Carbohydrate Polymers 241 (2020) 116227

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Carbohydrate Polymers
journal homepage: www.elsevier.com/locate/carbpol

Synthesis of cellulose microcrystals (CMC)/nylon 6,10 composite by T

incorporating CMC isolated from Pandanus ceylanicus
J.W.M.E.S. Weerappuliarachchia, I.C. Pererab, S.S. Gunathilakea,c, S.K.S. Thennakoonc,
B.S. Dassanayakea,d,*
a
Postgraduate Institute of Science, University of Peradeniya, Peradeniya, 20400, Sri Lanka
b
Department of Zoology and Environmental Sciences, Faculty of Science, University of Colombo, Colombo, Sri Lanka
c
Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya, 20400, Sri Lanka
d
Department of Physics, Faculty of Science, University of Peradeniya, Peradeniya, 20400, Sri Lanka

A R T I C LE I N FO A B S T R A C T

Keywords: The paper presents a novel candidate plant: Pandanus ceylanicus (PC) for cellulose extraction. The plant showed
Cellulose an average of 91.5 ± 0.2 % of cellulose yield which is the highest yield for Pandanus species reported. Cellulose
Cellulose microcrystals was extracted from the leaves of the plant by carrying out alkali and bleaching treatments, and cellulose mi-
Pandanus leaves crocrystals (CMC) were isolated from extracted cellulose fibers with sulphuric acid treatment. Chemical com-
Water absorption
position of PC leaves was investigated at different stages of treatment by using TAPPI standard methods. The
Nylon 6,10
extracted globular shaped CMC crystals had an average diameter less than a micro meter. Results revealed that
PC leaves are an efficient source of micro-cellulose which result in a high yield than most lignocellulosic bio-
masses. The CMCs were successfully incorporated with nylon 6,10 by in-situ interfacial polymerization of se-
bacoyl chloride and hexamethylenediamine in the presence of CMC. The CMC/nylon 6,10 composite showed
improved water absorption with low water retention time.

1. Introduction through β (1→4) – glycosidic bonds (Crawford, 1981). Most of the

During the last few decades, there has been a growing interest in the
field of materials science, since various biocomposites can be developed
through numerous chemical pathways with unique characteristics.
Recent research work has led to develop and progressively replace the
synthetic materials with biodegradable composites. As a result, lately
hybrid composites are fabricated by using natural fibers extracted from
eco-friendly lignocellulosic biomasses from different parts of the plants
(“Extraction of cellulose from pistachio shell and physical and me-
chanical characterisation of cellulose-based nanocomposites -
IOPscience,” n.d., Kampangkaew, Thongpin, &, Santawtee, 2014).
Throughout the world, there are countless number of plant sources
readily available with usable fibers. Due to their biodegradability, re-
newable nature (Varma et al., 1989) and low cost there has been
growing interest of their suitable applications in textile, paper manu-
facturing, bioenergy and medical industries.
The basic components of plant fibers are cellulose, hemicellulose
and lignin. Among them, cellulose is the fundamental constituent of the
fibers. Cellulose is an organic polysaccharide that consists of a linear
chain of hundreds to many thousands of D-glucose units that condense
physical, and chemical properties of cellulose, including high tensile
strength, chemical inertness, biodegradability, non-toxicity and re-
newable nature, depend on its chain length or the degree of poly-
merization (Hon, 1994). As the size of the cellulose fibers goes down,
they tend to possess additional properties such as high aspect ratio,
lightweight, high elastic modulus, large specific surface area, non-
abrasive nature and unique photonic characteristics. Therefore, micro-
and nano-sized cellulose crystals, obtained from the fibers have gained
an immense popularity in the fields of biodegradable materials research
and manufacturing fields.
The cellulose microcrystals (CMC) are generated by the removal of
amorphous regions of purified cellulose fibers by acid hydrolysis. CMCs
are rigid in structure with very limited flexibility, as they do not contain
amorphous regions, but instead exhibit crystalline shapes (Owolabi, Sri,
Megat-Yusoff, & Hamizol, n.d.). The crystals can be isolated from var-
ious lignocellulosic biomasses such as banana (Deepa et al., 2011),
cotton (Sun et al., 2007), pineapple leaves (Cherian et al., 2010), Ses-
bania javanica stems (Kampangkaew et al., 2014), rice husk (Rosa et al.,
2012), grass (Bhattacharya et al., 2008), pandanus spp. (Chenampulli
et al., 2013; Owolabi et al., n.d.; Teli & Jadhav, 2015) etc. The

⁎
Corresponding author at: Department of Physics, Faculty of Science, University of Peradeniya, Peradeniya, 20400, Sri Lanka.
E-mail address: buddhikad@pdn.ac.lk (B.S. Dassanayake).

https://doi.org/10.1016/j.carbpol.2020.116227
Received 7 December 2019; Received in revised form 26 March 2020; Accepted 26 March 2020
0144-8617/ © 2020 Elsevier Ltd. All rights reserved.
J.W.M.E.S. Weerappuliarachchi, et al.
fibrillation processes has been designed to remove hemicellulose,
lignin, and pectin, as cellulose is embedded as a matrix along with these
components in plant cell walls (North Carolina State University,
Department of Wood and Paper Science, 2008). In this paper, we pre-
sent a fibrillation process which is designed to isolate CMC as a sus-
pension. The suspension of CMC showed high durability. If necessary, it
can be freeze dried for long term saving and it can easily be re-sus-
pended.
Pandanaceae family possess more than 600 known species in which
Pandanus ceylanicus (screw pines) is an endemic plant to Sri Lanka
(“Ayurvedic Plants of Sri Lanka: Plants Details”, n.d.). It is a monocot
species, and a prostrate shrub which can grow to a height of 4−5 m.
The plants are frequently identified growing merely inland from the sea
or wet areas and along streams or riverbanks. In this study, an attempt
has been made to carefully investigate the fundamental properties of PC
fibers and to obtained cellulose crystals from the extracted cellulose
fibers by implementing a series of chemical treatments. Among afore-
mentioned biomasses, PC leaves are locally available, relatively low
cost and have been used traditionally for extracting fibers and making
mats and ropes due to their remarkable strength.
A thorough literature survey revealed that no significant work has
yet been reported in isolating cellulose nanofibers from Pandanus cey-
lanicus (PC). According to reported work, Pandanus tectorius (Owolabi
et al., 2020), Pandanus utilis (Chenampulli et al., 2013) pandanus
amaryllifolius (Yahida Yahya & Ngadi, 2014) and Pandanus odorifer (Teli
& Jadhav, 2015) has been used for the isolation of CMC. Being a locally
abundant plant with a considerable amount of fiber in its leaves, P.
ceylanicus is an ideal candidate for isolation of CMC. Since the extrac-
tion should be unique and fitting to the plant, typical extraction con-
ditions has been optimized to suit PC. The method of extraction, when
compared with the leading retting methods that are currently in use, is
less time consuming, low cost and convenient. The intent of this work is
to optimize the typical CMC extraction, as contest with PC leaves and
use isolated CMC to prepare an advanced polymer composite by in-
corporating it with nylon 6,10. For the best of the knowledge of the
authors, this is the first time CMC isolated from Pandanus ceylanicus is
incorporated with nylon 6,10 fibers.
Unlike most of the current extraction methods, the method reported
here starts directly from alkali treatment followed by the steam ex-
plosion, which helps to shorten the length of the procedure. The typical
extraction process has three main steps; alkali treatment, bleaching,
and acid hydrolysis. Alkali and bleaching steps are purifying treat-
ments, which eliminate non-cellulosic components such as hemi-
cellulose, pectin and lignin from the matrix (Chenampulli et al., 2013;
Hamad, 2008). Acid hydrolysis is an efficient and easy way to cleave
the amorphous regions in cellulose chains to produce microcrystalline
cellulose (Hamad, 2008). Previous researches have explained sulfuric
acid as the most effective type of acid, since the introduction of charged
sulphate groups stabilizes the suspension (Beck-Candanedo et al.,
2005). However, based on the plant type and environmental conditions,
it is very crucial to optimize the acid concentration, temperature and
reaction time, since they are critical parameters which affect the par-
ticle/fiber size and extraction efficiency. The reporting optimized
methodology has a low optimum temperature of 121 °C in the alkali
treatment as well as only 3 repeating steps in bleaching process using a
low concentration of bleaching agent. Additionally, the experiment
introduces sodium hypochlorite as bleaching agent rather than using
sodium chlorite reported in pervious extraction processes (Teli &
Jadhav, 2015). Sulfuric acid was selected as the hydrolyzing agent for
the acid hydrolysis step (Chenampulli et al., 2013), however, the ef-
fective concentration of the acid was reduced to 10 %, which is the
lowest reported acid amount used for the extraction process of Pan-
danus species. The aforementioned experimental conditions are unique
to the composition of PC leaves which was optimized until crystals were
obtained from cellulose fibers.
As the polymer material nylon was selected because of nylon’s
2
Carbohydrate Polymers 241 (2020) 116227
versatility and it is one of the most widely used engineering thermo-
plastics. Among other nylon types, nylon 6,10 has high strength and it
can be prepared by using simple chemical methods under relatively low
cost. Nevertheless, it has good resistance to most solvents and to dilute
mineral acids. It also resists the environmental stress cracking action of
salts such as zinc chloride (“Characterization and Failure Analysis of
Plastics - ASM International, Steve Lampman - Google Books, ” n.d.).
However, nylon 6,10 has very low moisture absorption which limits its
applications. The reported CMC/nylon 6,10 composite in this study has
a porous structure with a high water absorption capacity, which make it
a potential material for applications such as wound dressings in the
medical industry. Additionally, CMC provides biodegradability (Siró &
Plackett, 2010) to the nylon 6,10 fibers, hence it is possible to manu-
facture an environmentally friendly composite at a relatively low cost.
Since the selected lignocellulosic biomass is readily available in the
country at a considerably low cost and which the leaves have not a big
commercial value yet, this work will create a platform to get more
advantages from high cellulose content available in the P. celanicus
leaves.
2. Experimental design
2.1. Casting materials and chemicals
The chemical reagents of analytical grade such as 97 % sodium
hydroxide (NaOH), 99 % acetic acid (CH3COOH) and 98 % sulfuric acid
(H2SO4) were purchased from Sigma-Aldrich and 5.65–6 % Sodium
hypochlorite (NaOCl) was purchased from Fischer scientific, UK. All the
chemicals were used without further purification.
2.2. Plant material
Pandanus ceylanicus (PC) leaves were collected from Royal Botanical
Gardens, Peradeniya, Sri Lanka. The spiny margins and midribs of the
leaves were removed, after which the leaves were washed in running
water, air dried and stored at room temperature (30 °C).
2.3. Experimental
2.3.1. Step 1: alkali treatment followed by steam explosion
The PC leaves obtained after air drying were chopped into uniform
size of approximately 1−2 cm. They were soaked in a 1000 cm3 of 5 %
NaOH solution (1:10 g/ml, fiber: liquor ratio) and placed for 72 h under
a temperature of 30 °C. The steam explosion technique was applied
according to the method in Abraham et al. (2011). A laboratory auto-
clave which can work with 137 Pa pressure was used for steam explo-
sion. The mercerized was washed with deionized (DI) water until the
solution became pH neutral.
2.3.2. Step 2: bleaching treatment (delignification)
The resulted insoluble residue was then subjected to bleaching with
an acidified (pH 2) sodium hypochlorite solution (5 %, 1:15 g/ml) at
70 °C for 1 h. The process was repeated three times until the mass be-
came visually white in color. The step was performed to remove lignin.
The cellulose pulp was neutralized with NaOH solution and thoroughly
washed with DI water. The resulted pulp was dried in a vacuum oven at
60 °C.
2.3.3. Step 3: acid hydrolysis
The bleached pulp was then subjected to acid treatment with 10 %
acid solution (1:60 g/ml, cellulose pulp: sulfuric acid) while mechani-
cally stirring at 60 °C for 5 h. The hydrolysate then subjected to soni-
cation. Finally, it was neutralized by NaOH solution. The resulting
aqueous suspension was preserved for further characterization.
J.W.M.E.S. Weerappuliarachchi, et al.
2.3.4. Step 4: preparation of nylon 6,10 and CMC/nylon 6,10 composite
Sebacoyl chloride (0.60 g) in hexane (7.00 ml) and hexamethyle-
nediamine (0.30 g) and NaOH (0.20 g) in DI water (7.00 ml) were
gently mixed in order to prepare the pure nylon 6,10 fiber. NaOH was
added to the aqueous layer along with hexamethylenediamine in order
to facilitate the polymerization reaction by neutralizing the HCl formed
during the reaction. The thread was pulled slowly using a kymograph as
a spool, to get a thread with an even diameter. The synthesized nylon
thread was washed thoroughly using distilled water and air dried.
CMC/Nylon 6,10 composite was prepared by in-situ polymerization
of sebacoyl chloride and hexamethylenediamine in the presence of CMC
in the aqueous phase. For that, 3.50 ml of CMC suspension and 3.50 ml
of DI water was used to dissolve hexamethylenediamine during the
preparation process and it was used as the aqueous phase. This was
gently mixed with sebacoyl chloride dissolved in hexane and the
composite formed at the interface was slowly pulled out as a thread.
2.4. Characterization
2.4.1. Scanning electron microscopy (SEM)
The surface morphology of PC leaf fibers at different stages of
treatments as well as the surface of CMC incorporated nylon fibers were
observed using a Zeiss EVOLS 15 scanning electron microscope under a
beam current of 30 μA. Prior to SEM imaging, a fine layer of gold was
deposited on samples by means of plasma sputtering.
2.4.2. CMC yield
The yield of CMC isolated from the PC leaves were calculated using
the following formula.
Weight of dried cellulose (g )
Cellulose yield (%) =
Weight of raw fiber used for extraction (g ) (1)
2.4.3. X-ray diffraction (XRD)
The crystallinity of leaves at different stages of extraction was stu-
died using grazing incidence X-ray diffraction (GIXRD) PANalytical
diffractometer (model Empyrean) with CuKα (λ = 1.541 Å) radiation
as the diffracted monochromatic beam at 40 kV in 40 mA tube current.
The diffraction pattern was scanned at 0.02° scan step size with step
time of 2 min and 2θ in the range of 2°–70°.
The empirical method in Segal et al. (1959) was used to obtain the
crystallinity index (XC) of the samples using the following equation (Eq.
(2)).
IC − Iam
XC = × 100
IC (2)
where, Ic is the counter reading at peak intensity at a 2θ angle close to
22° and Iam is the counter reading at peak intensity at a 2θ angle close to
16° representing amorphous materials in cellulose fibers.
2.4.4. Chemical characterization
The chemical composition of PC leaves before and after chemical
treatments was investigated. The lignin (acid-insoluble) and α-cellulose
content were determined according to TAPPI standard methods T-223
and T-203, respectively.
2.4.5. Fourier transform infrared spectroscopy (FTIR)
FTIR spectroscopy was employed to examine the changes in the
chemical composition of the leaves after chemical treatment by using IR
Prestige-21 (SHIMADZU) FTIR spectrophotometer using ATR sampling
technique by recording 45 scans in transmittance mode in the range of
4000−500 cm−1. The untreated Pandanus leaves, alkali treated sample
and bleached cellulose samples were analyzed using FTIR.
2.4.6. Water absorption
Known amount of pre-weighted dry pure nylon and CMC/nylon
3
Carbohydrate Polymers 241 (2020) 116227
Table 1
Chemical composition of Pandanus leaves at different stages of treatment.
Sample Cellulose (%) Lignin (%)
Pandanus raw leaves 32.8 ( ± 0.5) 12.5 ( ± 0.1)
After alkali treatment 57.8 ( ± 0.4) 0.56 ( ± 0.1)
After bleaching 91.5 ( ± 0.2) 0
6,10 samples were placed in a 50.0 ml of DI water beakers separately at
room temperature and allowed to absorb water for 24 h. After 24 h, the
water remaining on the surface of the samples was wiped out and the
mass measurements were taken periodically until the fibers reached the
initial dry weight. Using the above-mentioned readings, the water re-
tention time of pure nylon and CMC/nylon 6,10 composite was calcu-
lated.
3. Results and discussion
Alkali treatment of the raw leaves removes the hemicelluloses, some
lignin, and wax cover of the external surface of leaves, thereby affecting
the chemical composition of the fibers. The steam explosion treatment
causes a sudden pressure drop, disrupting the fiber bundles. The main
goal of the bleaching step is to remove the remaining cement material
or lignin (Cherian et al., 2010). Hemicellulose is a water-soluble poly-
saccharide, and lignin is a complex organic compound with alkali so-
luble character. Therefore, percentage of lignin decreases from raw
leaves to bleached fibers during the alkali treatment as seen in Table 1.
The bleaching process depends on pH of the medium and temperature.
Hence, the reaction was carried out at a low pH and a high temperature.
Conditions were optimized until it gave the best yield in minimum acid
concentration under the shortest period of time.
3.1. Chemical composition
Table 1 shows the chemical composition of the three studied sam-
ples at different processing stages of treatment. Results reveal that the
PC is ideal for cellulose extraction, since the fibers were found to
contain 91.5 % of cellulose after the beaching step. This value is rela-
tively higher than the value recorded for other Pandanus species
(Sheltami et al., 2012). In accordance with the results, the fibers also
contained a low amount of lignin. Confirming that lignin has alkali
soluble character, percentage of lignin was found to reduce after alkali
treatment. The remaining amount reacts with NaOCl and can be dis-
solved out as lignin chloride during the bleaching step. Hence, the
chemical composition revealed the purification of cellulose, and the
resulted sample was exposed to acid hydrolysis to produce CMC. Pre-
vious researchers have reported that, acid hydrolysis leads to hydrolytic
cleavage of the glycosidic bonds between the two anhydroglucose units
of cellulose (Chenampulli et al., 2013). The resulted suspension was
later sonicated to disintegrate the cellulose structure into micro-
crystalline forms. It provided high turbulence and shear while reducing
the size.
3.2. Morphological analysis
Fig. 1(a)–(d) shows the photographs of P. celanicus plant and its
leaves at different stages of treatment. The color of the leaves changed
from green to light brown after alkali treatment and became white after
bleaching. SEM images of raw ground Pandanus leaves and their pro-
ducts at different stages of extraction (alkali treatment and bleaching)
are shown in Fig. 2(a)–(c). The diameters of the fibers in the raw leaves
were found to be in the range of 400–600 μm, and the image clearly
shows dermal tissues of the raw leaves. The image depicts that the fi-
bers in the original leaves were bound together by cement components,
which has partially diminished after the alkali treatment as seen in
J.W.M.E.S. Weerappuliarachchi, et al. Carbohydrate Polymers 241 (2020) 116227

Fig. 1. Photographs of (a) the P. celanicus plant (b) raw leaves (c) alkali treated sample and (d) bleached sample.

Fig. 2-(b). Furthermore, the alkali treatment seems to remove the ex- which acts as a cementing material and forms a bridging bond with
tractives from the leaves, justified by the surface change undergone as cellulose. However, under strong bleaching conditions, the binding
seen in Fig. 2-(b). However, it can also be seen that it did not lead to materials were eliminated, and defibrillated cellulose bundles were
free cellulose from the binding material. This is due to residual lignin seen as in Fig. 2-(c). Hence, the fiber diameters were found to decrease,

Fig. 2. SEM images of (a) raw ground leaves, (b) alkali treated leaves, and (c) bleached leave.

4
J.W.M.E.S. Weerappuliarachchi, et al.
Fig. 3. The aquous suspension of CMC.
increasing the aspect ratio. The network structure was further de-
stroyed by removing amorphous cellulose through acid hydrolysis.
Fig. 3 shows the final slurry obtained after the sonication. The
isolated CMC were suspended in the liquid and the slurry was freeze
dried in order to calculate the percentage yield of the CMC.
3.3. CMC yeild
According to the calculations (Eq. (1)), the average percentage yield
of CMC is 39.4 % which is higher than the percentage yield obtained
from banana, rachis, sisal, kapok, and coir, etc (Deepa et al., 2015).
3.4. X-ray diffraction measurments
The XRD analysis of the alkali treated fibers also revealed an in-
crease in the crystallinity during the process of converting PC leaves to
CMC. Both intra- and inter-molecular hydrogen bonding occur in cel-
lulose via hydroxyl groups, which results in various ordered crystalline
arrangements (Sheltami et al., 2012). Fig. 4 shows the XRD patterns for
Pandanus at different stages of treatment. The XRD graph obtained for
Pandanus ceylanicus is similar to the XRD pattern obtained for the
Pandanus odorifer according to the Teli and Jadhav (2015). The major
intensity peak is located at a 2θ value of around 22.6°, which is related
to the crystalline structure of cellulose I for all samples, whilst the
amorphous background is characterized by the low diffracted intensity
at a 2θ value of around 16.0° (Teli & Jadhav, 2015).
Crystallinity indices of raw leaves, alkali-treated leaves and
bleached leaves were found to be 63.5 %, 68.3 %, and 78.4 %
Fig. 4. XRD patterns of the P. celanicus leaves at different stages of treatments.
5
Carbohydrate Polymers 241 (2020) 116227
respectively. These results clearly demonstrate that the crystallinity of
the material has progressively increased during the chemical treat-
ments. These crystallinity indices of the samples are higher than the
values reported for other pandanus species (Chenampulli et al., 2013;
Teli & Jadhav, 2015). Moreover, it can also be seen that the diffraction
peak around 22.6° has become shaper upon chemical treatment. This
observation could be a result of better-defined crystalline domains.
Additionally, another visible peak is found around 31.0°, which might
be due to unique structural arrangement in Pandanus fibers and the
peak is prominent in the spectrum of raw fibers.
3.5. FTIR spectroscopy analysis
Fig. 5 shows the FTIR spectra obtained for PC leaves at different
stages of the treatment. The band located at 1734 cm−1 in the spectrum
of raw leaves is attributed to the C]O stretching of the acetyl and
uronic ester groups of hemicellulose or the ester linkage of carboxylic
groups of ferulic and p-coumaric acids of lignin and/or hemicellulose.
The disappearance of this band after the alkali and subsequent
bleaching treatments could have been caused by the removal of hemi-
cellulose and lignin from P. celanicus leave fibers during the chemical
treatment. For Pandanus ceylanicus, the lignin amount is significantly
low as can be seen in Table 1. Hence, the corresponding absorption
peak is not prominent. However, this peak disappears after bleaching,
indicating the removal of lignin (Sun et al., 2005).The absorbance peak
which appears in the frequency interval 1600–1650 cm−1 is found to
decrease from raw fibers to bleached fibers. The intensity of this peak
which is corresponding to C]C stretching decreases with alkali treat-
ment since aromatic lignin is being removed by this process. Similar
results have been reported for banana (“Treatment of banana fiber for
use in the reinforcement of polymeric matrices,” 2013), date palm tree
fibers (Alawar et al., 2009), hemp and kneaf tree fibers (Sgriccia et al.,
2008), upon the alkali treatment with NaOH. The peak around
2900 cm−1 originate from the asymmetric stretching vibration of C ̶ H
group. The peaks in the 3400–3300 cm−1 region can be assigned to the
adsorbed water, and the band around 1060 cm−1 relates to the C ̶ O
stretching of the carbohydrates. These different bands can be seen in all
spectra, regardless of the purification of the fibers (Sofla et al., 2016).
The CeC single bond appears at 920−870 cm-1 and the peaks appeared
in between 1400−1450 cm−1 are attributed to the deformation of C–H
in the CH3 (“Treatment of banana fiber for use in the reinforcement of
polymeric matrices,” 2013). In addition, the band at 1052 cm−1 is re-
ferred to the CeOeC pyranose ring skeletal vibrations (Lan et al.,
2011).
3.6. Water absorption
After the successful extraction of CMC, it was incorporated with
nylon 6, 10 by using the aforementioned method in experimental sec-
tion. The SEM images from CMC on the surface of nylon fibers are
presented in Fig. 6. As seen in Fig. 6(a), pure nylon 6, 10 depicts a
smoother and clearer surface compared to CMC/Nylon 6,10 composite
sample as shown in Fig. 6(b). This confirms the incorporation of micro
structures into the treated fibers. The average size of the crystals was
estimated to be 0.8–0.9 μm using the SEM images. The SEM image re-
veals that, CMC have been adhered to the surface of the nylon during
the incorporation. Further, the composite was washed three times using
distilled water before the SEM images were taken, to wash away the
loosely attached CMC to Nylon 6,10. Additionally, it was also confirmed
that the final composite is pH neutral, considering the potential use of
the composite as a raw material for wound dressings.
Water absorption behavior of micro- and nanocellulose crystals is
complex and different to that of the normal cellulose. It has been proven
that the structure and composition are important for the water ab-
sorption (Wang, Kalinichev, & Kirkpatrick, n.d.). However, due to the
complexity of understanding the water absorption by nylon/CMC
J.W.M.E.S. Weerappuliarachchi, et al. Carbohydrate Polymers 241 (2020) 116227

Fig. 5. FTIR spectrum of the P. celanicus leaves at different stages of treatments.

composite, it has not been studied as much as it should be (Haafiz et al.,

2013). To the best of the authors knowledge, this is the first study to
report the preparation of CMC incorporated nylon 6,10 and investiga-
tion of their water absorption. The CMC/nylon 6,10 showed improve-
ment of water absorption than pure nylon. Since each cellulose unit has
three free ̶ OH groups, the moisture absorption rate can increase with
the incorporation of CMC into nylon 6,10.
Further, it was noted that, the water retention time of CMC/Nylon
6,10 is significantly lower than pure nylon fibers. According to Fig. 7, it
can be seen that after 48 h, CMC/nylon 6,10 was dried completely
while pure nylon did not. This creates a potential application as a
wound dressing of CMC/nylon 6,10 composite fibers. As it has low
adherence with the wound it allows exudate to pass through while
maintaining moist in the wound bed. Further, after drying, the com-
posite can easily be removed from the skin without sticking to the skin/
wound. This kind of applications are particularly useful for patients
with sensitive or fragile skin (Jones et al., 2006).

4. Conclusion
This work presents a method which breaks the usual biological
natural retting process in isolating fibers from plant materials, which
could be an economically feasible approach of extracting CMC.
Cellulose from P. ceylanicus was successfully extracted using a simple
method and cellulose crystals were prepared from the extracted cellu-
lose fibers. The chemical composition further attests satisfactory
Fig. 7. Water absorption and water retention time of pure nylon, and CMC
incorporated nylon 6,10.
cellulose content for commercial extraction at low cost. The bleaching
and hydrolysis steps were optimized in accordance to plant material
while using the lowest possible acid amounts. The extraction process

Fig. 6. The surface morphology of (a) pure nylon and (b) CMC incorporated nylon.

6
J.W.M.E.S. Weerappuliarachchi, et al.
produced CMC with a diameter of about 0.8-0.9 μm. Hence, it can be
concluded that steam explosion combined with acid hydrolysis can be
successfully used in obtaining cellulose crystals in the micro dimension
from PC leaves. Out of other lignocellulosic biomasses available in Sri
Lanka, P. ceylanicus becomes a potential candidate for mass extraction
of CMC. CMC/nylon 6,10 fibers were successfully synthesized and the
composite showed improved water absorption and fast drying com-
pared to pure nylon. This feature makes the composite ideal to be used
as a raw material to prepare wound dressings with improved properties.
Research data
The datasets generated during and analyzed during the current
study are available from the corresponding author on reasonable re-
quest.
Conflict of interest statement
The authors declare that there is no conflict of interest.
CRediT authorship contribution statement
J.W.M.E.S. Weerappuliarachchi: Conceptualization,
Methodology, Formal analysis, Investigation, Writing - original draft.
I.C. Perera: Conceptualization, Resources, Writing - review & editing,
Supervision. S.S. Gunathilake: Conceptualization, Resources,
Supervision. S.K.S. Thennakoon: Formal analysis. B.S. Dassanayake:
Conceptualization, Formal analysis, Resources, Writing - review &
editing, Supervision, Project administration, Funding acquisition.
Acknowledgement
The authors are grateful to the Royal Botanical Garden, Peradeniya,
Sri Lanka. And sincerely acknowledge Department of Botany, Faculty of
Science, and University of Peradeniya, Sri Lanka.
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