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of high quality natural DOI: 10.1177/1528083719887533
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cellulose nano fibrils from
a novel material Ficus
natalensis barkcloth
Abstract
We report for the first time the extraction of cellulose nano fibrils from Ficus natalensis
barkcloth fibers by means of chemical treatments and catalytic oxidation of cellulose
fibers by using 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO). After every stage
of treatments, the structural properties of barkcloth fibers powder (BC-PW), cellulose
fibers (BC-NB) and cellulose nano fibrils (BC-CNF) were carefully characterized by
means of scanning electron microscopy (SEM) and transmission electron microscopy
(TEM) for morphological analysis, Fourier-transform infrared spectroscopy (FTIR) and
X-ray diffraction techniques for chemical analysis, and thermal properties were done by
thermo-gravimetric analysis. FTIR results revealed the progressive removal of non-
cellulosic contents and X-ray diffraction (XRD) analysis showed that the crystallinity
increased with the successive alkali and bleaching treatments. Finally, by evaluating the
TEM images, the average diameter of the nano-cellulose fibrils from Ficus natalensis
barkcloth was also confirmed as 28 0.6 nm and the length in hundred nano meters
was recorded. The resultant cellulose nano fibrils maintaining the cellulose I structure
had dimensional properties in nano-scale, higher crystallinity (68.5), and better thermal
1
College of Textiles, Donghua University, Shanghai, PR China
2
Innovation Center for Textile Science and Technology, Donghua University, Shanghai, China
3
School of Automation, Nanjing University of Science and Technology, Nanjing, China
4
Key Laboratory of Eco-Textile, Ministry of Education, Jiangnan University, Wuxi, China
Corresponding author:
Lifang Liu, Donghua University, Songjiang Campus, Shanghai 201620, China.
Email: lifangliu@dhu.edu.cn
2 Journal of Industrial Textiles 0(0)
stability (305.62 C). The barkcloth cellulose nano fibrils can be used in nano technology
like food packing material, nano composites and medical textiles.
Keywords
Materials, properties, structure properties, fibrous materials, cellulose nano fibrils
Introduction
Environmental fortification has become an important and challenging issue in the
recent years [1]. The reason is the formation of non-biodegradable materials
like fossil fuels and the byproducts of petroleum refineries [2]. Additionally,
these caused severe issues in the health of humans and marine life [3]. Therefore,
due to the increasing contemplations of the United Nation Organization (UNO)
environmentalist and World Health Organization (WHO) attention, recently, a lot
of studies have focused on the conservation and environment preservation [4,5].
The key advantage of these investigations is the use of natural polymers from
natural resources like plants and animal matter.
Cellulose is the most abundant natural biopolymer in the world [6]. It is widely
present in plants (approximately 40–55 wt.%) and bacteria [7] and considered to be
the lasting renewable biomass, nontoxicity, biodegradability, stability, low cost
and consequently a good substitute to synthetic products [8–10]. Cellulose and
their derivatives are utilized in various applications such as coating development,
food packing, electrical elements, papermaking and textures [11]. Furthermore, it
has a unique structure which comprised of highly stereo-regular linear homo-
polysaccharide of B-1, 4-linked anhydro-D-glucose units with a high aspect
ratio, i.e. 2–50 nm wide and hundreds of nanometer long which endows the cellu-
lose with tensile stiffness (2–6 GPa) [12–14]. The cellulose nanomaterial exhibited
considerable features and characteristics, such as hydrophilicity, high elastic mod-
ulus (140–150 GPa), lightweight (1.5 g/cm3), low thermal expansion coefficient in
the axial direction, broad chemical-modification capacity, crystallinity character
and high surface area [15–19].
The extraction of cellulose fibers to produce polymeric materials is a complex
phenomenon [20]. In the learning resources, several methods (acid hydrolysis,
mechanical defibrillation and TEMPO oxidation) have been applied to break
the inter-fibrillar hydrogen bonds between the hydroxyl groups of cellulose for
the extraction of nano-materials or nano-crystals [14]. Amongst all, acid hydrolysis
(late 1940s) is described as the primary method which yielded crystalline rod-
like cellulose nano-crystals (CNC) [21]. In the mechanical defibrillation method,
the nano cellulose fibrils (CNF) are isolated from the constituent of
fiber matrix [22]. The 2,2,6,6-tetramethylpiperidin-1-oxyl- (TEMPO) mediated
Farooq et al. 3
Experimental works
Materials
Ficus natalensis plants are observed in almost all regions in Kenya and Uganda.
Bio-degradable barkcloth from Ficus natalensis tree was obtained from Kenya,
after extraction techniques as mentioned in Rwawiire et al. [34]. All the chemicals
sodium bromide (NaBr, 99%), sodium chlorite (NaClO2, 80%), sodium hydroxide
(NaOH, 98%), sodium hypochlorite (NaClO, solution, 15%) and hydrochloric
acid (HCl, 37%) were purchased from Sinopharm Chemical Reagent Co., Ltd,
Shanghai, China. Deuterated dimethyl sulfoxide (DMSO), ethanol (CH3CH2OH,
solution, 98%) and 2,2,6,6-Tetramethylpiperidin-1-yl oxyl (TEMPO, 98%) were
obtained from Aladdin Chemistry Co. Ltd, Shanghai, China.
NaOH treatment. A total of 50 g/l cleaned and dried barkcloth residual fibers in
powder form was taken and then mixed with 1.0 M NaOH solution for 2 h at 80 C
under constant stirring by keeping the beaker on a magnetic stirrer. Alkali-treated
samples were washed with deionized water for several times, filtered and dried at
40 C for 6 h in the vacuum oven.
fibers from barkcloth (10 g) were distributed in the 190 g water for 6 h and later a
fixed amount of NaBr 0.20 g and TEMPO 0.02 g was added to the solution. By
adding drop wise 12% NaClO (18 g) solution The reaction was started under
constant stirring by adding 12% NaClO (18 g) solution dropwise. The pH
(10–10.5) was monitored continuously with the pH meter and adjusted with
sodium hydroxide aqueous solution (0.5 mol/L). After that 5 mL ethanol was
added to stop the reaction followed by stirring for another 20 min. The obtained
product was washed several times with deionized water to remove the chemicals
and centrifuged at 1960g for 15 min; 1.0 g nano cellulose slurry was dispersed into
100 g of water and placed in an ice bath for 5 min sonication at 10,000 r/min.
Characterization
Composition analysis
The composition (cellulose, lignin, and ash content) of barkcloth was determined
by using the standard methods. Calorimetric method was used to determine the
cellulose content by using anthrone reagent [39]. For lignin content, APPITA
P11s-78 method was employed as mentioned in [40], while TAPPI method
211-om 93 as reported in [41] was used to measure the ash content at 525 C.
6 Journal of Industrial Textiles 0(0)
mentioned in [42] using the maximum intensity of the diffraction from the 002
plane (I002), and the minimum intensity between the 002 and 110 peaks (Iam).
I002 Iam
CrIð%Þ ¼ 100 (1)
I002
Figure 2. (a) Photographs of untreated cut pieces of Ficus natalensis barkcloth material
(b) alkali-treated samples (c) final bleached product.
Figure 3. (a) Barkcloth raw material, (b) barkcloth fibers powder (BC-PW).
powder. Figure 4(b) shows freeze dried needle shaped, closely linked and soft foam
like cellulose nano fibrils, when water was transfered out from the fibrous network
by freeze drying method. The freeze-dried CNF consisted of thin film pieces inter-
laced with sub-micron fibrils.
Figure 4. (a) cellulose fibers (BC-NB), (b) freeze dried cellulose nano fibrils.
Figure 5. (a) Transmission electron micrograph from diluted suspension of CNF extracted from
Ficus natalensis barkcloth fibers (b) diameter distribution of cellulose nano fibrils.
dimension of CNF samples, the TEM image was evaluated by using the image J
software to get the diameter frequency distribution data. The diameter distribution
through image J software of 100 samples of CNF extracted from Ficus natalensis
barkcloth fibres was taken to better understand the dimensions and shape as
shown in Figure 5(b), and the diameter was distributed mainly from 15 to
41 nm, average diameter of about 28 0.6 nm and length in several hundred
nano meters.
peaks are reported in Table 1. The spectrum of all the samples has broad absorp-
tion bands having peaks around 3306–3401 cm1, which is corresponded to –OH
stretching vibrations of methyl groups [11] and peaks at 2900 cm1 are ascribed to
the C–H stretching vibrations of methylene groups. It is worth noting that these
two characteristics peaks are assigned to stretching of hydrogen bonds and bend-
ing of hydroxyl (OH) groups due to cellulose existence in all three samples, indi-
cating that cellulose was not removed during alkalization, bleaching and TEMPO
oxidation of all the samples. A shoulder was observed around 1165 cm1 in the
spectrum corresponding to the BC-PW ascribed to C–C stretching vibration.
Similarly, the broad absorption band at around 1028 cm1 is due to C–O–C pyra-
nose ring stretching vibration. Meanwhile, the BC-PW shows absorption peaks
at 1603 cm1 which corresponds to O–C ¼ O asymmetric stretching, but in case of
BC-CNF, the peaks moved to the point 1606 cm1 which is bit sharper than
BC-PW, attributed to carboxylate groups caused by TEMPO oxidation process [12].
Thermal analysis
The thermal stability of both untreated and chemically treated Ficus natalensis
barkcloth fiber samples was done by thermogravimetric analysis (TGA). Figure 7
graphically represented the TGA and derivative thermogravimetry (DTG) curves
obtained for BC-PW, BC-NB and TEMPO-oxidized barkcloth cellulose nano
fibers BC-CNF which occurs over a wide range of temperature according to the
degradation of all the samples constituents [54]. Regardless of their treatment, an
initial weight loss of the samples occurs below 100 C. The initial weight reduction
is attributed to the amount of water moisture content presented in each sample.
Farooq et al. 11
Figure 7. TGA and DTG curves of barkcloth fiber powder (BC-PW), alkali treated, bleached
fibers (BC-NB) TEMPO oxidized cellulose nano fibrils (BC-CNF).
Compared to BC-PW, the sample BC-NB has higher thermal stability because of
the presence of hemicellulose, lignin, and pectin in untreated sample (BC-PW) [55].
That’s why BC-PW shows onset degradation temperature at about 251 C and final
degradation temperature was at 363 C as similar finding was reported by Tendo
et al. [56]. But in the case of alkali and bleach-treated sample, BC-NB shows higher
onset degradation temperature of 310.62 C and degrading ends at 342 C, close to
the literature which recommends that cellulose degradation takes place between
275 and 400 C [35,57,58]. Meanwhile, cellulose nano fibrils show degradation
peaks lower than those of barkcloth powder (BC-PW) and cellulose fibers (BC-
NB). Decrease of decomposition temperatures of CNF is due to the introduction
of unstable sodium carboxylate groups during TEMPO oxidation [59]. Similarly,
Figure 7 shows the DTG curves for every sample; BC-PW shows two degradation
12 Journal of Industrial Textiles 0(0)
peaks which is due to decomposition of non-cellulosic materials and the other peak
shoulder is possibly ascribed to the decomposition of cellulosic compounds.
Meanwhile, BC-NB shows one sharp DTG curve which gave significance evidence
of the removal of non-cellulosic impurities after the alkali treatment and bleaching
of barkcloth fibers. Conversely, the sample of BC-CNF shows reduction in the
early onset degradation temperature with respect to other samples, as TEMPO
oxidation caused the destruction and conversion of macro cellulose into micro
cellulose chains and converted into low molecular weight chains so the activation
energy decreases making the sample less thermal resistant.
X-ray diffraction
XRD evaluation was completed to investigate the crystalline structures of the
fibers and relationship between fiber structures and properties. The X-ray
diffractograms of barcloth fibers powder BC-PW, alkali and bleached treated
fibers BC-NB and cellulose nano fibrils BC-CNF are shown in Figure 8. The
XRD diffractrograms indicated that the diffraction peaks at around 16.02 ,
22.25 and 34.68 have been observed for all the samples, and similar results
were also observed in Haafiz et al. [14]. Figure 8 has illustrated that the diffraction
peaks at around 16.02 (broad) corresponding to 110, 22.25 (sharp intense) cor-
responding to 002 and 34.68 (small) corresponding to 004 [23] have been observed
for the crystallographic planes of the cellulose I. But the diffraction peak at 22 of
cellulose nano fibrils (BC-CNF) is sharper than the other samples due to higher
crystallinity value.
Farooq et al. 13
BC-PW 36.8
BC-NB 62.3
BC-CNF 68.5
Conclusion
To our knowledge, the Ficus natalensis barkcloth fibers are the first reported material
for the simultaneous cellulose extraction and derivatization of nano cellulose fibrils
directly from the TEMPO oxidation which can be an efficient material for nano
technology. Chemical purification for cellulose extraction by means of alkali treat-
ment and bleaching was done, obtained cellulose fibers were TEMPO oxidized to get
the cellulose nano fibrils (CNF). The infrared spectroscopy, morphological investi-
gation, and X-ray diffraction analyses confirmed the removal of non-cellulosic mate-
rials. An increase of crystallinity index induced by the chemical treatments from
36.8% to 68.5% was examined, while the diameter reduced to 20–25 nm having
length in hundred nano meters. The overall yield of cellulose fibers based on the
raw material was comparatively good as 34.5 1%. So, the cellulose and nano cel-
lulose fibrils from the barkcloth materials could act as an excellent filler in the
biocomposites.
Funding
The author(s) disclosed receipt of the following financial support for the research, author-
ship, and/or publication of this article: The work was supported by “National Key R&D
Program of China (2018YFC2000900)” and “Fundamental Research Funds for the Central
Universities” (2232018A3-04)”.
ORCID iDs
Amjad Farooq https://orcid.org/0000-0002-0318-2597
Muhammad A Naeem https://orcid.org/0000-0002-6356-1935
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