Ind. Eng. Chem. Res.

2011, 50, 871–876 871

Isolation of Cellulose Nanoparticles from Sesame Husk

Bindu Sekhar Purkait,† Dipa Ray,*,† Suparna Sengupta,‡ Tanusree Kar,§ Amar Mohanty,|,⊥ and
Manju Misra|,⊥
Department of Polymer Science & Technology, UniVersity of Calcutta, 92 A.P. C Road, Kolkata 700009, India,
Calcutta Institute of Engineering & Management, Tollygunge, Kolkata 700040, India, Department of Materials
Science, Indian Association for the CultiVation of Science, 2A and B Raja S.C Mallick Road, Kolkata 700032, India,
School of Engineering, Thornbrough Building, UniVersity of Guelph, Guelph, N1G 2W1, ON, Canada, and
Bioproducts DiscoVery and DeVelopment Centre, Department of Plant Agriculture, Crop Science Building,
UniVersity of Guelph, Guelph, N1G 2W1, ON, Canada

Preparation of green cellulose nanoparticles (CNPs) from renewable resources is becoming an important area
of research. An agro-waste such as sesame husk has been used for the first time to generate cellulose
nanoparticles. Sesame husk, which is deep brown in color, was treated with 0.7% sodium chlorite solution,
followed by alkali treatment. This chemically treated mass was subjected to acid hydrolysis with 35% sulfuric
acid. Cellulose microwhiskers were released from the husk, forming a white colloidal suspension and leaving
a solid residue at the bottom. These microwhiskers were examined by optical microscopy and transmission
electron microscopy (TEM). The microwhiskers were observed to be multifaceted, existing in associated
form and having width in the range of 1-2 µm. These microwhiskers were subjected to homogenization,
after which spherical cellulose nanoparticles (CNPs) were produced having diameters in the range of 30-120
nm. X-ray diffraction study of these white cellulose nanoparticles and the residue showed a highly crystalline
nature of the cellulose particles. Atomic force microscopy also confirmed the spherical shape of the cellulose
nanoparticles. The block hardness and modulus of the CNPs were measured by nanoindentation tests.

1. Introduction beet13 have been used as raw materials to isolate cellulose

Over the past few decades, there has been an enormous
increase in interest toward natural fibers among material
scientists and researchers. Instead of conventional petroleum-
based plastic products, natural-fiber-reinforced biocomposites
can be utilized in various fields such as automotives, packaging,
and agriculture. Thus, the environment can be protected from
pollution by using these ecofriendly polymers. Cellulose and
many cellulose products are favorable polymers from the
viewpoint of the environment, as they can be safely returned to
the natural carbon cycle by simple rotting. Cellulose in its
nanocrystalline form has a very high tensile strength and a high
Young’s modulus and is a very good reinforcing filler for
various composite materials.1-3 Jute micro-/nanofibers were
effectively prepared by Wang et al.4 Spherical cellulose nano-
particles with sizes ranging from 60 to over 570 nm were
developed by Zhang et al.5 Nanocrystalline cellulose (NCC) can
be used for regenerative medicine as studied by Fleming et al6
and optical applications as reported by Revol et al.7
Cellulose nanofibrils or nanoparticles can be generated by
mechanical or chemical treatments such as acid hydrolysis.
During acid hydrolysis, hydrolytic cleavage of the glycosidic
bonds takes place mainly in the amorphous regions of the
cellulose, releasing individual crystallites. A technique for the
production of nanocrystalline cellulose with a narrow size
distribution was reported by Bai et al.8 Isolation and charac-
terization of cellulose from sugar cane bagasse was reported
by Sun et al.9 Wood fibers,10 cotton,11 sea animals,12 and sugar
* To whom correspondence should be addressed. Tel.: +91-033-
2350 1397. Fax: +91-033-2351 9755. E-mail: roy.dipa@gmail.com.
†
University of Calcutta.
‡
Calcutta Institute of Engineering & Management.
§
Indian Association for the Cultivation of Science.
|
School of Engineering, University of Guelph.
⊥
Department of Plant Agriculture, University of Guelph.
10.1021/ie101797d  2011 American Chemical Society
Published on Web 12/14/2010
nanofibrils by chemical methods. Cellulose nanowhiskers from
coconut husk fibers were prepared by Imam et al.14 A study of
the mechanical, thermal, and morphological properties of
microcrystalline cellulose particles prepared from cotton slivers
using different acid concentrations was performed by Ray et
al.15 Gas-phase surface esterification of cellulose microfibrils
and whiskers was reported by Berlioz et al.16 Current interna-
tional research into cellulose nanofibers and nanocomposites
was described by Eichhorn et al.17 Microfibrillated cellulose
from the peel of prickly pear fruits was prepared by Habibi et
al.18
The shapes and size distributions of crystalline nanoparticles
prepared by acid hydrolysis of native cellulose were reported
by Samira et al.19 The effects of alkaline treatments on structural
and morphological features of cellulose microfibrils from banana
rachis were reported by Robin et al.20 Cellulose nanowhiskers
from grass of Korea were prepared by Pandey et al.21 Properties
of nanofibrillated cellulose from different raw materials and their
reinforcement potential were discussed by Zimmerman et al.22
Characterization of microcrystalline cellulose and cellulose long
fibers modified by iron salt was reported by Sain et al.23
Mechanical methods include a high-pressure refiner treatment,24
a grinder treatment,25 and a high-pressure homogenizer
treatment.4,5 The fibers made by these mechanical methods could
be bundles of microfibers or nanofibers.
In the previous literature reports, various types of cellulosic
resources were used as precursors for the generation of cellulose
nanoparticles. In this work, we chose sesame husk as the starting
material. The main objective was value addition to this
agricultural waste, which is presently used only as cattle
feedstock. The lignin content of deep-brown-colored sesame
husk is high, around 40%. This separated lignin can also be
recovered and utilized, which will make the process even more
economical. This will open new avenues for using such
872 Ind. Eng. Chem. Res., Vol. 50, No. 2, 2011

abundant, renewable, and inexpensive agrowaste materials for

developing value-added products.
In the present work, cellulose nanoparticles (CNPs) were
obtained from sesame husks by various chemical treatments.
These CNPs were subjected to atomic force microscopy (AFM),
field-emission scanning electron microscopy (FE-SEM), trans-
mission electron microscopy (TEM), X-ray diffraction (XRD),
and nanoindentation studies to investigate their properties.
Different cellulosic resources have been used by researchers to
generate cellulose nanofibrils or nanowhiskers or nanoparticles,
but use of agro-waste as a precursor is very rare. This is the
novelty of this work, where a value has been added to a waste
material apart from the generation of green, ecofriendly cel-
lulosic nanofillers for diversified applications.

2. Experimental Section
2.1. Materials. Sesame husk was collected from a local
sesame oil mill. Sodium chlorite and sodium bisulfite (Lo-
baChemie Product) were used for delignification step. Sodium
hydroxide and acetic acid, from Merck, were used for removal
of the hemicellulose fraction. Sulfuric acid (laboratory-grade
Merck product) was used for acid hydrolysis. A high-speed
homogenizer (Remi, model RQ 127A) was used to reduce the
particle size to the nanolevel.
2.2. Pretreatment of Sesame Husk. To isolate the cellulose
nanoparticles, it is important to remove the lignin and hemi-
cellulose fractions from sesame husk as far as possible. The
rigidity of the highly crystalline cellulose particles cannot be
fully exploited if they remain embedded within the amorphous
cementing materials such as lignin and hemicellulose. Hence,
in this study, we first separated these noncellulosic constituents
from the sesame husk. The chemical treatment of the sesame
husk is depicted in Figure 1. Delignification was done by
standard sodium chlorite (0.7% NaClO2) treatment as reported
by Ray et al.26 The raw sesame husk was treated with 0.7%
sodium chlorite solution at pH 4 and kept for 2 h at near-boiling
temperature with continuous stirring. Then, it was filtered and
washed, and the material was put into 2% sodium bisulfite
solution. The bisulfite-treated mass was filtered, washed, and
dried in an oven until constant weight was observed. A deep-
yellow-colored solid residue was obtained. Nearly 35-40%
weight loss was observed due to removal of the lignin. This
dried mass was then subjected to alkali (17.5% NaOH) treatment
for removal of the hemicellulose fraction. The total weight loss
observed after alkali treatment was nearly 20%. Finally, this
chemically treated mass (M) was subjected to acid hydrolysis.
2.3. Preparation of Cellulose Nanoparticles from
Sesame Husk. The chemically treated husk (M) was hydrolyzed
with 35% sulfuric acid with constant stirring for 3 h at 50 °C
following the standard hydrolysis procedure of Dong et al.27
Hydrolyzed solution resulted in a white colloidal suspension
and an amorphous solid residue at the bottom (R). This mixture
was subjected to differential centrifugation to separate the
colloidal suspension from the residue. This colloidal suspension
was further transferred into centrifuge bottles and centrifuged
for 15 min at 9000 rpm. The fractions were washed continuously
by adding distilled water and by several centrifugation steps.
A similar process has been reported by some researchers in their
work.28,29 The cellulose suspension was then homogenized with
high-speed homogenizer (Remi model RQ 127A) for 1 h at a
speed of 2000 rpm and was sonicated for 2 h. When 1 g of
chemically treated mass (M) was acid-hydrolyzed, the yield of
Figure 1. Flow-sheet diagram showing the preparation of cellulose
nanoparticles from sesame husk.
cellulose whiskers was nearly 0.2 g. The preparation of cellulose
nanoparticles from sesame husk is shown by a flow diagram in
Figure 1.
3. Testing Method
The prepared CNP suspension was subjected to TEM analysis
at two stages: just after the acid hydrolysis and after homog-
enization. A transmission electron microscope [Technai G2 Spirit
biotwin electron microscope (SEI)] with a voltage range of
210-240 V and a frequency range of 50-60 Hz, operated with
a thermo ionic tungsten electron gun at 80 kV voltage, was used
for the study. A drop of aqueous suspension of CNP was poured
on a carbon-coated Cu grid (300 mesh) with a micropipet and
dried prior to TEM examination. The CNPs were characterized
by AFM using a Veeco MultiMode scanning probe microscope
with a Nanoscope IIIa controller. A drop of aqueous suspension
of CNP was poured on a glass coverslip with a micropipet and
dried prior to AFM examination. Images were collected using
tapping mode with a phosphorus-doped silicon tip (model
RTESP) with a nominal frequency of 312 kHz. Field emission-
scanning electron microscopy (FE-SEM) was performed using
a model JEOL JEM-6700F instrument. An ADCON optical
microscope was used for monitoring the change in sesame husk
upon acid hydrolysis. CNP powder was obtained by freeze-
drying at -110 °C for 2 days. The XRD analysis of CNP
powder was done with an X’Pert PRO model Rigaku MINISLEX
instrument at a scanning rate of 4°/min. Nanoindentation of CNP
pellet was performed using a Nanoindentor TM II apparatus.
Pellets of CNP powder were made for the nanoindentation tests.
To make the pellets, a measured amount of CNP powder was
 Ind. Eng. Chem. Res., Vol. 50, No. 2, 2011 873

Figure 2. SEM micrograph of sesame husk.

Figure 4. TEM micrographs of cellulose microwhiskers.

Figure 3. Optical micrographs showing the gradual release of cellulose

whiskers from the husk after (a) 45, (b) 120, and (c) 180 min of acid
hydrolysis.
compacted in a metal mold in a compression molding machine,
which was described in detail in our previous work.15 The
measurements of hardness and elastic modulus were obtained
using a Berkovich indentor. The reported values are the means Figure 5. Particle size distribution of cellulose nanoparticles after (a) 45
min and (b) 1 h of high-speed homogenization.
from at least six indentations.
cally treated mass, when subjected to acid hydrolysis, revealed
a unique transformation. Very fine cellulosic microwhiskers of
4. Results and Discussion
nearly 1-2 µm length were gradually released from the husk.
Characterization of CNPs. The sesame husk (Figure 2) was The optical micrographs showing the gradual release of the
initially chemically treated with sodium chlorite and alkali cellulose microwhiskers from the husk are presented in Figure
solution to remove the noncellulosic constituents. This chemi- 3a-c. The images in parts a-c of Figure 3 were taken after
874 Ind. Eng. Chem. Res., Vol. 50, No. 2, 2011

Figure 6. AFM images of cellulose nanoparticles prepared by homogenization.

45, 120, and 180 min, respectively, of acid hydrolysis. The

structures of the sesame husk were gradually disintegrated, and
the fine microwhiskers came from them. These whiskers were
observed by TEM to obtain an accurate idea of the shape and
size of the cellulose whiskers. The TEM images (Figure 4)
clearly reveal the many-sided structure of the whiskers and their
association with one another. Crystalline arrays of cellulose
nanofibrils are also evident from the diffraction and Kikuchi
lines obtained from TEM (Figure 4c). Preparation of such
cellulose microwhiskers, isolated from an agro-husk, is reported
for the first time here. This indicates that such cellulose
microwhiskers remain encapsulated by a noncellulosic husky
cover and, if isolated, can be employed as a useful material.
Acid hydrolysis finally resulted in a white colloidal suspension
and a solid residue that settled at the bottom (R). The colloidal
suspension of cellulose particles was separated, made acid-free,
and then subjected to high speed homogenization. Particle size
analysis was carried out after 45 min and 1 h of homogenization.
The particle size distributions are shown in Figure 5a,b, and
the maximum peak intensities were observed at 342 and 235 Figure 7. FE-SEM images of cellulose nanoparticles prepared by
nm for 45-min and 1-h homogenized samples, respectively. The homogenization.
particles were investigated by AFM, shown in Figure 6. The
particles were mostly spherical, but some were elliptical.
The size and shape were also observed by FE-SEM after 2 h of
high-speed homogenization, which revealed particles in the size
range of 30-120 nm (Figure 7). A very uniform breakdown
occurred that produced a uniform range of spherical cellulose
nanoparticles. TEM also showed the spherical nature of the
cellulose nanoparticles (Figure 8). Similar spherical cellulose
nanoparticles were reported by Ibrahim et al in a recent study.28
The XRD graphs of these CNPs, the amorphous residue (R),
and the precursor sesame husk (SH) are shown in Figure 9.
The CNPs were highly crystalline, exhibiting a very sharp peak
at 2θ ) 25°, whereas the residue (R) was fully amorphous. This
sharp peak was evident in the XRD graph of the untreated, raw
sesame husk (SH) (Figure 9 inset). A similar very sharp XRD
peak was observed in the case of microcrystalline cellulose
particles derived from newsprint, reported in our previous
work.30
A pellet, prepared from CNP powder, was subjected to
nanoindentation tests to investigate the block modulus and block
hardness of the CNPs and to determine the viscoelastic behavior Figure 8. TEM micrograph of cellulose nanoparticles prepared by
of the particles (Figure 10). There was a very high penetration homogenization.
of 19000 nm when a load of 100 mN was applied, which can
be ascribed to the fragmentation of the pellet during nanoin- CNPs were 1.76 VHN and 0.3 GPa, respectively. These
dentation, forming smaller plastically deformable cellulose observations fully conform to our previous work,15 where we
nanoparticles. The block hardness and block modulus of the reported the modulus and hardness of microcrystalline cellulose

Figure 9. XRD graph of sesame husk (inset), cellulose nanoparticles, and
noncellulosic amorphous residue.
Figure 10. Load-displacement curve of cellulose nanoparticles obtained
by nanoindentation.
particles prepared by 35% acid hydrolysis of cotton. These
observations indicate that 35% acid hydrolysis yields softer
cellulose particles than 64% acid hydrolysis.
5. Conclusions
The present work shows that cellulose whiskers can be
isolated from sesame husk, which is an agro-waste material.
Chemical treatment with sodium chlorite and alkali removed
the noncellulosic constituents by nearly 50% by weight. The
remaining portion, when hydrolyzed with 35% sulfuric acid,
released very well-defined cellulose microwhiskers, which were
1-2 µm in diameter. These whiskers were further homogenized
to reduce their size. High-speed homogenization resulted in a
lowering of the size of the cellulose particles having diameters
in the range of 30-120 nm. All of the microscopic investigations
confirmed the uniform spherical nature of the particles. XRD
analysis revealed a highly crystalline nature of the cellulose
particles, and the residue separated during acid hydrolysis was
fully amorphous. CNPs were made into a pellet that was
subjected to nanoindentation. The block hardness and block
modulus of the CNPs were found to be 1.7 VHN and 0.3 GPa,
respectively. The separated lignin (almost 50%) will also be
Ind. Eng. Chem. Res., Vol. 50, No. 2, 2011 875
recovered, and suitable application of the lignin particles will
be explored. Although extensive research to use cellulose
nanofillers as reinforcements in polymer matrix composites is
ongoing, some problems are yet to be solved. A major difficulty
is faced during drying of the nanocellulose, because the fibers
have a strong tendency to reaggregate and the nanosize effect
is partially lost. Another problem is associated with the
dispersion of hydrophilic nanocellulose particles into hydro-
phobic polymer matrixes. Therefore, the particles require surface
modification to increase their suitability as reinforcing fillers
in polymer cmatrixes. These points are now being investigated
to increase the versatility and usefulness of such fillers.
Acknowledgment
D.R. is thankful to AICTE (All India Council for Technical
Education), Government of India, for granting her CAYT
project. The authors are thankful to Himel Chakrabarty (CSIR
Fellow, BESU) for helping in nanoindentation tests. The authors
are also thankful to Prof. Arup Mukherjee and Ms. Subhadra
(CSIR Fellow) of the Dept. of Chemical Technology, University
of Calcutta, for their help in particle size analysis.
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ReceiVed for reView April 20, 2010
ReVised manuscript receiVed November 16, 2010
Accepted November 23, 2010
IE101797D