2020 - Weerappuliarachchi Et Al 2020 Carbohydrate Polymers
2020 - Weerappuliarachchi Et Al 2020 Carbohydrate Polymers
2020 - Weerappuliarachchi Et Al 2020 Carbohydrate Polymers
Carbohydrate Polymers
journal homepage: www.elsevier.com/locate/carbpol
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.
⁎
Corresponding author at: Department of Physics, Faculty of Science, University of Peradeniya, Peradeniya, 20400, Sri Lanka.
E-mail address: [email protected] (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. Carbohydrate Polymers 241 (2020) 116227
fibrillation processes has been designed to remove hemicellulose, versatility and it is one of the most widely used engineering thermo-
lignin, and pectin, as cellulose is embedded as a matrix along with these plastics. Among other nylon types, nylon 6,10 has high strength and it
components in plant cell walls (North Carolina State University, can be prepared by using simple chemical methods under relatively low
Department of Wood and Paper Science, 2008). In this paper, we pre- cost. Nevertheless, it has good resistance to most solvents and to dilute
sent a fibrillation process which is designed to isolate CMC as a sus- mineral acids. It also resists the environmental stress cracking action of
pension. The suspension of CMC showed high durability. If necessary, it salts such as zinc chloride (“Characterization and Failure Analysis of
can be freeze dried for long term saving and it can easily be re-sus- Plastics - ASM International, Steve Lampman - Google Books, ” n.d.).
pended. However, nylon 6,10 has very low moisture absorption which limits its
Pandanaceae family possess more than 600 known species in which applications. The reported CMC/nylon 6,10 composite in this study has
Pandanus ceylanicus (screw pines) is an endemic plant to Sri Lanka a porous structure with a high water absorption capacity, which make it
(“Ayurvedic Plants of Sri Lanka: Plants Details”, n.d.). It is a monocot a potential material for applications such as wound dressings in the
species, and a prostrate shrub which can grow to a height of 4−5 m. medical industry. Additionally, CMC provides biodegradability (Siró &
The plants are frequently identified growing merely inland from the sea Plackett, 2010) to the nylon 6,10 fibers, hence it is possible to manu-
or wet areas and along streams or riverbanks. In this study, an attempt facture an environmentally friendly composite at a relatively low cost.
has been made to carefully investigate the fundamental properties of PC Since the selected lignocellulosic biomass is readily available in the
fibers and to obtained cellulose crystals from the extracted cellulose country at a considerably low cost and which the leaves have not a big
fibers by implementing a series of chemical treatments. Among afore- commercial value yet, this work will create a platform to get more
mentioned biomasses, PC leaves are locally available, relatively low advantages from high cellulose content available in the P. celanicus
cost and have been used traditionally for extracting fibers and making leaves.
mats and ropes due to their remarkable strength.
A thorough literature survey revealed that no significant work has
2. Experimental design
yet been reported in isolating cellulose nanofibers from Pandanus cey-
lanicus (PC). According to reported work, Pandanus tectorius (Owolabi
2.1. Casting materials and chemicals
et al., 2020), Pandanus utilis (Chenampulli et al., 2013) pandanus
amaryllifolius (Yahida Yahya & Ngadi, 2014) and Pandanus odorifer (Teli
The chemical reagents of analytical grade such as 97 % sodium
& Jadhav, 2015) has been used for the isolation of CMC. Being a locally
hydroxide (NaOH), 99 % acetic acid (CH3COOH) and 98 % sulfuric acid
abundant plant with a considerable amount of fiber in its leaves, P.
(H2SO4) were purchased from Sigma-Aldrich and 5.65–6 % Sodium
ceylanicus is an ideal candidate for isolation of CMC. Since the extrac-
hypochlorite (NaOCl) was purchased from Fischer scientific, UK. All the
tion should be unique and fitting to the plant, typical extraction con-
chemicals were used without further purification.
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 2.2. Plant material
to optimize the typical CMC extraction, as contest with PC leaves and
use isolated CMC to prepare an advanced polymer composite by in- Pandanus ceylanicus (PC) leaves were collected from Royal Botanical
corporating it with nylon 6,10. For the best of the knowledge of the Gardens, Peradeniya, Sri Lanka. The spiny margins and midribs of the
authors, this is the first time CMC isolated from Pandanus ceylanicus is leaves were removed, after which the leaves were washed in running
incorporated with nylon 6,10 fibers. water, air dried and stored at room temperature (30 °C).
Unlike most of the current extraction methods, the method reported
here starts directly from alkali treatment followed by the steam ex- 2.3. Experimental
plosion, which helps to shorten the length of the procedure. The typical
extraction process has three main steps; alkali treatment, bleaching, 2.3.1. Step 1: alkali treatment followed by steam explosion
and acid hydrolysis. Alkali and bleaching steps are purifying treat- The PC leaves obtained after air drying were chopped into uniform
ments, which eliminate non-cellulosic components such as hemi- size of approximately 1−2 cm. They were soaked in a 1000 cm3 of 5 %
cellulose, pectin and lignin from the matrix (Chenampulli et al., 2013; NaOH solution (1:10 g/ml, fiber: liquor ratio) and placed for 72 h under
Hamad, 2008). Acid hydrolysis is an efficient and easy way to cleave a temperature of 30 °C. The steam explosion technique was applied
the amorphous regions in cellulose chains to produce microcrystalline according to the method in Abraham et al. (2011). A laboratory auto-
cellulose (Hamad, 2008). Previous researches have explained sulfuric clave which can work with 137 Pa pressure was used for steam explo-
acid as the most effective type of acid, since the introduction of charged sion. The mercerized was washed with deionized (DI) water until the
sulphate groups stabilizes the suspension (Beck-Candanedo et al., solution became pH neutral.
2005). However, based on the plant type and environmental conditions,
it is very crucial to optimize the acid concentration, temperature and
2.3.2. Step 2: bleaching treatment (delignification)
reaction time, since they are critical parameters which affect the par-
The resulted insoluble residue was then subjected to bleaching with
ticle/fiber size and extraction efficiency. The reporting optimized
an acidified (pH 2) sodium hypochlorite solution (5 %, 1:15 g/ml) at
methodology has a low optimum temperature of 121 °C in the alkali
70 °C for 1 h. The process was repeated three times until the mass be-
treatment as well as only 3 repeating steps in bleaching process using a
came visually white in color. The step was performed to remove lignin.
low concentration of bleaching agent. Additionally, the experiment
The cellulose pulp was neutralized with NaOH solution and thoroughly
introduces sodium hypochlorite as bleaching agent rather than using
washed with DI water. The resulted pulp was dried in a vacuum oven at
sodium chlorite reported in pervious extraction processes (Teli &
60 °C.
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 2.3.3. Step 3: acid hydrolysis
lowest reported acid amount used for the extraction process of Pan- The bleached pulp was then subjected to acid treatment with 10 %
danus species. The aforementioned experimental conditions are unique acid solution (1:60 g/ml, cellulose pulp: sulfuric acid) while mechani-
to the composition of PC leaves which was optimized until crystals were cally stirring at 60 °C for 5 h. The hydrolysate then subjected to soni-
obtained from cellulose fibers. cation. Finally, it was neutralized by NaOH solution. The resulting
As the polymer material nylon was selected because of nylon’s aqueous suspension was preserved for further characterization.
2
J.W.M.E.S. Weerappuliarachchi, et al. Carbohydrate Polymers 241 (2020) 116227
2.3.4. Step 4: preparation of nylon 6,10 and CMC/nylon 6,10 composite Table 1
Sebacoyl chloride (0.60 g) in hexane (7.00 ml) and hexamethyle- Chemical composition of Pandanus leaves at different stages of treatment.
nediamine (0.30 g) and NaOH (0.20 g) in DI water (7.00 ml) were Sample Cellulose (%) Lignin (%)
gently mixed in order to prepare the pure nylon 6,10 fiber. NaOH was
added to the aqueous layer along with hexamethylenediamine in order Pandanus raw leaves 32.8 ( ± 0.5) 12.5 ( ± 0.1)
After alkali treatment 57.8 ( ± 0.4) 0.56 ( ± 0.1)
to facilitate the polymerization reaction by neutralizing the HCl formed
After bleaching 91.5 ( ± 0.2) 0
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. 6,10 samples were placed in a 50.0 ml of DI water beakers separately at
CMC/Nylon 6,10 composite was prepared by in-situ polymerization room temperature and allowed to absorb water for 24 h. After 24 h, the
of sebacoyl chloride and hexamethylenediamine in the presence of CMC water remaining on the surface of the samples was wiped out and the
in the aqueous phase. For that, 3.50 ml of CMC suspension and 3.50 ml mass measurements were taken periodically until the fibers reached the
of DI water was used to dissolve hexamethylenediamine during the initial dry weight. Using the above-mentioned readings, the water re-
preparation process and it was used as the aqueous phase. This was tention time of pure nylon and CMC/nylon 6,10 composite was calcu-
gently mixed with sebacoyl chloride dissolved in hexane and the lated.
composite formed at the interface was slowly pulled out as a thread.
3. Results and discussion
2.4. Characterization
Alkali treatment of the raw leaves removes the hemicelluloses, some
2.4.1. Scanning electron microscopy (SEM)
lignin, and wax cover of the external surface of leaves, thereby affecting
The surface morphology of PC leaf fibers at different stages of
the chemical composition of the fibers. The steam explosion treatment
treatments as well as the surface of CMC incorporated nylon fibers were
causes a sudden pressure drop, disrupting the fiber bundles. The main
observed using a Zeiss EVOLS 15 scanning electron microscope under a
goal of the bleaching step is to remove the remaining cement material
beam current of 30 μA. Prior to SEM imaging, a fine layer of gold was
or lignin (Cherian et al., 2010). Hemicellulose is a water-soluble poly-
deposited on samples by means of plasma sputtering.
saccharide, and lignin is a complex organic compound with alkali so-
luble character. Therefore, percentage of lignin decreases from raw
2.4.2. CMC yield
leaves to bleached fibers during the alkali treatment as seen in Table 1.
The yield of CMC isolated from the PC leaves were calculated using
The bleaching process depends on pH of the medium and temperature.
the following formula.
Hence, the reaction was carried out at a low pH and a high temperature.
Weight of dried cellulose (g ) Conditions were optimized until it gave the best yield in minimum acid
Cellulose yield (%) =
Weight of raw fiber used for extraction (g ) (1) concentration under the shortest period of time.
2.4.5. Fourier transform infrared spectroscopy (FTIR) Fig. 1(a)–(d) shows the photographs of P. celanicus plant and its
FTIR spectroscopy was employed to examine the changes in the leaves at different stages of treatment. The color of the leaves changed
chemical composition of the leaves after chemical treatment by using IR from green to light brown after alkali treatment and became white after
Prestige-21 (SHIMADZU) FTIR spectrophotometer using ATR sampling bleaching. SEM images of raw ground Pandanus leaves and their pro-
technique by recording 45 scans in transmittance mode in the range of ducts at different stages of extraction (alkali treatment and bleaching)
4000−500 cm−1. The untreated Pandanus leaves, alkali treated sample are shown in Fig. 2(a)–(c). The diameters of the fibers in the raw leaves
and bleached cellulose samples were analyzed using FTIR. 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-
2.4.6. Water absorption bers in the original leaves were bound together by cement components,
Known amount of pre-weighted dry pure nylon and CMC/nylon which has partially diminished after the alkali treatment as seen in
3
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.
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J.W.M.E.S. Weerappuliarachchi, et al. Carbohydrate Polymers 241 (2020) 116227
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J.W.M.E.S. Weerappuliarachchi, et al. Carbohydrate Polymers 241 (2020) 116227
4. Conclusion
Fig. 7. Water absorption and water retention time of pure nylon, and CMC
This work presents a method which breaks the usual biological incorporated nylon 6,10.
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 cellulose content for commercial extraction at low cost. The bleaching
method and cellulose crystals were prepared from the extracted cellu- and hydrolysis steps were optimized in accordance to plant material
lose fibers. The chemical composition further attests satisfactory 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. Carbohydrate Polymers 241 (2020) 116227
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CRediT authorship contribution statement North Carolina State University, Department of Wood and Paper Science (2008).
BioResources (vol. 3). Retrieved fromDept. of Wood and Paper Science, College of
Natural Resources, North Carolina State Universityhttps://ojs.cnr.ncsu.edu/index.
J.W.M.E.S. Weerappuliarachchi: Conceptualization, php/BioRes/article/view/BioRes_03_4_1403_Ioelovich_Cellulose_Nanostruc_Polymer_
Methodology, Formal analysis, Investigation, Writing - original draft. Review/0.
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Supervision. S.K.S. Thennakoon: Formal analysis. B.S. Dassanayake: Rosa, S. M. L., Rehman, N., de Miranda, M. I. G., Nachtigall, S. M. B., & Bica, C. I. D.
(2012). Chlorine-free extraction of cellulose from rice husk and whisker isolation.
Conceptualization, Formal analysis, Resources, Writing - review &
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editing, Supervision, Project administration, Funding acquisition. 08.084.
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Acknowledgement estimating the degree of crystallinity of native cellulose using the X-ray dif-
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The authors are grateful to the Royal Botanical Garden, Peradeniya, Sgriccia, N., Hawley, M. C., & Misra, M. (2008). Characterization of natural fiber surfaces
Sri Lanka. And sincerely acknowledge Department of Botany, Faculty of and natural fiber composites. Composites Part A: Applied Science and Manufacturing,
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Science, and University of Peradeniya, Sri Lanka. Sheltami, R. M., Abdullah, I., Ahmad, I., Dufresne, A., & Kargarzadeh, H. (2012).
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