhikari et al., 2021 synthesized a
nanoceutical cotton ZnO composite fabric using the hydrothermal method to filter
viral particles without compromising on user’s breathing mechanism [45]. The
design of this nanoceutical fabric was constructed to find application as a one-way
valve in a face mask that would facilitate breathing while trapping and filtering
airborne viral pathogens and reducing transmission through droplets. It is therefore
undisputable that cotton nanocomposite fabrics are the textiles of the future as a
shield of protection in the war against the multitude of rising murderous pathogens
of this millennia.

2. Synthesis of cotton based cellulose nanocomposites using in situ and

ex situ methods

Cotton textiles are used widely in numerous applications and various industries
particularly as sportswear and medical textiles due to its exceptional properties such
as breathability, hypo allergenicity, hygroscopicity and low cost [46]. Some of the
drawbacks of cotton include low tensile strength, UV-vulnerability, enhanced capac-
ity for microbial growth and easily wrinkled [47]. Inserting nanoparticles into cotton
as antimicrobial agents to form nanocomposites is a way forward to manufacture
value-added fabric material [48]. These nanocomposites which are formed through
the in situ or ex situ deposition of nanoparticles in the fabric material has endowed
multi-functionalities to the cotton fabrics such as self-cleaning, UV protection
and electric conductivity [49]. Cotton based textiles can actually be designed with
self-cleaning features when hydrophobic surfaces are fabricated on these textiles to
repel water in such a way that spherical droplets of water can remove stains through
a mechanism known as easy roll-off. Wu et al., 2016 demonstrated that a sequential
deposition of poly(ethylenimine), silver nanoparticles (AgNp) and fluorinated
decylpolyhedral oligomeric silsesquioxane (F-POSS) on cotton fabrics resulted in
a superhydrophobic surface entailing a 169° angle of water contact with a 3° sliding
angle [50]. Cotton based nanocomposites embedded with ZnO, TiO2 and reduced
graphene oxides have also shown great promise in UV protection [51] and electro-
magnetic interference (EMI) shielding properties [52].
Fabrics with antimicrobial properties are sought after for the manufacture of
healthcare textiles particularly as packaging material for drugs and syringes or
medical tools, for the personal protective gear of medical personnel, in wound
dressing, surgical aprons and hospital bedding [53]. While cotton is undoubtedly
widely popular in the textile industry, its fibers are highly hydrophilic with a high
tendency of water absorption and oxygen retention and with a large surface area
causing it to be a breeding ground for bacteria and fungi [54]. Cotton nanocomposites
have been designed to incorporate metallic nanoparticles for the demonstration of
antimicrobial activity [55]. Incorporation of antimicrobial metallic nanoparticles into
cotton to generate nanocomposites could be carried out via ex situ or in situ meth-
ods. An understanding of the interactions of the intramolecular forces in a cotton
5
Cotton

nanocomposite architecture is critical in the selection of methods which appropriates

its functionality.

2.1 In situ synthesis of cotton based cellulose nanocomposites

The in situ synthesis of cotton based nanocomposites is a key approach to generate

composites with uniform dispersity using sol–gel or hydrothermal methods. In this
method, nanoparticles such as Ag, TiO2, CuO or ZnO are synthesized in situ using a
precursor, such as the aqueous salt solution of the metal and a reducing agent which
could be in the form of catalysts or plant extracts as in green synthesis. This would
lead to the self-assembly of nanoparticles in a one-pot synthesis [56]. The advantage
of using this method is that it initiates a unique assembly of nanostructures with
enhanced control of particle size, morphology and aggregation. However, synthetic
processes have to be designed meticulously to optimize appropriate assembly of
nanoparticles into composite structure to ensure the serving functionality of the
resulting nanocomposite [57].
The cellulose structure of cotton fiber constitutes complex chain conforma-
tions based on its chirality, length and morphology which varies consistently based
on the high degree of polymerization of cellulose chains in its fiber which is about
15,000 [58]. One of the major challenges in the synthesis of cotton nanocompos-
ites is to ensure uniform dispersion of nanoparticles without particle aggregation.
Nanoparticles aggregate due to high surface area, high surface energy and strong
inter-particle attractions [59] leading to lower Gibb’s free energy making it detrimen-
tal to material performance [60]. The spatial distribution and nanoparticle assembly
in a nanocomposite is primarily dependent on the delicate balance of intermolecular
forces between nanoparticles within the matrix of its [61]. For proper particle
dispersion, thermodynamic miscibility must be achieved [62]. Dispersion of the
nanoparticles is highly dependent on the hydrogen bonding capacity of the cotton
cellulose network. Where self-assembly of nanoparticles is strategically manipulated
within a polymer matrix, it would result in a novel functionality of the forthcoming
nanocomposite and expand its horizons for application due to its emerging properties
such as water resistance, modulation of light, electrical conductivity and antibacterial
sustenance [63]. It has to be noted that the ultimate performance of the nanocom-
posite is dependent on the interaction of the introduced nanoparticles and the cotton
matrix which modulates the self-assembly architecture of the nanocomposite. Cotton
fibers possess a backbone structure that is largely comprised of hydroxy groups which
impart a strong affinity to water molecules, inducing microbial growth and raising
the risk of contamination. The incorporation of the nanoparticle assembly however,
renders the composite surface to be hydrophobic. Hydrogen bonding is the primary
determinant in the spatial arrangement and self-assembly mechanism of molecules in
cotton nanocomposites caused by the OH groups present in the glycoside backbones
of the cotton cellulose fibers [57]. Hydrophobic interactions are also prevalent in
cotton nanocomposites but are also responsible for the aggregation of nanoparticles
in the structure [64]. Another force that participates in the self-assembly of nanopar-
ticles in biopolymers during the in-situ synthesis of cotton nanocomposites is the van
der Waals force, a short-ranged force, relatively weaker than hydrogen bonding, cre-
ated by a transient dipole moment produced by an attractive force when nanoparticles
move into close proximity [65].
Vajja et al., (2017) developed cotton nanocomposite material through the in situ
generation of copper nanoparticles (CuNPs) using a one-step hydrothermal method
6
Cotton Based Cellulose Nanocomposites: Synthesis and Application
DOI: [Link]

which demonstrated excellent antibacterial activity [49] while El-Naggar et al.,

(2016) incorporated Titanium oxide nanoparticles (TiO2NPs) on cotton fabrics
through in situ synthesis. The resulting nanocomposite demonstrated a microbial
reduction of more than 95% which was sustained after more than 20 washing cycles
[66]. In a separate work, Marnatha et al., (2018) generated bimetallic Ag and Cu
nanoparticles in situ in cotton fabric polymer matrix using Aloe vera leaf extract and
observed that besides demonstrating potent antimicrobial activity against Escherichia
coli, Pseudomonas, Klebsiella, Bacillus and Staphylococcus, the agglomeration of
these nanoparticles were also prevented through in situ synthesis [67]. ZnO nanopar-
ticles (ZnO Nps) are hydrophobic, inert and cost-effective and well known for its
photocatalytic activity, thermal stability, absorption in a broad range UV radiation
and flame-retardant properties [68]. ZnO Nps coating on cotton textiles have dem-
onstrated improved UV protective and antimicrobial properties [69]. However, most
of the cotton ZnO nanocomposites are prepared with polymeric binders using the
pad-dry-cure method [70]. The nanocomposite produced using this method produces
fabrics of high stiffness, poor wash durability and low air permeability [71]. As ZnO
Nps are deposited on the surface of the fabric, it does not form any chemical bonds as
ZnO does not have any ionic interaction with the OH groups of the cellulose, causing
it to only have a lose bond to the surface of the textile. Fabrics used as hospital bed-
ding and PPV go through frequent vigorous washing and surface deposition of ZnO
is not an appropriate method to generate cotton nanocomposites for applications that
require high washing frequency. In situ generation of nanoparticles in these textiles
are a better option. Verbic et al., 2021 demonstrated in situ synthesis of ZnO on cotton
fabric using pomegranate peel extract as a reducing agent and wood ash as alkali
with excellent UV protective properties due to the uniform dispersion of ZnONps
[72]. In another investigation, the in situ synthesis of ZnO cotton nanocomposites
was demonstrated using the one pot hydrothermal method which showed excellent
antibacterial, UV protection, and photo catalytic performance [73].

2.2 Ex situ synthesis of cotton based cellulose nanocomposites

The ex situ synthesis of cotton based cellulose nanocomposites is carried out

through a 2-step process. In the first step, metal oxide or metallic nanoparticles are
prepared either through homogeneous precipitation, wet chemical and hydrothermal
methods [74]. In the second step, the prepared nanoparticles are dispersed directly
onto the cotton fabric to form a nanocomposite. One method to disperse the prepared
nanoparticles in the fabric is through blending. In this approach, pre-synthesized
nanoparticles are mixed in the biopolymer such as starch or cotton through solvent
mixing or melting. Compared to the in situ method, a thorough dispersion of the
nanoparticles are necessary before being added to the polymer to prevent aggrega-
tion of the nanoparticles due to high surface energy. This method of nanocomposite
preparation is less tedious and flexible compared to in situ synthesis and can be scaled
up for commercial scale due to its to lower investment cost. The drawback using this
method is to prepare uniformly dispersed nanoparticles in biopolymers such as cotton
and which could remain stable in the long-term without aggregation [74].
An ex situ method used to form cotton nanocomposites of added value was by
surface coating the material with metallic or metal oxide nanoparticles. Daoud et al.
(2004) reported the deposition of anatase TiO2NPs on cotton and observed that the
coated cotton nanocomposite had enhanced UV protection, antibacterial potential
and self-cleaning properties [75]. Uddin et al. (2021) showed ex situ deposition of
7
Cotton

TiO2NPs on cotton fabric using the sol–gel method which demonstrated similar
properties [76]. A nanocomposite of AgNp loaded with SiO2 nanoparticles was pre-
pared using the sol–gel technique in which AgNps were generated using the Ocimum
lamiifolium plant extract and the Stőber method used to obtain a SiO2 impregnated
Ag nanocomposite. When this nanocomposite was loaded onto cotton fabric, it
demonstrated potent antimicrobial activity with no toxicity observed on mamma-
lian cells [53]. In a separate method, ZnONps were applied on the surface of cotton
fabric surface through layer-by-layer assembly [77]. This method otherwise known
as multilayer decomposition was rarely used in textile coating. Here, cotton fabric
was first cationised to generate positive charges on the surface of the fabric and then
soaked alternately in anionic ZnO solution at pH 11, deionized water, cationic ZnO
solution at pH 3 and deionized water repeatedly until 10–16 layers of ZnONps were
deposited. Finally, the nanocomposite material was dried at 60°C and cured at 130°C
for 3 min [78].
The ex situ synthesis of cotton nanocomposites using AgNP for antimicrobial
activity have been carried out through the incorporation of silver salts and organic
compound complexes of silver. However, this method entails a weak adhesion of this
antimicrobial agent to the cotton fabric, allowing the rapid release of AgNp with
increased washing resulting in lowered laundering durability. The release of Ag+ ions
from antimicrobial cotton nanocomposites also poses unnecessary duress to health
and the environment due to its potent toxicity [79]. The weak adhesion of AgNps
to cotton fabrics using the sorption process is a shortcoming in the production of
antibacterial cotton nanocomposite material and surface modification is required
to improve loading efficiency [80]. Shahidi et al., 2010 reported plasma-treatment
of the cotton fabric prior to coating with AgNps which enhanced absorption and
demonstrated increased quantity of AgNps on the surface of cotton. These nanocom-
posite fabrics showed 95% - 100% reduction in bacterial population which remained
consistent after 10 times consecutive laundering [81].

3. Cotton based nanocomposites constructed from nanocellulose

extracted from cotton cellulose nanofibers

Cotton nanofibers are natural fibers which mostly constitute holocellulose (cel-
lulose and hemicellulose) and lignin and has several advantages such as lower density,
availability, biodegradability and exceptional mechanical properties which make it
an ideal candidate as a polymer nanocomposite. The valorisation of agro residues of
cotton would result in novel materials that could be used as fillers or reinforcement
materials to form nanocomposites of potent value. Unlike other plants such as jute,
flax and kenaf which are made up of only 25% cellulose and wood-based trees which
contain 40–50% cellulose, cotton fibers are made up of 90% cellulose [82]. The cel-
lulose in the cotton fibers are among the highest in molecular weight among all plant
fibers and the most crystalline and fibrillated [83]. Cotton fiber comprises cellulose
with 1,4-d-glucopyranose structural units [84] which accumulate as microfibrils
arranged in regular pattern with excellent mechanical properties such as the Young’s
Modulus and low thermal expansion [85]. Nanofibers generated from cellulose
isolated from cotton fibers can be categorized as nanowires with aspect ratio beyond
1000, nanorods with aspect ratios between 3 and 5, nanoribbons and nanotubes with
aspect ratios >10 [17]. Dried cotton fibers comprise large amounts of cellulose and
hemi-cellulose which increase in tensile strength and durability when the impurities
8
Cotton Based Cellulose Nanocomposites: Synthesis and Application
DOI: [Link]

are removed. These cellulose based fibers are usually added as reinforcement mate-
rial to generate nanocomposites needed in construction, automotive and electronics
industry, as membranes for ultrafiltration, ion exchange and fuel cells and as binders
in pharmaceuticals and cosmetic fillers [86]. Cellulose nanofibrils gives greater tensile
strength compared to natural fibers and it has exceptionally large surface to volume
ratio compared to its bulk form [87].
The extraction of cotton nanocellulose can be carried out using mechanical
methods such as high-pressure homogenization, ball grinding, ultrasonication or
high-speed blending [88] or chemical methods using acid hydrolysis with strong
acids such as sulfuric acid or hydrochloric acid, oxidation with TEMPO (2,2,6,6-tet-
ramethylpyperidine-l-oxyl) [89] or a combination of both mechanical and chemical
methods [90]. It is found that acid hydrolysis removes the amorphous regions in
the cotton fiber and generates nanocellulose with high crystallinity and uniform
size distribution [89]. Sulfuric acid generates a more stable colloidal suspension
of cellulose nanocrystals [24] and is preferred to hydrochloric acid which causes
mass aggregation of cellulose nanocrystals because of the minimal surface charge
that causes a lack of electrostatic repulsion force between the crystal particles [91].
Also, the hazards of inorganic acids and their corrosive nature are detrimental to the
environment [92]. Mechanical processes generate nanofibers at a high success rate but
the strong mechanical shearing forces causes disruption of the fibers, depict exces-
sive energy consumption and homogenizer obstruction after prolonged use [88]. To
elude the shortcomings presented by both the mechanical and chemical processes
of nanocellulose extraction, pre-treatment with cellulase or enzymatic hydrolysis
has been considered. Enzymatic hydrolysis is an appropriate pretreatment method
used to disrupt interfibrillar cohesive forces and facilitate the disintegration of cotton
fibers, while decreasing the size and degree of polymerization of cellulose fibers
[93]. This method has been found to be highly selective and carried out at conditions
with lower energy requirements [14]. Additionally, it replaces harmful solvents with
biodegradable enzymes such as cellulases, which does not release hazardous emissions
to the environment [94]. Cellulose is comprised of highly ordered crystalline regions
interspersed with disorganized amorphous regions. The amorphous regions of
cellulose are more susceptible to enzymatic degradation compared to the crystalline
area. Cellulase enzyme has the potential of selective hydrolyzation of the amorphous
region while maintaining the crystalline region, making it a process of choice to iso-
late cellulose nanocrystals. Therefore, this route has become increasingly popular as
a sustainable method to prepare cellulose nanocrystals because of its high selectivity,
mild conditions, and weak changes in surface chemistry [93]. Moreover, it complies
with the principles of green chemistry as it leaves no carbon footprint, generates no
hazardous waste and poses less water and energy consumption [95].
The addition of nanocellulose extracted from cotton as a reinforcing agent to a
polymer system such as plastic, rubber or concrete improves the mechanical, thermo-
dynamic and adsorption properties of the composite without changing the original
qualities of the parent material [94]. Cotton fibers with a diameter in the range of
10–30 nm and a high aspect ratio are observed to improve the mechanical properties
in a polymer composite for non-food packaging applications [96]. These nanocom-
posites have been postulated to hold tremendous potential in biomedicine as scaffolds
in tissue engineering and for encapsulation in drug delivery [97]. The advances in
mammalian cell culture technology are astounding. Here, nanocomposite biopolymers
perform as biomimetic substrates for cell adhesion and proliferation. The nanotop-
ography of substrates constructed from biomolecules such as collagen which includes
9
Cotton

surface roughness and porosity, influences interface interaction with mammalian cells
or tissue that could improve cell adhesion and multiplication [98]. The incorporation
of nanomaterials into these polymer matrixes can yield composites with the necessary
properties for cell and tissue culture. Cotton based cellulose nanofibers (CCN) have a
tremendous potential to be engineered for polymer composite reinforcement [91] as it
mimics the structure of collagen in directionality and surface functionalization which
is paramount to the adhesion, spreading and proliferation of cells [99].
Translating cotton based nanocellulose into polymer nanocomposites can be car-
ried out using electrospinning, cast drying, freeze drying, vacuum assisted filtration,
wet spinning, layer by layer assembly, micropatterning, melt blending, intercalated
polymerization, sol-gel and solvent evaporation technique [100]. The solvent evapora-
tion technique is the simplest method for nanocomposite synthesis which involves
nanocellulose dispersion in polymer solution through energetic agitation followed by
controlled evaporation of the solvent and composite film casting [101]. Li et al., (2014)
prepared a nancomposite of cotton nanofiber in high density polyethylene (HDPE)
using 2 different pretreatment methods. The first was blending the HDPE in a cotton
CNF suspension, dehydrating and freeze drying the mixture followed by compound-
ing and extrusion. This was a rapid, eco-friendly method as there were no chemical
solvents involved in the process. In the second method, polyoxyethylene (PEO) was
used as a dispersion agent to coat the cotton CNF before adding to HDPE granules and
extraction. FESEM results revealed that both methods produced well dispersed CNF in
HDPE and generated an excellent network structure of the cotton CNF/HDPE com-
posites but the nanocomposite produced using the blending method was preferred as it
demonstrated greater bending strength (MOR) and bending modulus (MOE) [102].
Nanocomposites have several advantages over conventional composites in their
superior tensile strength, thermal capacity and barrier properties, biodegradability,
recyclability and low weight [103]. Insertion of nanocellulose to biodegradable poly-
mers to form bio-nanocomposites may improve the brittleness, poor barrier proper-
ties and low thermal stability of pure biodegradable polymers [104]. Much work has
been carried out in recent times to explore the design of bionanocomposites en route
to the development of higher quality bioplastics [105, 106].
A problem faced in generating cotton based cellulose nanocomposites is the
limited dispersion of nanocellulose in polymers. This can be overcome by attaching
a hydrophobic group to the surface of the cellulose matrix through esterification,
acetylation or silanization which increases compatibility with the matrix. Solution
casting is commonly used in the preparation of nanocomposite films but it its unsuit-
able for commercial scale production. Another method known as extrusion using
melt processing has shown much promise for large scale production of cotton based
cellulose nanocomposites [107]. However, for transforming research to industry and
commercialization of cotton based cellulose nanocomposites, it is necessary to weigh
the production costs, waste emissions, energy consumption, feasibility of the pro-
cess and compliance to environmental ethics. Overall, the application prospects for
nanocellulose appear to be very optimistic, but further research is needed to develop
viable methods from laboratory to industrialization.

4. Conclusion

Nanocomposites are defined as multi-element materials with at least one element

having a dimension of less than 100 nm [108]. In this chapter we have reviewed cotton
10
Cotton Based Cellulose Nanocomposites: Synthesis and Application
DOI: [Link]

based cellulose nanocomposites which are constructed by adding multifunctional

nanoparticles to the cotton fabric using in situ or ex situ processes or by extract-
ing nanocellulose structures from cotton fibers and incorporating it into polymer
matrices. This results in novel nanocomposites with enhanced antimicrobial activity,
polymer reinforcement and enhanced adhesion and adsorption in inert matrixes.
The introduction of metallic nanoparticles into cotton textiles has resulted in high
performance multifunctional cotton nanocomposites which demonstrate excellent
antimicrobial activity, water repellency, UV protection and antistatic finishes. These
nanocomposites are gaining much interest particularly in generating antimicrobial
material for protection against emerging pathogens. It is projected that further
research in nanocomposite technology would decipher the details of the functional
properties and performance of existing and emerging cotton nanocomposites and
to determine the toxicity and safety of the generated fabrics. Additionally, there is a
pressing need that the discoveries in the laboratory should be translated to commer-
cial applications through the design of fabrication processes that favor cost effective,
large scale production.
The incorporation of cotton nanocellulose into polymers as fillers to form rein-
forced nanocomposites also shows much promise particularly in the creation of
chemical and biodegradable polymers of increased strength and tensile modulus and
as scaffolds and support substrates in biomedicine. Yet there are issues that need to
be addressed prior to translation into commercial viability such as the influence of
the size and morphology of cotton nanocellulose fillers in the polymer matrix and the
structural compatibility of the resulting polymer, biocompatibility of the nanocom-
posites in biomedical applications and the poor dispersion of cotton nanocellulose in
the polymeric domain structure [109]. It is believed that these issues will be addressed
aggressively in the near future to pave the way for the birth of a new breed of nano-
composite material using cotton nanostructures.

Conflict of interest

The author declares no conflict of interest.

Author details

Patricia Jayshree Samuel Jacob

Nilai University, Nilai, Malaysia

*Address all correspondence to: patricia_jay@[Link]

© 2022 The Author(s). Licensee IntechOpen. This chapter is distributed under the terms of
the Creative Commons Attribution License ([Link]
which permits unrestricted use, distribution, and reproduction in any medium, provided
the original work is properly cited.
11
Cotton

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