International Journal of Nanoscience and Nanoengineering

2015; 2(6):43-50
Published online November 3, 2015 (http://www.openscienceonline.com/journal/nano)

Extraction and Characterization of Nanocellulose

from Xanthoceras Sorbifolia Husks
Na Ma, Dongyan Liu, Yueyue Liu, Guoxin Sui*
Institute of Metal Research, Chinese Academy of Sciences, Shenyang, China

Email address
gxsui@imr.ac.cn (Guoxin Sui), dyliu@imr.ac.cn (Dongyan Liu), nma@imr.ac.cn (Na Ma)

To cite this article

Na Ma, Dongyan Liu, Yueyue Liu, Guoxin Sui. Extraction and Characterization of Nanocellulose from Xanthoceras Sorbifolia Husks.
International Journal of Nanoscience and Nanoengineering. Vol. 2, No. 6, 2015, pp. 43-50.

Abstract
Nanocellulse as a kind of biomaterial with nanoscale, performs considerable potential applications in a many fields. Extracting
nanocellulose might create a novel path to use of Xanthoceras sorbifolia husks. In this work, nanocellulose was extracted from
Xanthoceras sorbifolia husks through a series of chemical treatments. The morphology, chemical structure, thermal behaviors
and crystallinity of untreated husks, cellulose fibers and nanocellulose were compared. The mechanical properties of
nanocellulose film were investigated. The nanocellulose of Xanthoceras sorbifolia husks had a rod-like aspect, the diameter was
about 38nm. The essential chemical structure of cellulose was not broken during the treatments. The chemical treatments for
Xanthoceras sorbifolia husks caused the changes of the thermal properties and crystallinity. The transparent nanocellulose film
made by Xanthoceras sorbifolia husks nanocellulose showed high storage modulus at low temperature. The tensile strength and
Youngs modulus of nanocellulose film were 75.9MPa and 15.9GPa, respectively.

Keywords
Nanocellulose, Xanthoceras Sorbifolia Husks, Extracting, Nanocellulose Film, Properties

sources exhibits high stiffness and Youngs modulus [1]. The

1. Introduction
Nowadays, more and more attention has been paid on
natural materials due to their special properties such as
renewability, biodegradability and carbon neutrality. Plant
fibers are one of the abundant sources for natural resources.
Generally, plant fibers are mainly composed of cellulose,
hemicellulose and lignin. Cellulose is a linear, stereoregular
homopolymer consisting anhydroglucose units linked at one
and four carbon atoms by-glycosidic bonds, the properties of
cellulose including good mechanical properties, low density
and biodegradability. There are several types of cellulose (I, II,
III, IV and V) and typeIhas the best mechanical properties [1].
Hemicellulose and lignin are amorphous polymers, which are
not as strong as cellulose.
Nanocellulose as a kind of natural material with nanoscale,
can be obtained from sugarcane bagaasse [1, 2], hemp [3],
sisal [4], cotton [5, 6], curaua [7], bacterial [8], etc. The shape
and properties of nanocellulose are dependent on the source
and the extraction method [1, 2, 5]. Generally, the diameter of
nanocellulose is less 100nm and the length varies from 100nm
to several micrometers. The nanocellulose from conventional
Youngs modulus of the cellulose crystal structure (typeI) is
assumed to be approximately 138GPa [9]. Otherwise
nanocellulose is also considered to have higher specific
surface area, water holding capacity and crystallinity [3]. Thus
nanocellulose performs considerable potential as an effective
reinforcement for high quality special application composites
[3]. It can be used to product ultrathin displayer, light weight
body armor, wound dressing, etc.
Nanocellulose can be used to produce films, sometimes
called nanopapers in the literature [10]. Similar to
conventional paper, nanopaper constitutes a network of fibers.
Despite this structural similarity, nanopaper has superior
mechanical properties, low porosity, and it is naturally
transparent [11].
The methods for nanocellulose extracting mainly include
mechanical, chemical and enzymatic methods. Mechanical
method can produce refined, fine fibers with several
micrometers long and between 20 to 90nm in diameter [12].
The acid hydrolysis is selective for cellulose fibers, the
amorphous regions in the cellulose fibers are destroyed by
acid hydrolysis, resulting in cellulose nanocrystals [13].
Bacrterial cellulose is less than 100nm wide and 2-4nm in
 International Journal of Nanoscience and Nanoengineering 2015; 2(6): 43-50
diameter [7] with a network form.
Xanthoceras sorbifolia, is also called yellow horn, shiny
leaf yellow horn, golden horn and Chinese flowering chestnut,
which belongs to the family of Sapindaceae. It is a small tree
and endemic to northern China, wild or cultivated trees are
found in 18 provinces of China, including Beijing, Inner
Mongolia, Shandong, Liaoning, Jilin etc. The seed of
Xanthoceras sorbifolia contents abundant oil. As a source of
biodiesel, its development has receives special support from
Chinese governments [14]. However, Xanthoceras sorbifolia
husks, which are the residua of biodiesel production, has not
be utilized sufficiently yet. Extracting nanocellulose might
create a novel path to use of Xanthoceras sorbifolia husks.
In this work, nanocellulose was extracted from Xanthoceras
sorbifolia husks through a series of chemical treatments for
the first time. The morphology, chemical structure, thermal
behaviors and crystallinity of the nanocellulose and the
mechanical properties of nanocellulose film were
investigated.
2. Materials and Method
2.1. Materials
The Xanthoceras sorbifolia husks were supplied by Institute
of Applied Ecology, Chinese Academy of Science. The husks
were smashed and sieved to make sure that the size of particle
distributed from 8 meshes to 30 meshes. Sodium hydroxide,
methylbenzene, acetic acid and hydrogen peroxide were
provided by Sinopharm Chemical Reagent Co. Ltd. Ethyl
alcohol and sulfuric acid used were purchased from Dongbao
Company (Shenyang, China).
2.2. Methods
2.2.1. Alkalization
The debris of Xanthoceras sorbifolia husks were immersed
in 5wt% sodium hydroxide solution at ambient temperature
for 12h. Then the debris were washed with water for several
times until the debris were neutral. The treated debris were
dried in the oven at 80C for 24h.
2.2.2. Wax Removal
After alkalization, the debris of husks were immersed in the
solution of methylbenzene and ethyl alcohol (volume ratio of
1:1), and kept boiled for 8h. The residue was washed with
ethyl alcohol for several times and dried in the oven at 80C
for 24h for use.
2.2.3. Delignification
The husks was soaked in hydrogen peroxidee (30vol%) and
acetic acid solution (volume ratio of 1:1), and boiled with
magnetic stirring at 60C for 7h. The residue was washed with
water and filtered until the filtrate was neutral. The method
above was repeated once to make sure the reaction was
sufficient. The fibers obtained was boiled in 5wt% sodium
hydroxide solution at 80C for 2h, washed with water to
neutral and dried in the oven at 80C for 24h. The cellulose
fibers from Xanthoceras sorbifolia husks were obtained. Some
44
cellulose fibers were dispersed in water by ultrasound. The
mixed liquor was poured onto plastic petri dish, cellulose
fibers film could be peeled for use after the water fully
evaporated.
2.2.4. Preparation of Nanocellulose
The fibers were heated at a ratio of 1:50 (w:w) of 60wt%
sulfuric acid solution with magnetic stirring at 55C for 2h.
Then 500ml cold deionized water was poured into the solution
to stop the reaction. The suspension was washed with
deionized water by centrifugation at 10,000 rpm for 10 min.
When the nanocellulose could not be separated by
centrifugation, 5wt% sodium hydroxide solution was dropped
in the suspension to neutralize the free acid until the PH value
of the suspension was 7. The nanocellulose suspension was
obtained. The suspension was poured onto plastic petri dish,
the transparent nanocellulose film could be peeled for use
after the water fully evaporated.
2.3. Characterizations
2.3.1. Scanning Electron Microscopy (SEM)
The husks, cellulose fibers and nanocellulose were coated
with a thin of gold and investigated using a JSM-6301F
Scanning Electron Microscope.
2.3.2. Atomic Force Microscopy (AFM)
AFM was used to characterize the morphology and
dimensional distribution of the nanocellulose obtained from
Xanthoceras sorbifolia husks. A drop of nanocellulose
suspension was dropped on the surface of a glass slide and
dried at ambient condition. Measurements were performed in
taping mode by atomic force microscope (AFM, Veeco
NanoScope IIIa) at ambient temperature. The diameters of
100 nanofibers were counted to illustrate dimensional
distribution of the nanocellulose.
2.3.3. Fourier Transform Infrared (FTIR)
Spectroscopy
The attenuated total reflectance-Fourier transform infrared
spectroscopy (ATR-FTIR) spectra of the husks, cellulose
fibers and nanocellulose were obtained using Bruker Tensor
27. The spectra were recorded in the range from 4000cm-1 to
600cm-1 at 4cm-1 resolution.
2.3.4. Differential Scanning Calorimetry
(DSC)
The thermal behaviors of the husks, cellulose fibers and
nanocellulose were studied by TA Q20 differential scanning
calorimetry under nitrogen atmosphere. Each sample was
heated from 40C to 120C and kept at 120C for 5min to
remove the moisture in the sample and then heated to 400C.
The heating rate was 10C/min.
2.3.5. Thermogravimetric Analysis (TGA)
The thermal stabilities of the husks, cellulose fibers and
nanocellulose were studied by SETSYS Evolution 18
Integrative Analyzer under argon atmosphere. The mass of
sample was 5-10mg. The samples were heated from 150C to
45 Na Ma et al.: Extraction and Characterization of Nanocellulose from Xanthoceras Sorbifolia Husks
700C at a rate of 10C/min.
2.3.6. X-ray Diffraction (XRD)
The X-ray diffraction patterns of the husks, cellulose fibers
and nanocellulose were obtained by Rigaku D/max 2500PC
diffractometer, using CuK at 50KV and 300mA. Scattered
radiation was detected in the range of 2=5-50, at a scan rate
of 2/min.
2.3.7. Dynamic Mechanical Analysis (DMA)
The storage modulus curves of cellulose fiber and
nanocellulose films from 30C to 200C were obtained by
Q800 dynamic mechanical analysis with a heating rate of
3C/min at a constant frequence of 1Hz.
Fig. 1. Morphologies of untreated husks (a), cellulose fibers (b), nanocellulose suspension (c) and nanocellulose film (d) from Xanthoceras sorbifolia husks.
The photos of untreated husks, cellulose fibers,
nanocellulose suspension and nanocellulose film of
Xanthoceras sorbifolia husks were shown in Fig. 1. Untread
husks were brown chippings. They looked to be fluffy. After
delignification, white colored cellulose fibers with compact
structures were obtained, indicating purer cellulose, which
was more suitable for extracting nanocellulose [2]. The
nanocellulose presented white coloring in the suspension
through the hydrolysis by sulfuric acid. Because the
incorporation of sulfate groups on cellulose surface created a
negative electrostatic layer, the nanocellulose could suspend
steadily in water [7]. The nanocellulose film showed good
film integrity and high transparency, which could be
functionalized for using in transparent electrode materials.
Fig. 2 showed the SEM morphologies. It could be seen that
surface of untreated husk was very rough and porous. There
Fig. 2. SEM morphologies of untreated husks (a), cellulose fibers (b) and nanocellulose (c) from Xanthoceras sorbifolia husks.
The dimension of nanocellulose was influenced by many
factors, such as reagents, conditions of the treatments,
however, the most important factor was the raw materials [15,
16]. The diameters of the nanocellulose were calculated using
Nano Measurer software from 100 nanofibers in the amplitude
2.3.8. Tensile Properties of Nanocellulose
Film
The tensile strength and Youngs modulus of the
nanocellulose film were tested by a WSM-20kB universal
testing machine with a speed of 0.1mm/min. A load cell was
200N. The specimens were rectangles with the size of
20mm8mm. Ten specimens were tested. The thicknesses
were about 30m.
3. Results and Discussion
3.1. Morphology and Scanning Electron
Microscopy (SEM)
was some non-cellulosic substance on the surface. The size of
cellulose fiber was smaller obviously. The surface became
smoother, which implied the removal of the non-cellulosic
substance through the treatments processing. After acid
hydrolysis, the diameter of the fiber became much smaller,
which was under 100nm. It meant that the nanocellulose of
Xanthoceras sorbifolia husks was obtained.
3.2. Atomic Force Microscopy (AFM)
Fig. 3 showed the AFM micrographs of nanocellulose
obtained by sulfuric acid hydrolysis. Two modes were used to
record the data, one was height image, the other was amplitude
image. It could be seen that the nanocellulose extracted from
Xanthoceras sorbifolia husks had a rod-like aspect.
image. The result was shown in Fig.4. The diameters of all the
nanocellulose calculated were below 100nm. Almost 85%
nanofibers had the diameters between 30nm to 45nm. The
average diameter of the nanocellulose extracted from
Xanthoceras sorbifolia husks was 37.6nm.
 International Journal of Nanoscience and Nanoengineering 2015; 2(6): 43-50
Fig. 3. AFM images of nanocellulose from Xanthoceras sorbifolia husks:
height image (a) and amplitude image (b).
Fig. 4. Size distribution of nanocellulose from Xanthoceras sorbifolia husks.
3.3. Fourier Transform Infrared Spectroscopy
(FTIR)
The chemical structures of the Xanthoceras sorbifolia husks,
cellulose fibers and nanocellulose were analysed by
attenuated total reflectance-Fourier transform infrared
46
spectroscopy (ATR-FTIR). The spectra were shown in Fig. 5.
The infrared spectra of cellulose, hemicellulose and lignin had
been studied in the literature before. There were alkanes,
esters, aromatics, ketones, alcohols and different
oxygen-containing functional groups [4].
The shapes of the spectra were almost similar. The infrared
spectra of all samples showed two main absorbance regions.
One was at low wavelengths in the range 600-1800cm-1, the
other was at high wavelengths in the range 2700-4000cm-1.
According to the literature [17, 4, 18], the peaks presented at
1102cm-1 and 1170cm-1 were attributed to the C-O-C
stretching vibration of pyranose ring skeletal in cellulose
molecules. The peak at around 1640cm-1 indicated O-H
bending vibration of absorbed water. All the samples were dry
carefully in the same condition before FTIR tests, but the
absorbed water in the cellulose molecules was very difficult to
eliminate due to the cellulose-water interaction [19].
Moreover, all the spectra presented a peak at 2900cm-1, which
was resulted from C-H stretching vibration of alkyl or
aliphatic. There was a broad band around 3300cm-1, which
denoted free O-H stretching vibration of OH groups. The
results showed that most peaks did not change with the
treatments, which implied that the structure of the cellulose
was not broken severely during extracting process.
Fig. 5. ATR-FTIR spectra of untreated husks, cellulose fibers and
nanocellulose from Xanthoceras sorbifolia husks.
However, there are some differences between the spectra of
untreated and treated husks. The peak at 1735cm-1 in the
spectrum of untreated Xanthoceras sorbifolia husk was
considered to represent C=O stretching vibration of the acetyl
and uronic ester groups from pectin, hemicellulose or the ester
linkage of carboxylic group of ferulic and p-coumaric acid of
lignin and/or hemicellulose [20]. Otherwise, the peak at
1602cm-1 and 1516cm-1 were associated with the aromatic
C=C in plane symmetrical stretching vibration of aromatic
ring in lignin [21, 20]. The peak at 1240cm-1 also been
supposed to represent C-O out of plane stretching vibration of
the aryl group in lignin [22]. Those peaks disappeared in the
spectra of cellulose fiber and nanocellulose. The absence of
the peaks implied that after the chemical processing, the
contents of pectin, hemicellulose and lignin were lower than
those in untreated husks.
47 Na Ma et al.: Extraction and Characterization of Nanocellulose from Xanthoceras Sorbifolia Husks

3.4. Differential Scanning Calorimetry(DSC)
The thermal behaviors of the Xanthoceras sorbifolia husks,
cellulose fibers and nanocellolose were compared using
differential scanning calorimetry (DSC). Fig. 6 showed the
DSC results of the husks, cellulose fibers and nanocellulose.
In the order to remove the absorbed water in cellulose
completely, the samples were kept at 120C for 5min. It could
be seen that the three curves were different because of the
different components.
would sulfate the accessible hydroxyl groups on cellulose
fibers and dissolve the amorphous region. To some degrees,
the structure of cellulose might be changed and the molecular
weight or degree of polymerization would decrease [1]. The
molecular weight and size distribution of cellulose crystals
would became wider [4]. These could explain why there was
an earlier and wider endothermic peak in the curve of
nanocellulose
3.5. Thermogravimetric Analysis (TGA)

Thermal stability was an important property for

nanocellulose especially in polymer nanocomposites field, in
which used processing temperature of other polymers [13]. In
this work, thermogravimetric analysis used to measure the
mass change of the materials with the increase of the
temperature from 150C to 700C. Cellulose, hemicellulose
and lignin decomposed at different temperatures due to the
difference in their chemical structures. In the research of Yang
et al [23], cellulose started decomposition at 315C and
persisted until 400C. Maximum weight loss rate was at
355C. Hemicellulose decomposed from 220C to 315C, and
the maximum weight loss rate reached at 268C. However, the
decomposition of lignin extended to a wider range of
temperature from 200C to 700C due to the different
activities of the chemical bonds presented in its structure.
Fig. 6. DSC curves of untreated husks, cellulose fibers and nanocellulose Untreated husks, cellulose fibers and nanocellulose might
from Xanthoceras sorbifolia husks. have different thermal stability because of the different
contents of cellulose, hemicellulose and lignin. The results of
Two districts could be divided by 120C in the curves. In all TG and DTG were shown in Fig. 7.
curves, from 40C to 120C, the endothermic peaks appeared
resulting from water evaporation. The thermal behaviors of
the materials at the temperature from 120C to 400C were
quite different. No obvious endothermic peak appeared in the
curve of untreated husks. However, there was a wide
exothermic peak from 250C to 370C, which might attribute
to the decompose of the substance such as lignin, wax,
hemicellulose, cellulose, etc. Because there was much
non-cellulosic substance in untreated husks and most of that
was amorphous, the heat released by amorphous substance
decomposing was more than the heat absorbed by crystallites
fusion. Thus, the fusion peak could not be seen in the curve.
In the curve of cellulose fibers, a narrow fusion peak at
around 360C could be seen obviously, which was similar to
the DSC curve of commercial cellulose in Moran et al[4]s
work. However, the thermal degradation of cellulose would
happen at around 355C [23]. The degradation and the fusion
of cellulose might be at the same time, which caused the
superposition of peaks. The narrow fusion peak appeared in
the curve implied the high cellulose purity in cellulose fibers
obtained from Xanthoceras sorbifolia husks. Through the
treatment processing, the cellulose crystallites might rearrange
and reoriented, which would lead to a more compact crystal
structure [1] having better thermostability. That might lead to
the higher fusion point than cellulose crystallites mentioned in
the literature.
The endothermic peak of nanocellulose was around 210C Fig. 7. TG (a) and DTG (b) curves of untreated husks, cellulose fibers and
and the peak was not uniform. Hydrolysis by sulfuric acid nanocellulose from Xanthoceras sorbifolia husks.
 International Journal of Nanoscience and Nanoengineering 2015; 2(6): 43-50 48

The decomposition of untreated husks could be divided into angle close to 22 representing crystalline material and I (am)
three stages. There was a shoulder peak between 225C and is the counter reading at peak intensity at a 2 angle close to 18
320C in the DTG curve. According to the literature [23], it representing amorphous material in this research.
mainly presented the decomposition of hemicellulose. In this The pattern of untreated husks was blurring and the
stage, almost 20% weight was lost. The second stage was crystallinity index was just 35.7%, both of which implied that
probably from 310C to 385C, which was at the temperature there were much amorphous substance in Xanthoceras
of cellulose decomposition. The solid residues was close to sorbifolia husks. Due to the decreasing of non-cellulosic
40% at 385C. The weight lost above 385C was not apparent, substance, the peak in the pattern of cellulose fibers was
and most lost was attributed to the lignin decomposition. narrow and sharp, the crystallinity index went up to 70.2%. In
Finally, there was about 30% weight left for untreated husks. the pattern of nanocellulose, there were a sharper peak and a
The cellulose fibers underwent a two-step degradation higher crystallinity index (77.6%), which meant the removal
process. The shoulder peak around 280C in the DTG curve of of amorphous phase and the excellent mechanical properties
untreated husks disappeared, which implied the decreasing of of the nanocellulose from Xanthoceras sorbifolia husks.
hemicellulose. The decomposition started around 260C.
From 260C to 385C, almost 75% weight lost with the
temperature increasing. About 22% weight left at 700C.
Actually, hemicellulose, lignin and other non-cellulosic
substance started their decompositions at low temperature.
The reduction of these substance would cause the
decomposition happened at higher temperature. Otherwise,
the removal of these non-cellulosic substances through the
treatments would make the structure of cellulose more dense
and compact. These factors might be the reasons cellulose
fibers had better thermal stability than that of untreated husks.
The decomposition process of nanocellulose was
complicated. It presented multiple steps. About 30% weight
left at 700C. The nanocellulose from Xanthoceras sorbifolia
husks began to decompose at about 190C, which was the
lowest of three materials. The poor thermal stability might
result from the drastic reduction in molecular weight and the
Fig. 8. XRD patterns of untreated husks, cellulose fibers and nanocellulose
sulfonation by sulfuric acid [5, 7, 24], which would make the from Xanthoceras sorbifolia husks.
nanocellulose decompose at lower temperature. Otherwise,
sulfuric acid also acted as flame retardants, which led to the
increasing in char fraction [24]. There were mainly two peaks
in the curve of DTG. One was at around 220C, which was
attributed to the sulfated and/or small molecular weight
cellulose. The other was at around 350C, which presented the
degradation of unsulfated cellulose. The broad distribution of
molecular weight [4] and different sulfonation degrees [25]
would make multiple peaks appear in the DTG curves.
3.6. X-ray Diffraction

Generally, cellulose included crystalline phase and

amorphous phase. In order to study the crystallinity of
nanocellulose from Xanthoceras sorbifolia husks, X-ray
diffraction was carried out. The X-ray diffraction patterns of
untreated husks, cellulose fibers and nanocellulose were
shown in Fig.8. It could be seen that there was a well-defined Fig. 9. DMA curves of cellulose film and nanocellulose film.
main peak around 2=22 in both patterns. The results meant
that the main form of cellulose of Xanthoceras sorbifolia 3.7. Dynamic Mechanical Analysis (DMA)
husks was cellulose typeIwhich was stronger than cellulose Dynamic mechanical analysis involves imposing a small
type II [26, 27]. The crystallinity index (Ic) was calculated by cyclic strain on a sample and measuring the resulting stress
using the following equation [28]: response, or equivalently, imposing a cyclic stress on a sample
(I 002 -I(am)) and measuring the resultant strain response. DMA could
Ic= 100 (1) determine mechanical properties as a function of temperature.
I(002)
The storage modulus curves of cellulose fiber and
where I(002) is the counter reading at peak intensity at a 2
49 Na Ma et al.: Extraction and Characterization of Nanocellulose from Xanthoceras Sorbifolia Husks
nanocellulose films were shown in Fig. 9. The storage
modulus of nanocellulose film was much higher than that of
cellulose fiber film at the whole range of temperature, which
might contributed by compact interconnected network of
nanocellulose whiskers [29]. The storage modulus of cellulose
fiber film decreased with temperature rising. The storage
modulus of nanocellulose film increased a little first and then
decreased with temperature rising. The highest storage
modulus of nanocellulose film was about 9500MPa at around
90C, which might result from the water loss of the film.
Fig. 10. Tensile Strength (a) and Youngs modulus (b) of nanocellulose film
from Xanthoceras sorbifolia husks.
3.8. Tensile Properties of Nanocellulose Film
Some researches were in the tensile properties of
nanofibrillated film, which was made of nanocellulose
produced through mechanical and enzymatic methods [11, 30,
31]. However, few tensile properties of nanocellulose film
made of nanocellulose produced through chemical method
have been reported. Therefore, the tensile properties of
nanocellulose film were studied in this work. Similar to the
properties of nanocellulose, different source and film
production method would cause the difference in the tensile
properties of nanocellulose film. The tensile strength and
Youngs modulus of nanocellulose film were shown in Fig. 10.
In this work, the largest values were 75.9MPa and 15.9GPa.
The average tensile strength was 62.6MPa. It approached to
74.55MPa, which was the tensile strength of bacterial
cellulose film in Martinez-Sanzs work [31]. However, the
tensile strength is still lower than that of nanofibrillated
cellulose films, which is probably due to the lower aspect ratio
of the nanocellulose obtained by acid hydrolysis method. The
average Youngs modulus was 12.0GPa, which was in the
range of 12-19 GPa reported by Henriksson [11].
4. Conclusion
Nanocellulose suspension of Xanthoceras sorbifolia husks
was obtained by several steps. The nanocellulose of
Xanthoceras sorbifolia husks had a rod-like shape, the
diameter was about 38nm. Much non-cellulosic and
amorphous substance in the husks was removed during the
treatments. However, FTIR showed the chemical structure of
cellulose was almost not changed. Cellulose fibers from
Xanthoceras sorbifolia husks had high cellulose purity and
better thermal stability. Due to the effect of hydrolyzation by
sulfuric acid, the fusion point and the thermal stability of
nanocellulose were lower. The crystallinity index of
nanocellulose was as high as 71.5%, which implied the
excellent mechanical properties and application prospects of
the nanocellulose from Xanthoceras sorbifolia husks. The film
made by Xanthoceras sorbifolia husks nanocellulose was
transparent. The maximum tensile strength and Youngs
modulus of the nanocellulose film were 75.9MPa and
15.9GPa.
References
[1] Mandal A, Chakrabarty D. Isolation of nanocellulose from
waste sugarcane bagasse (SCB) and its characterization.
Carbohydr Polym 2011; 86: 1291-1299.
[2] Teixeira EdM, Bondancia TJ, Ricardo Teodoro KB, Correa AC,
Marconcini JM, Caparelli Mattoso LH. Sugarcane bagasse
whiskers: Extraction and characterizations. Ind Crop Prod 2011;
33: 63-66.
[3] Bei W, Sain M, Oksman K. Study of structural morphology of
hemp fiber from the micro to the nanoscale. Appl Compos
Mater 2007; 14: 89-103.
[4] Moran JI, Alvarez VA, Cyras VP, Vazquez A. Extraction of
cellulose and preparation of nanocellulose from sisal fibers.
Cellulose 2008; 15: 149-159.
[5] Teixeira EdM, Correa AC, Manzoli A, Leite FdL, Caue RdO,
Capparelli Mattoso LH. Cellulose nanofibers from white and
naturally colored cotton fibers. Cellulose 2010; 17: 595-606.
[6] Saraiva Morais JP, Rosa MdF, Moreira de Souza Filho MdS,
Nascimento LD, do Nascimento DM, Cassales AR. Extraction
and characterization of nanocellulose structures from raw
cotton linter. Carbohydr Polym 2013; 91: 229-235.
[7] Corra A, Morais Teixeira E, Pessan L, Mattoso L. Cellulose
nanofibers from curaua fibers. Cellulose 2010; 17: 1183-1192.
 International Journal of Nanoscience and Nanoengineering 2015; 2(6): 43-50
[8] Nakagaito AN, Iwamoto S, Yano H. Bacterial cellulose: the
ultimate nano-scalar cellulose morphology for the production
of high-strength composites. Appl Phys A 2005; 80:93-97.
[9] Nishino T, Takano K, Nakamae K. Elastic modulus of the
crystalline regions of cellulose polymorphs. J Polym Sci Pol
Phys 1995; 33 (11): 1647-1651.
[10] Kulachenko A, Denoyelle T, Galland S, Lindstrom SB. Elastic
properties of cellulose nanopaper. Cellulose 2012; 19: 793-807.
[11] Henriksson M, Berglund LA, Isaksson P, Lindstrm T, Nishino
T. Cellulose Nanopaper Structures of High Toughness.
Biomacromolecules 2008; 9: 1579-1585.
[12] Taniguchi T, Okamura K. Biodiesel production from
Xanthoceras sorbifolia in China: Opportunities and challenges.
Polym Int 1998; 47: 291-294.
[13] Alemdar A, Sain M. Isolation and characterization of
nanofibers from agricultural residues Wheat straw and soy
hulls. Bioresource Technol 2008; 99: 1664-1671.
[14] Yao ZY, Qi JH, Yin LM. Biodiesel production from
Xanthoceras sorbifolia in China: Opportunities and challenges.
Renew Sust Energ Rev 2013; 24: 57-65.
[15] Beck-Candanedo S, Roman M, Gray DG. Effect of Reaction
Conditions on the Properties and Behavior of Wood Cellulose
Nanocrystal Suspensions. (Biomacromolecules 2005; 6:
1048-1054.
[16] Eichhorn SJ, Dufresne A, Aranguren M, Marcovich NE,
Capadona JR, Rowan SJ, Weder C, Thielemans W, Roman M,
Renneckar S, Gindl W, Veigel S, Keckes J, Yano H, Abe K,
Nogi M, Nakagaito AN, Mangalam A, Simonsen J, Benight AS,
Bismarck A, Berglund LA, Peijs T. Review: current
international research into cellulose nanofibres and
nanocomposites. J Mater Sci 2010; 45: 1-33.
[17] Oh SY, Yoo DI, Shin Y, Seo G. FTIR analysis of cellulose
treated with sodium hydroxide and carbon dioxide. Carbohydr
Res 2005; 340: 417-428.
[18] Nelson ML, O'Connor RT. Relation of certain infrared bands to
cellulose crystallinity and crystal lattice type. Part II. A new
infrared ratio for estimation of crystallinity in celluloses I and II.
J Appl Polym Sci 1964; 8: 1325-1341.
[19] Baird MS, Hamlin JD, O'Sullivan A, Whiting A. An insight
into the mechanism of the cellulose dyeing process: Molecular
50
modelling and simulations of cellulose and its interactions with
water, urea, aromatic azo-dyes and aryl ammonium compounds.
Dyes Pigments 2008; 76: 406-416.
[20] Sun XF, Xu F, Sun RC, Fowler P, Baird MS. Characteristics of
degraded cellulose obtained from steam-exploded wheat straw.
Carbohydr Res 2005; 340: 97-106.
[21] Paul G, Paul W. Identification of Cellulosic Fibres by FTIR
Spectroscopy: Thread and Single Fibre Analysis by Attenuated
Total Reflectance. Stud Conserv 2003; 48: 269-275.
[22] Le Troedec M, Sedan D, Peyratout C, Bonnet JP, Smith A,
Guinebretiere R, Gloaguen V, Krausz P. Influence of various
chemical treatments on the composition and structure of hemp
fibres. Compos Part A-Appl S 2008; 39: 514-522.
[23] Yang H, Yan R, Chen H, Lee DH, Zheng C. Characteristics of
hemicellulose, cellulose and lignin pyrolysis. Fuel 2007; 86:
1781-1788.
[24] Roman M, Winter WT. Effect of Sulfate Groups from Sulfuric
Acid Hydrolysis on the Thermal Degradation Behavior of
Bacterial Cellulose. Biomacromolecules 2004; 5:1671-1677.
[25] Wang N, Ding E, Cheng R. Thermal degradation behaviors of
spherical cellulose nanocrystals with sulfate groups. Polymer
2007; 48: 3486-3493.
[26] Paakko M, Vapaavuori J, Silvennoinen R, Kosonen H,
Ankerfors M, Lindstrom T, Berglund LA, Ikkala O. Long and
entangled native cellulose I nanofibers allow flexible aerogels
and hierarchically porous templates for functionalities. Soft
Matter 2008; 4: 2492-2499.
[27] Borysiak S, Doczekalska B. X-ray diffraction study of pine
wood treated with NaOH. Fiber text East Eur 2005; 13: 87-89.
[28] Mwaikambo LY, Ansell MP. Chemical modification of hemp,
sisal, jute, and kapok fibers by alkalization. J Appl Polym Sci
2002; 84: 2222-2234.
[29] Liu DY, Sui GX, Bhattacharyya D. Synthesis and
characterisation of nanocellulose-based polyaniline conducting
films. Compos Sci Technol 2014; 99: 31-36.
[30] Syverud K, Stenius P. Strength and barrier properties of MFC
films. Cellulose 2009; 16: 75-85.
[31] Martinez-Sanz M, Lopez-Rubio A, Lagaron JM. High-barrier
coated bacterial cellulose nanowhiskers films with reduced
moisture sensitivity. Carbohydr Polym 2013; 98: 1072-1082.