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Study on Nanocellulose by High Pressure Homogenization in Homogeneous

Isolation

Article in Fibers and Polymers · March 2015

DOI: 10.1007/s12221-015-0572-1

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Fibers and Polymers 2015, Vol.16, No.3, 572-578 ISSN 1229-9197 (print version)
DOI 10.1007/s12221-015-0572-1 ISSN 1875-0052 (electronic version)

Study on Nanocellulose by High Pressure Homogenization in

Homogeneous Isolation
Yihong Wang1,2, Xiaoyi Wei2, Jihua Li2,3, Fei Wang2, Qinghuang Wang2,3*, Jiacui Chen2, and Lingxue Kong4
1
College of Food Science and Technology of Huazhong Agricultural University, Wuhan 430070, China
2
Agriculture Products Processing Research Institute, Chinese Academy of Tropical Agricultural Sciences,
Zhanjiang 524001, China
3
National Center of Important Tropical Crops Engineering and Technology Reseach, Haikou 571101, China
4
Institute for Frontier Materials, Deakin University, Victoria 3216, Australia
(Received August 29, 2014; Revised November 16, 2014; Accepted November 22, 2014)

Abstract: Nanocellulose from cotton cellulose was prepared by high pressure homogenization (HPH) in ionic liquids (1-
butyl-3-methylimidazolium chloride ([Bmim]Cl). The nanocellulose possessed narrow particle size distribution, with
diameter range of 10-20 nm. Weight average molecular weight (Mw) of nanocellulose treated by HPH was lower (173.8 kDa)
than the one ILs treated cellulose (344.6 kDa). X-ray photoelectron spectroscopy (XPS), Fourier transform infrared
spectroscopy (FT-IR), and Solid-state CP/MAS 13C NMR measurements were employed to study the mechanism of structural
changes, which suggested that network structure between cellulose chains were destructed by the shearing forces of HPH in
combination with ionic liquids. The intermolecular and intra-molecular hydrogen bonds of cellulose were further destroyed,
leading to the long cellulose molecular chains being collapsed into short chains. Therefore, the nanocellulose could provide
desired properties, such as lower thermal stability and strong water holding capacity. Results indicated that it had great
potential in the applications for packaging, medicines, cosmetics and tissue engineering.
Keywords: Nanocellulose, High pressure homogenization, Homogeneous isolation, Hydrogen bonds, [Bmim]Cl

Introduction reproducibility and ease of scaling up in industry [10], such

as the formation of emulsions to extend the shelf life [11], a
As one of the most abundant material on earth, cellulose is novel approach for the preparation of co-crystals [12] and so
a key constituent and an attractive renewable feedstock for on. In this process, samples is passed at high pressure
mankind’s energy needs [1]. However, cellulosic fibers have through a narrow homogenization gap at a very high velocity
a complex crystalline structure, which is held together via a [13]. Molecular refinement was achieved by application of
network of hydrogen bonds and hydrophobic interactions, shearing forces during high-pressure homogenization, which
making deconstruction of the crystals difficult. For these causes disintegration of large particles into thinner ones [14].
reasons, the development of biodegradable materials, including It can overcome the huge resistance to influence the molar
cellulose-based products, is a subject of great challenge [2]. mass distribution and functionality of macromolecules [15].
By innovative nanotechnology, we can shift the focus from However, this requirement limits the possible scaling-up of
macroscopic properties to the nanoscale and manipulate or production and results in low efficiency and low capacity
self-assemble molecule by molecule to expand the application [16]. In our previous study, we prepared nanocellulose from
of cellulose [3,4]. sugarcane bagasses by high pressure homogenization in a
Currently, there are various viable methods for fabricating homogeneous media. The homogeneous solution was passed
nanocellulose, such as chemical methods [5], biological through a high pressure homogenizer without any clogging
methods [6], physical methods [7], and synthetic methods [17], which could avoid enormous resistance of cellulose in
[8]. However, there are many shortcomings among these solid state. However, owing to its astonishing intrinsic properties,
methods that limit its applications. For example, chemical we do further study to analysis the mechanism of the process,
methods require a strongly acidic or alkaline, which would and to develop this kind of environmental friendly and
contaminate environment. Biological treatment is time efficient materials for different high-value applications.
consuming, costly and expensive. Special equipment and In the present work, cotton cellulose was chosen for raw
over energy consumption [9] are often required in the materials because of its relatively high content of cellulose,
preparation of nanocellulose by physical methods. A highly which can make a model reducing the influence from lignin
desirable feature of a method in fabricating nanocellulose is and hemicellulose. Nanocellulose from cotton cellulose was
eco-friendly and energy saving technology. then isolated by high pressure homogenization coupled with
High pressure homogenization is a conventional approach an ionic liquids pretreatment. The structural and physicochemical
in many technical applications because of high efficiency, properties of the nanocellulose were studied by X-ray
photoelectron spectroscopy (XPS), Fourier transformed
*Corresponding author: qinghuangwang@163.com infrared (FT-IR) spectra, Solid-state CP/MAS 13C NMR

572
Study on Nanocellulose by High Pressure Homogenization Fibers and Polymers 2015, Vol.16, No.3 573

measurements, rheological measurement and transmission X-ray Photoelectron Spectroscopy (XPS) Measurements
electron microscopy (TEM). The mechanical principles and XPS measurements analysis was conducted on a spectrometer
changes in conformation of nanocellulose were also analyzed. (Thermo VG Multilab 2000) using an Al Ka X-ray source
On the basis of these investigations, a possible mechanism and charge neutralizer. Survey spectra and high resolution
of nanocellulose by high pressure homogenization in scans were acquired with pass energies of 160 eV and 20 eV,
homogeneous isolation was proposed. respectively. All spectra were energy referenced to the
valence band and C 1s CHx environment at 285 eV. All
Experimental sample transfers were made in air. The curve fitting for
component peaks was carried out with a nonlinear least-
Materials and Reagents squares algorithm using a mixture of Gaussian and Lorentzian
Defatted cotton cellulose was obtained from Gauke (Hubei) peak shapes.
Cotton Supplies Co., Ltd. with the proportion of cellulose of Fourier Transform Infrared Spectrometry (FT-IR)
98 %. Ionic liquids 1-butyl-3-methylimidazolium chloride Measurements
([Bmim]Cl) was synthesized according to the previous work The dried samples from original cellulose, ILs treated
[17]. The purity of the obtained [Bmim]Cl was verified in cellulose and nanocellulose were analyzed with a Spectrum
terms of NMR and FT-IR analysis. All other reagents and GX-1, PerkinElmer, USA spectrometer to observe the
chemicals are of analytic grade. changes in the chemical bonds and structure. The spectra
(4000-400 cm-1) were recorded with a resolution of 1 cm-1
Nanocellulose Preparation and 64 scans per sample. About 2 mg samples were prepared
Nanocellulose was prepared according to our previous by mixing with 120 mg of spectroscopic grade KBr then
work [18]. Defatted cotton cellulose was cut into pieces, and compressed to form a disc.
then pretreated by 1 % sodium hydroxide solution before Solid-state CP/MAS 13C NMR Measurements
use. The 1 % (w/w) cotton cellulose/[Bmim]Cl solution was Solid-state 13C NMR spectra were recorded on an Infinity
stirred in the microwave oven (Qpro-M, Questron Inc., Plus 400 spectrometer (Varian; magnetic field: 9.4 T, 13C
Canada) at 110-150 oC for several minutes under magnetic frequency: 100.12 MHz) with a CP-MAS unit at room
stirring, until cellulose was completely dissolved to form a temperature. The spinning rate and contact time were 5.0 kHz
clear and viscous solution. After completely dissolution, the and 1.0 ms, respectively. The pulse width was 2.10 μs, the
cellulose/[Bmim]Cl solution was cooled to 80 oC. And then spectral width was 50.00 kHz. The 13C NMR spectra of
it was homogenized by a high pressure homogenizer (AH100D, samples were recorded for 2000 scans with a pulse delay of
ATS Engineering Inc., Canada) at pressure levels ranging 20.48 ms in order to obtain reliable integrations.
from 40 MPa to 140 MPa for up to 50 cycles. Deionized Rheological Experiments
water was rapidly added to the stirred cellulose/[Bmim]Cl Rheological characterization of cellulose/[Bmim]Cl solution
solution (distilled water-to-cellulose/[Bmim]Cl solution was carried out in a controlled-stress (Rheoscope, ThermoHaake,
ratio of 5:1), and then washed and centrifuged. Finally, the Germany) rheometer, using parallel-plate geometry (60 mm
regenerated cellulose was dried in a vacuum freeze drying diameters, 1 mm gap). Small-amplitude oscillatory shear
equipment until reaching a constant weight. (SAOS) tests were performed inside the linear viscoelastic
region, in a frequency range of 0.1-100 rad s-1. The experimental
Measurements temperature was mainly set at 40 oC. At least two replicates
Photon Correlation Spectroscopy (PCS) Measurements of each test were carried out on fresh samples. In the studied
Particle size distributions were obtained using a photon shear rate ranges, non-Newtonian behavior was described by
correlation spectroscopy (Malvern Instruments, UK). The the fitting of the experimental data (apparent viscosity-shear
aqueous solution of nanocellulose was treated by ultrasound rate) with the power law equation:
for 5 min. And then the solution was cooled to room n–1
η = Kγ· (1)
temperature. Particles size was performed by the analysis of
the intensity autocorrelation function. where K is the consistency coefficient, γ· is the shear rate (s-1)
Transmission Electron Microscopy (TEM) Measurements and n is non-Newtonian index. The plot of ln(η) against
Transmission electron microscopy (TEM) was performed ln( γ· ) for equation (1) should give a linear relationship, from
on a JEM-100 (JEOL, Tokyo, Japan) with acceleration which n can be determined from the slope [19].
voltage of 100 kV. Nanocellulose was treated by HPH were Gel Permeation Chromatography (GPC) Measurements
deposited from an aqueous dilute dispersion and casted one The gel permeation chromatography (GPC) with manual
drop onto copper grid with carbon film support. Samples injector included a G1311B 1260 Quat Pump and a differential
were observed directly with TEM after it was dried under refractometer detector. Prior to injection, samples and
20 oC without further staining. mobile phase (DMAc/0.5 % LiCl) were filtered through a
574 Fibers and Polymers 2015, Vol.16, No.3 Yihong Wang et al.

PTFE membrane filter. The following parameters were used [Bmim]Cl solution was passed through high pressure
for GPC measurements: flow: 1.00 ml min-1; columns: X- homogenizer to prepare nanocellulose.
stream 104, 105; injection volume: 100 μl; run time: 36 min. The particle size distributions of cellulose are directly
Eight polystyrene standards of narrow polydispersity, i.e., proportional to the homogenization pressure and the number
4,910 Da, 10,440 Da, 28,770 Da, 74,800 Da, 139,400 Da, of homogenization cycles (Figure 1). The mean particles
473,600 Da, 1,390,000 Da and 2,704,000 Da (Polymer sizes of nanocellulose at different cycles are shown in Figure
Laboratories, Church Stretton, UK) were used to calibrate 1(a). It could be seen that the diameter of nanocellulose
the columns. The linear coefficient of determination (r2) exhibited a significant reduction from 3500 nm to less than
between the weight average molecular weight (Mw) of the 1300 nm after only 10 cycles. In the following cycles, the
standards and elution time was 0.99. Data acquisition and reduction rate continued to decrease. And after 30 cycles, it
processing were done by using High Resolution Data Acquisition was down to a plateau with a 610 nm value. Polydispersity
System. The results were obtained with triplicate injections of nanocellulose dispersions was no more than value of 0.3
of the two separately prepared solutions. during the HPH process, indicating that nanocellulose treated
by HPH had a stable and narrow particle size distribution.
Results and Discussion Figure 1(b) shows the mean particles sizes of nanocellulose
at different pressure levels for 30 cycles. The value of
Preparation of Nanocellulose particle sizes decreased with the increasing homogenization
The cotton cellulose was dissolved in [Bmim]Cl to form a pressure. However, if more cycles or higher pressure involved,
homogeneous solution. The cellulose/[Bmim]Cl solution temperature of solution would be increased, causing a
was heated with exceptional efficency by microwave oven degradation of cellulose [20-22]. In terms of economical
because the degradation of cellulose could be avoided at
high temperature for a short time. Then the cellulose/

Figure 1. The mean particle sizes on different conditions; (a) Figure 2. TEM of ILs treated cellulose and nanocellulose at a
operation from 10 cycles to 50 cycles at pressure of 80 MPa and pressure of 80 MPa with 30 cycles; (a) ILs treated cellulose and
(b) pressure from 40 MPa to 120 MPa. (b) nanocellulose.
Study on Nanocellulose by High Pressure Homogenization Fibers and Polymers 2015, Vol.16, No.3 575

factor, the optimum condition of HPH was at a pressure of and relative content is C 1s2, which represents carbon singly
80 MPa with 30 cycles. bound to oxygen, i.e. hydrogen-type species. More detailed
Typical microstructures of a dilute suspension of ILs surface composition analysis of different samples were
treated cellulose and nanocellulose are shown in Figure 2. shown in the high resolution C 1s2 XPS spectra in Table 2.
Clearly, the nanocellulose (Figure 2(b)) was circular-like in The binding energy of the signal for samples -C-O-
shape with a size of 10-20 nm, which is much smaller than backbone carbon atoms shifts from 286.54 eV for original
the ones of ILs treated cellulose (Figure 2(a)). Interestingly, cellulose to 285.95 eV for ILs treated cellulose. It might be
the self-aggregated nanocellulose particles were independent because the hydrogen atoms of molecular hydrogen bonds
from each other. It can be in accordance of a steady value of was replaced by the cationic of ionic liquid, which moved to
0.3 for polydispersity of nanocellulose dispersions. a higher binding energy [24]. In the other hand, the binding
energy of the nanocellulose is the same as the one of ILs
Structure Analysis of Nanocellulose treated cellulose. It suggested that ILs appear to be solvents,
The previous results [18] showed that the crystallinity presumably solubilizing cellulose through hydrogen bonds
index (original cellulose, ILs treated cellulose and nanocellulose from hydroxyl functions to the chloride of [Bmim]Cl
were 60.16 %, 40.71 % and 32.62 %, respectively) of nano- [25,26]. In addition, the number of hydroxyl shifts from
cellulose decreased. A similar trend is also observed for 9.74 % for the original cellulose to 22.16 % for the nanocellulose.
thermal decomposition temperatures values, which were The increase of hydroxyl is due to the increasing of free
339 oC, 290 oC, and 287 oC for the original cellulose, ILs hydrogen bonds [27], which might be because cellulose
treated cellulose and nanocellulose, respectively. Moreover, chains were destructed by the interplay of the shearing
the water-holding capacity (WHC) for cellulose was forces and anions of ILs during the HPH process.
3.5±0.10 ml g-1; while, the one for nanocellulose was 6.4± FT-IR: Fourier Transform Infrared Spectrometry
0.10 ml g-1. To understand the changes in supramolecular Measurements
structure of cellulose under homogeneous liquid state by Figure 3 shows the FT-IR spectra of three samples. The
HPH, the morphological and chemical characteristics of bands of original cellulose at 3425 cm-1 was assigned to the
original cellulose, ILs treated cellulose and nanocellulose covalent hydrogen bonds [28]. The band of nanocellulose
were further analyzed by measuring rheological measurements, shifted to a higher wave number, indicating that the O-H
XPS, GPC, FT-IR spectroscopy and CP/MAS 13C NMR. vibration modes are either free or weakly hydrogen bonds
XPS: X-ray Photoelectron Spectroscopy Measurements [29,27] during cellulose treated by HPH. It was verified by
X-ray photoelectron spectroscopy measurements is used the results of XPS measurements.
in many investigations of surface chemical analysis of raw, The absorption band at 1452 cm-1 in original cellulose was
scoured and hydrogen peroxide bleached cotton material assigned to the intra-molecular hydrogen bonds involved in
[23]. The surface composition of three samples were investigated the O(3)H-O(5) [29-31]. Intensity of bands became weak
by XPS in Table 1. and shifted down to 1426 cm-1 after HPH, indicating that
The C 1s peak is de-convoluted into three subpeaks, intra-molecular bond (O(3)H-O(5)) was destroyed by the
C 1s1, C 1s2, C 1s3. The notable change of binding energy

Table 1. XPS analysis of three samples in the C 1s2 binding energy

(B.E.) region
Binding energies and
Sample O C peak area (%)
C 1s2; at. %
Original cellulose 32.49 55.47 286.54 9.74
IL treated cellulose 36.67 62.87 285.95 16.92
Nanocellulose 39.42 60.39 285.94 22.16

Table 2. Comparison of 13C chemical shifts of three samples

Chemical shifts (ppm)
Samples
C1 C4 C3, C5, C2 C6
Original cellulose 105.29 89.21, 85.22, 75.14, 71.89 65.0
83.71
IL treated cellulose 105.28 84.15 74.77 62.75 Figure 3. FT-IR spectra of samples; (a) original cellulose, (b) ILs
Nanocellulose 105.16 84.12 74.92 62.73 treated cellulose, and (c) nanocellulose.
576 Fibers and Polymers 2015, Vol.16, No.3 Yihong Wang et al.

interaction of shearing forces and ILs.

The peaks at 1022 cm-1 and 1060 cm-1 in original cellulose
represented C-O valence vibration. The split between two
peaks decreased when cellulose was treated by HPH, which
means that the sum and difference of two n C-O vibrations
localized on two adjacent hexose rings had changed [27].
This change of splitting could be resulted from the cleavage
of glycosidic bond [9,27,30], leading to the fracture of
molecular chains. In addition, the peak 1160 cm-1 decreased
when the nanocellulose was treated by HPH , which derived
from skeletal stretching vibrations (including C-O-C bridge
stretching) [30], was another evidence of the glycosidic
bond breakage between cellulose chains.
NMR: Solid-state CP/MAS 13C NMR Measurements
Figure 4 shows the solid-state CP-MAS 13C NMR spectra
for three samples, and the assignment of the spectra is given Figure 5. Rheological properties of cellulose/[Bmim]Cl solution;
in Table 2. The single at the C3, C5, C2 signals of (a) dissolution of cellulose/[Bmim]Cl and (b) dissolution of
nanocellulose is considered to the equivalent anhydroglucose cellulose/[Bmim]Cl treated by HPH.
residues along the cellulose chains [32].
The 13C NMR spectrum shows a clear difference at the C4 with and without treating by HPH were investigated by
signal position which assigns to O(3)H-O(5) intra-molecular steady shear sweep experiments in Figure 5. From the figure,
hydrogen bonds. The C4 peak for nanocellulose was displaced it showed that the solution systems gave a shear thinning
to a higher magnetic field. The reason may be that intra- behavior, which suggested that cellulose/[Bmim]Cl solution
molecular hydrogen bonds of cellulose chains was destroyed was pseudo-plastic fluid.
by the shearing forces in cooperation with the anions of ILs, Rheological properties of cellulose/[Bmim]Cl solution
which are consistent with the results of FT-IR measurements. with different structures could be obtained by calculating the
The peak C6, intra-molecular hydrogen bonds O(2)H- non-Newtonian index. According to the eq1, non-Newtonian
O(6), shifted toward a higher magnetic field when cellulose index of the homogeneous solution with and without treating
dissolved in [Bmim]Cl. It suggested that t-g conformation of by HPH were 0.9507 and 0.8345, respectively. The results
the C6-OH group (for cellulose I) changed into a g-t showed that cellulose/[Bmim]Cl solution treated by HPH
conformation (for cellulose II) with the simultaneous formation was almost close to Newtonian fluid due to the destroyed
of intra-molecular hydrogen bonds O(2)H-O(6) [33]. entanglement of cellulose chains, which was damaged by
Rheological Properties the mutual action of the shearing forces from high pressure
The complex viscosity of cellulose/[Bmim]Cl solution homogenization and the anions of ILs. Moreover, at the same
temperature, when the flow index (n) increased, the
solutions became less pseudo-plastic (higher n values). It
was suggested that the ability of cellulose chains motion of
the cellulose/[Bmim]Cl solution was enhanced and the
resistance between molecular chains decreased. In addition,
changes in the structure of cellulose caused by cellulose
gegradation will be ignored, according to Delmotte et al.
[34]. Therefore, it might be the tangles of cellulose chains
[16] and the formation of a continuous cellulose network
was destroyed by the interaction of shearing forces with ILs
during the high pressure homogenization process. It was
further confirmed by the results of XPS, FT-IR spectroscopy
and CP/MAS 13C NMR measurements.

Table 3. Gel permeation chromatograms of three samples

Samples Mw×104 Mn×104 Mp×104 PD
Original cellulose 97.04 18.87 32.81 5.14
Figure 4. Comparison of 13C chemical shifts of three samples; IL treated cellulose 34.46 8.26 29.74 4.17
(a) original cellulose, (b) ILs treated cellulose, and (c) nanocellulose. Nanocellulose 17.38 3.82 21.61 4.55
Study on Nanocellulose by High Pressure Homogenization Fibers and Polymers 2015, Vol.16, No.3 577

GPC: Gel Permeation Chromatography Measurements hydrogen bonds of cellulose were further destroyed, leading
In order to clarify the effects of high pressure homogenization to the long molecular chains being collapsed into short
on supramolecular structure of cellulose, weight average chains through the shearing forces of HPH with ILs
molecular weight of three samples were analyzed in Table 3. incorporating anions. The results of XPS measurements, FT-
Weight average molecular weight of nanocellulose significantly IR measurements and Solid-state CP/MAS 13C NMR
decreased, which gave cause for the decreasement of the measurements further supported the observation. Incorporation
homogeneous solution treated by HPH in viscosity [2]. of these desired properties into applications, is currently in
Molecular hydrogen bonds between cellulose chains was progress.
destroyed by the interaction of the shearing forces from high The HPH process brought about the changes in the
pressure homogenization and the anions of ILs is a major physical and morphological structure of cellulose, and thus
cause of decreasement in weight average molecular weight, leading to the desired properties. For example, nanocellulose
which was due to that cellulose degradation is very slight is applied to nanocellulose-containing composites due to the
and degradation will occur only on cellulose’s C3 and C5 degree of nanodispersion of cellulose in diverse solvents.
but not on the C1 and C4 of the aromatic nuclei [34]. It is in Experimental results show that crystallinity and weight
agreement with the previous findings that cellulose chains average molecular weight of nanocellulose treated by HPH
were broken by the shearing force from HPH [17]. were reduced. It will expand the application in cosmetics
Additionally, the results of FT-IR and CP/MAS 13C NMR coupled with other fillers or coating agents [35,36].
measurements further supported that intra-molecular bond
(O(3)H-O(5)) of nanocellulose was destroyed by the Acknowledgments
interaction of shearing forces of HPH with ILs.
We great acknowledge financial support by the Fundamental
Mechanism Study Scientific Research Funds for Chinese Academy of Tropical
Agricultural Sciences (1630062013012), the Prior Special
Cellulose chains were permeated by anionic of [Bmim]Cl Fund for Chinese Central Government 948 Research program
when cellulose dissolved in [Bmim]Cl. The hydrogen bonds (2012-Z10), and the Chinese National Engineering Research
between cellulose chains were attacked by anionic of [Bmim]Cl. Center building program (2011FU125Z09). This work is
The disorder of cellulose structure was transformed to the also supported by Major Science and Technology Projects of
order of cellulose structure, and the homogeneous solution Hainan Province (ZDZX2013023-3).
was obtained. Upon high-pressure homogenization, con-
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