Current Research in Green and Sustainable Chemistry 3 (2020) 100032

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Current Research in Green and Sustainable Chemistry

journal homepage: www.elsevier.com/journals/
current-research-in-green-and-sustainable-chemistry/2666-0865

Isolation and characterization of cellulose from cashew (Anacardium

occidentale L.) nut shells
A.A. Bamgbola a, *, O.O. Adeyemi a, O.O. Olubomehin a, A.K. Akinlabi b, O.S. Sojinu b,
P.O. Iwuchukwu c
a
Department of Chemical Sciences, Olabisi Onabanjo University, Ago-Iwoye, Ogun State, Nigeria
b
Department of Chemistry, Federal University of Agriculture, Abeokuta, Ogun state, Nigeria
c
Department of Pure and Applied Zoology, Federal University of Agriculture, Abeokuta, Nigeria

A R T I C L E I N F O A B S T R A C T

Keywords: Cashew nut shells are agro-waste after the flesh and oil have been extracted from edible cashew nut. In this study,
Cellulose cashew nut shells (CNS) were utilized as the raw material for obtaining purified cellulose. The modified acid
Cashew hydrolysis method was used to isolate cellulose from dewaxed CNS using 7% (w/v) nitric acid, alkaline treatment
Nut
(17.5% w/v NaOH) and bleaching with 3.5% (v/v) sodium hypochlorite solution (NaOCl). Micromophologies,
Shells
chemical functional groups and thermal stabilities of the obtained crystalline cellulose samples were obtained via
Crystalline
Acid hydrolysis Scanning Electron Microscopy (SEM), Fourier Transforms Infrared Spectroscopy (FTIR) and Thermogravimetry
Analysis (TGA) respectively. The presence of inherent elements such as C, Ca, Mg and Fe were obtained in the
distinct rod-like shaped cellulose. Structural changes revealed via FTIR and XRD show that, after undergoing a
temperature range of 300–400
C  10%, a yield of 20.8% of highly crystalline cellulose whose crystallinity index
of 77.7%. This implies that the CNS can be repurposed as raw material for the production of cellulose fibres that
are used for packaging, reinforcement and binders for some industrial products.

1. Introduction formation of a highly ordered three-dimensional crystal structure [1].

Among biomass, cellulose is one of the most naturally abundant
polysaccharides consisting of glucose molecules linked together by
glycosidic oxygen bridges [15]; each monomer (glucose) is composed of
β-1,4-linked glucopyranose unit that is aligned at 1800 to its neighbour
[16]. [5] reported its straight-chain formation is most suitable for pro-
ducing strong fibres. Pectin (an example of cellulose of plant origin)
slows down the movement of food in the digestive tract, which thereby
allows for more necessary nutrients to be absorbed by the body instead of
being quickly passed through as waste. Likewise, insoluble fibres like
cellulose expedite the digestive movement of food molecules, which is
imperative in the quick removal of waste [2].
Cellulose has distinctive properties required for various industrial
applications like reinforcing element for composite material such as
water and moisture [9,39,45] and biomedical implants [35]. Proper-
ties such as self-cohesive energy, non-thermoplastic material and
strong hydrogen bonds inter/intra molecular chains, allows the
Cellulose nanocrystals (CNCs) are unique nano materials derived from
cellulose that has gained more attention considering its usage in the
vast area of research such as biomedical engineering, food, drugs,
sensor, optical and electronics [16,18,21,26,38]. Also, it is environ-
mentally friendly [15], has mechanical strength as well as high specific
surface area [22,46].
There is a potential stable supply of cellulose [7] as different studies
have shown that its source can be obtained from a variety of natural
matter such as plants, algae [25] and bacteria [14]. Bio-wastes are
considered as an alternative source for raw material in producing cellu-
lose, as there is a continuous depletion of major sources such as fossil fuel
and agricultural residues [17,27]. Hence, manufacturing companies are
gradually drifting toward recyclable biomass of natural origin especially
with plant resources that are not edible such as processed cashew nut
shells. Different scientific works have shown the potential use of cashew
plant [13]. The objective of this study is to isolate and characterize cel-
lulose from Cashew (Anacadium occidentale L.) nut shells (CNS).

* Corresponding author.
E-mail addresses: bamgbolabakie@yahoo.com (A.A. Bamgbola), oo_adeyemi@yahoo.co.uk (O.O. Adeyemi), olubomehin.oseyemi@oouagoiwoye.edu.ng
(O.O. Olubomehin), akakinlabi@yahoo.com (A.K. Akinlabi), sojinuok2000@yahoo.com (O.S. Sojinu), princewill.chukwu@gmail.com (P.O. Iwuchukwu).

https://doi.org/10.1016/j.crgsc.2020.100032
Received 13 August 2020; Received in revised form 11 October 2020; Accepted 12 October 2020
Available online 4 November 2020
2666-0865/© 2020 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
A.A. Bamgbola et al. Current Research in Green and Sustainable Chemistry 3 (2020) 100032

2. Materials and methods Table 1

Proximate percentage composition of sampled cashew nut shell.
Cashew nut shells (CNS) used for this study were collected from the Parameter % Composition
heap of processed cashew nuts at the cashew processing unit of the
Dry Matter (DM) 90.97
Federal University of Agriculture, Abeokuta, Ogun state, Nigeria (Fig. 6). Moisture Content (MC) 9.03
Cashew nut shell was handpicked and washed to remove debris, after Ash 8.5
which they were dried in the oven at 70
C. Dried nut shells were pul- Crude Protein 19.52
verized and sieved using a mesh size of 60 μm to obtain equilibrium size Crude Fibre 18.82
Neutral Detergent Fibre (NDFDM) 52.02
for further analysis (Fig. 1). Acid Detergent Fibre (ADFDM) 35.08
Acid Detergent Lignin (ADLDM) 7.00
2.1. Proximate analysis of cashew hard nutshells (CNS) Metabolizable Energy (MJ/kg) 8.61
Cellulose 28.08
Hemicellulose 16.94
Proximate analysis of dewaxed milled samples of CNS was done using Ether Extract 2.33
the nondestructive near-infrared reflectance spectroscopy technology. No free nitrogen (Nfe) 50.83
Proximate composition was obtained from the NIRS DS2500 flour Nonfibrous carbohydrates (Nfc) 17.63
analyzer by Foss Analytical, Denmark.

2.2. Cellulose Isolation- modified acid hydrolysis method 2.3. Cellulose characterization

Cellulose was isolated from the dried dewaxed samples by modified
acid hydrolysis method using 7% nitric acid for 2 h at control tempera-
ture of 90
C with continuous stirring. The resulting dark slurry was
washed until the filtrate became neutral to litmus (Johnson universal
indicator paper). The cellulosic material further treated in with 17.5%
sodium hydroxide (NaOH) for 2 h 30 min at 70
C with constant stirring
and the resulting slurry was washed with water until filtrate turns neutral
to litmus (Johnson universal indicator paper). The isolated product was
bleached with 3.5% hypochlorite solution (NaOCl) at 80
C with
continuous stirring for 30 min, after which a white product obtained
(cellulose). The cellulose isolated was then filtered using sintered glass
crucible, No. 2, air-dried for 5 days and then grinded to fine cellulose
powder (Fig. 1) using a porcelain mortar.
2.3.1. Fourier transform infrared spectroscopy (FTIR) of isolated product
and dewaxed CNS
The FTIR spectra of dewaxed cashew nut shells and isolated products
were treated with transparent KBr pellets (1:100, w/w) were obtained
from a Bulk M530 spectrophotometer. The spectra were collected at
ambient conditions in the transmittance mode from an accumulation of
128 scams at a 4 cm1 resolution over the regions of 4000–400 cm1.
2.3.2. Scanning Electron Microscopy (SEM)/Electron diffraction X-ray
(EDX)
Cellulose fibers were magnified on SEM and photomicrograph was
taken using JEOL JSM-7600F scanning electron microscope (JEOL Ltd.,
Japan). All samples were coated with gold before SEM analysis.

Fig. 1. Experimental Flow Diagram of Cellulose Isolation from cashew nut shells.

2
A.A. Bamgbola et al. Current Research in Green and Sustainable Chemistry 3 (2020) 100032

Fig. 2. SEM micrographs of (a) CNS as raw material; (b) alkali treated CNS; (c) isolated cellulosic product. 2d. EDX spectra of isolated cellulose from CNS.

2.3.3. X-Ray diffraction (XRD) l200  lam

Crystalline indexðCrlÞ ¼  100
The XRD analysis was performed on CHNS and the isolated cellulose l200
using Angstrom Advanced ADX2700 powder X-ray diffractometer
where l200 is the maximum intensity of the diffraction at 200 peaks (2θ ¼
equipped with a graphite-monochromated Cu Kα radiation source at 40
22.248) and lam is the intensity of the diffraction at 2θ ¼ 12.2881.
kV and 30 mA. The diffraction intensities were recorded in the 2θ ¼ 5
–
70
with a step size of .3 and a scan speed of .05/sec. The XRD pattern
2.3.4. Thermogravimetric analysis (TGA)
was processed using JCPDS card numbers. The crystalline index (Crl) was
Thermal stability of extracted cellulose was evaluated using a TGA-
determined using the formular documented in [37].

Fig. 3. X-ray diffractogram of bleached cashew nut shells.

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A.A. Bamgbola et al. Current Research in Green and Sustainable Chemistry 3 (2020) 100032

Fig. 4. FTIR spectra of the dewaxed CNS (a), Peak height at identified wavelength (cm1) (b), FTIR spectra of the isolated cellulose from CNS (c), Peak height at
identified wavelength (cm1) (d).

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A.A. Bamgbola et al. Current Research in Green and Sustainable Chemistry 3 (2020) 100032

Fig. 5. A: TG analysis of the isolated Cellulose from cashew nut shells, B: DTG analysis of Isolated cellulose from cashew nut shells.

5
A.A. Bamgbola et al.
Fig. 6. Heap of waste cashew nut shells at the Federal University of Agriculture, Abeokuta, Ogun State.
4000 Thermogravimetric analyzer (PerkinElmer, Netherland) from 30
C


to 950
C at a rate of 10 C/min under purging nitrogen atmosphere (50
mL/min).
3. Results and discussion
The proximate composition of the dewaxed CNS used in this study is
shown in Table 1. The dry matter (DM- 90.97%), moisture content (MC-
9.03%) and ash content (AC- 8.5%) reported here varied slightly from
88.6%, 12.4% and 3% for DM, MC and AC in [29] for cashew nutshells.
The relatively low ash and moisture content compared to its dry matter
were within range for some analysed dry sawdust of some hardwood
reported in [11]; this could suggest CNS an alternative for fuel or energy
production for domestic use. Also, the percentage composition of cellu-
lose and hemicellulose in the dewaxed sample of 28.08% and 16.94%
respectively, were lower than that obtained for other agricultural
biomass such as cashew apple bagasse, kenaf, fibre flax and onion skin
documented in [13] and [33]. The cellulose composition in the dewaxed
CNS used in this study suggests that more than one-quarter of the waste
CNS can be converted to useful renewable cellulose.
The microstructure of the cellulose isolated observed under a
scanning electron microscope (SEM/EDX) is shown in Fig. 2. The mi-
crographs shown in Fig. 2a and b exhibited a porous structure due to
degradation of lignin by alkali treatment, however, the structure
shown in Fig. 2c revealed a loose structure, thus indicating the suc-
cessful removal of residual lignin by 3.5% hypochlorite solution
(NaOCl). This implies that if consistent experimental conditions such as
constant temperature, specified reaction time with consistent stirring
would transform an amorphous agro-waste CNS into individual rod-
like cellulose fibres. A similar result has been reported for walnut
(Juglans regia) shell treated with an acetate buffer/(NaCIO2) solution
[8]. Furthermore, the EDX spectra in Fig. 2d show some quantifiable
percent of inherent elementals such as Ca (4.5), Mg (4.0), O (15.0), C
(8.5), Si (57.0), and Fe (11.5) after CNS have successfully undergone
bleaching and thus transform into cellulose fibres. These elements are
easily metabolizable because they are of the organic source. The high
concentration of Si reported from the EDX may be due to the dead
layer of Si–Li detector [10].
X-Ray diffraction of isolated cellulose is shown in Fig. 3. Peaks varied
at 2 theta ¼ 12.895, and 20.454, these values are comparable to that
obtained for treated Calotropis procera in [40]; on the other hand [34];
have opined that these values are attributed to cellulose characteristic
peaks. Presence of sharp peaks in the crystallographic plane indicates
crystalline structure because of the hydrogen bonding interaction and
6
Current Research in Green and Sustainable Chemistry 3 (2020) 100032
Van der Waals force between adjacent molecules [20]. The crystallinity
of the cellulose obtained after bleaching is 77.7%, which is comparable
with the crystalline index reported in [28,47] for soy hulls and corn husk
respectively. It is thus concluded that the modified acid hydrolysis
method used in this study gives good yield of cellulose with high crys-
tallinity index.
The infrared spectra of both the dewaxed biomass and isolated cel-
lulose from the CNS are shown in Figs in 4a and 4c. Absorption regions
were observed in curves of high wavenumber (2800–3400 cm1) and low
wavenumbers (600–1750 cm1), similar absorption regions were
observed in [4] this implies different functional groups in the molecule
give rise to bands of differing intensity. Vibration intensity observed at
763 cm1 for the dewaxed CNS is higher than 707 cm1 observed in Ali
et al. (2017) for treated samples of coffee silverskin. The studies of [36]
showed that vibration peaks at this level are due to CH2 rocking vibration
in cellulose. It is worthy to note that cellulose contains polymorphic
crystalline domains which are characterized by its origin and type of
chemical used for treating samples [41]. The bands detected at 1190 and
1060 cm1 could be assigned to the stretching vibrations of C– O of epoxy
and alkoxy respectively. The bands detected at 1628 and 1617 cm1 is
comparable to that obtained in [12]; it can be attributed to strong
stretching of C–– C stretching of α,β-unsaturated ketone in both cellulose
and dewaxed samples [24]; reported bands at 1645 cm1 corresponds to
O–H vibration of absorbed water due to hydroxyl groups in cellulose for
sugarcane plant. On the other hand [20]; agreed that band at 1634–1617
cm1 were as a result of stretched hydrogen bonds and the bending vi-
brations of hydroxyl (OH) groups bound to the cellulose structure. Band
peak at 1745–1734 cm1 were absent in the cellulose isolate, this depicts
the total removal of the carbonyl group (C– – O) in hemicellulose and
lignin. This further implies that modified acid hydrolysis method, alkali
and bleaching treatment protocols used in this study completely removed
the lignin and polysaccharides, such as pectin, xylan and hemicelluloses
[31]. Similarly, peak bands at 1502 cm1 and 1248 cm1 which have
been reported in [42] corresponding to aromatic skeletal vibrations of
lignin were absent in the cellulose isolate obtained in this study. Band
peaks 2875.176 cm1 and 3352.647 cm1 reported in this study are
attributed to stretching vibrations of C–H groups of cellulose and O–H
stretching vibrations of hydrogen-bonded hydroxyl groups in the cellu-
lose molecules [6,23]. FTIR spectra analysis also showed a variation in
the peak position of bands at 3000 and 2000 cm1 between the dewaxed
CHN and cellulose isolate. A similar result was documented in [12]
which reported a slight shift in peak position for the band at 3500 and
2000 cm1 range, this could be attributed to the high sensitivity in
changes of the intra and inter molecular hydrogen bonds related to
A.A. Bamgbola et al.
alteration in cellulose.
The thermal stability of isolated cellulose from cashew hard nutshells
is well presented in the thermogravimetric analysis (TGA). The thermo-
gram curves are shown in Fig. 5a. The observed weight loss (%) in the
thermogravimetric curve between 30 and 100
C can be linked to
evaporation of absorbed moisture in the isolated cellulose. Decomposi-
tion in the obtained cellulose occurred at only one stage and degraded
from 300 to 400
C. This is linked to cellulose degradation. The similar
range has been reported in previous studies such as [44,32] and [3] for
cellulose degradation, on the other hand [43]; reported similar range
indicates glycosyl decomposition in the cellulose fibre. The narrow range
observed in DTG curves in Fig. 5b, depicts effective removal of lignin
from the sample using the bleaching compound.
4. Conclusion
The step-wise modified acid hydrolysis method, assisted by thermal
processing successfully isolated cellulose from cashew hard nutshells.
The obtained cellulose physically exhibited distinct rod-like morphology.
The structural changes were measured by FTIR, XRD, while thermal
analysis was measured using the TGA revealed a lower thermal stability
and higher crystallinity (77.7%) as compared to the native cellulose. This
work has demonstrated that CNS, which is an abundant agricultural
waste, can be repurposed as raw material for the production of cellulose
fibre.
Author contribution
Conceptualization: Bamgbola A.A.
Methodology: Bamgbola A.A. and Olubomehin O.O.
Supervision: Adeyemi, O.O., Olubomehin, O.O. and Akinlabi, A.K.
Reviewing and Editing: Adeyemi, O.O., Olubomehin, O.O., Akinlabi,
A. K. and Sojinu, O.S.
Roles/Writing: Bamgbola A.A. and Iwuchukwu P.O.
Declaration of competing interest
None.
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