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Cellulose-based aerogel from Eichhornia crassipes

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as an oil superabsorbent
Cite this: RSC Adv., 2016, 6, 98563
Tiantian Yin, Xinying Zhang, Xiaoyan Liu,†* Beibei Li and Chaoqun Wang

Received 14th September 2016
Accepted 5th October 2016
DOI: 10.1039/c6ra22950f
www.rsc.org/advances
Cellulose-based aerogels (CBAs) were prepared based on Eichhornia crassipes as a raw material and a paper
wet-strengthening agent as a cross-linker via a green and simple process. The hydrophobic CBAs had
excellent properties, including low density (<0.0055 g cm
3), high porosity (>99.6%), excellent oil/solvent
sorption capacities (58.06–101.14 g g
1), superhydrophobicity (water contact angle as high as 154.8 ),
and superior elasticity. Moreover, the absorbed oil could be quickly recovered by squeezing, and the oil
sorption capacity was still as high as 75% of the original sorption capacity after 16 cycles. This work
provides a facile and cost-effective method to fabricate a novel superabsorbent from waste biomass
materials, which is very promising in terms of using waste to deal with oil pollution.

complicated synthetic procedures of inorganic aerogels and the

Introduction
Water pollution caused by oil spills has become one of the most
serious disasters due to its severe threat to the marine
ecosystem.1,2 Thus, it is vital to choose appropriate strategies for
collecting oil completely from water in time. Among the existing
measures used for oil recovery, physical adsorption is generally
considered as an effective and promising method, due to its
low-cost and convenience of operation.3,4 At present, various
materials have been used for oil sorption, including inorganic
mineral materials, organic synthetic products and organic
natural materials.5,6 Compared with the inorganic and synthetic
organic adsorbents, natural organic adsorbents have received
widespread attention because of their higher biodegradability,
high biomass and cost effectiveness. High oil sorption capa-
bility is one of the most important criteria when choosing oil
sorption materials, and mainly depends on the storage space of
materials.7 However, the low storage space as well as the
insufficient buoyancy of most natural organic materials limited
their further application. Even so, there is a growing demand for
synthesizing oil superabsorbents based on renewable and
sustainable natural organic materials.
Owing to its low density and high porosity, aerogels have
been extensively investigated. Various types of aerogels can be
classied into two typical groups: inorganic aerogels (e.g., SiO2,8
carbon nanotubes9 and graphene10–12) and organic aerogels (e.g.,
polypropylene13 and cellulose14–17). Besides high oil sorption
capability, an ideal sorbent should be low-cost, renewable and
easily fabricated. Among them, expensive raw materials or
College of Environment and Chemical Engineering, Shanghai University, Shanghai
200444, PR China. E-mail: lxy999@shu.edu.cn; Fax: +86 21 66137761; Tel: +86 21
66137767
† Current address: College of Environment and Chemical Engineering, Shanghai
University, No. 99, Shangda Road, Baoshan District, 200444, Shanghai, China.
slow degradation of aerogels that are based on synthetic poly-
mers (e.g., polypropylene13) have limited their widespread
application. Therefore, cellulose-based aerogels appear to be
a promising sorbent considering that cellulose is a cheap and
abundant source, and due to their high structural exibility and
good mechanical properties.18–22 For achieving cellulose-based
aerogels, several efforts have been made using some cellulose
solvents, e.g., alkaline/urea,23 NaOH/PEG aqueous solutions,24
a hydrothermal process (KOH, 3 mol L
1)25 and ionic liquids
(AmImCl).18 However, the above preparation processes use
a large amount of chemicals and produce alkaline and acidic
waste. Even though ionic liquids as green cellulose solvents
were introduced to fabricate cellulose aerogels, the expenditure
of ionic liquids is still too expensive to use in industrial
manufacturing.
Herein, a cost-effective and environmentally friendly
method is reported to prepare cellulose-based aerogels (CBAs)
by using Eichhornia crassipes as a raw material and a paper wet-
strengthening agent (the effective component is 12.5 wt%
polyamide epichlorohydrin resin, PAE) as a cross-linker. Using
Eichhornia crassipes as a starting material for the synthesis of
aerogels provides the possibility of being able to recycle these
aquatic plants, thereby reducing any heavy burden on the
environment. PAE is commonly used in the papermaking
industry as it can signicantly enhance the wet-strength of the
paper.26 Thus, PAE can be directly used in cellulose-based
aerogels without any pretreatment and can signicantly
reduce the use of solvent and the entire synthesis duration.
Through a combination of freezing, freeze-drying and subse-
quent hydrophobic modication, cellulose-based aerogels
(CBAs) that have good exibility, high porosity, super-
hydrophobicity and outstanding oil sorption capabilities
were obtained.

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Materials and methods
Materials
Eichhornia crassipes was harvested from the waterways of
Shanghai, China. Methyltrimethoxysilane (98%, MTMS), and
other chemicals including benzene, absolute ethyl alcohol,
sodium chlorite, glacial acetic acid, sodium hydroxide and
hydrochloric acid were all of analytical reagent grade and were
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purchased from Shanghai Sinopharm Chemical Reagent Co.,
Ltd, China. The paper wet-strengthening agent (effective
component is 12.5 wt% polyamide epichlorohydrin resin, PAE)
was supplied by Jiangsu Si Lida Chemical Co., Ltd, China.
Deionized water was self-made in the laboratory. Crude oil
(density at 20  C ¼ 0.6770 g cm
3, viscosity ¼ 0.994 mm2 s
1)
was supplied by the China National Offshore Oil Corporation.
Diesel oil (density at 20  C ¼ 0.82 g cm
3, viscosity ¼ 6.51 mm2
s
1), soybean oil (density at 20  C ¼ 0.93 g cm
3, viscosity ¼ 7.26
mm2 s
1), lubricating oil (density at 20  C ¼ 0.79 g cm
3,
viscosity ¼ 47–57 mm2 s
1) and silicone oil (density at 20  C ¼
0.96 g cm
3, viscosity ¼ 95 mm2 s
1) were purchased from the
local market, Shanghai, China.
Purication of cellulose from Eichhornia crassipes
The harvested plant samples were washed and sun-dried. The
stalks of Eichhornia crassipes were ground and then screened.
Powder with 40 mesh was used for the preparation of cellulose.
The purication of cellulose was determined according to the
procedures described by Shaoliang Xiao et al.27 Briey, 10 g of
dried powder was extracted with benzene/ethanol (2 : 1, v/v) at
90  C for 6 h in a Soxhlet extractor. Next, the treated sample was
air-dried and treated with 600 mL 1 wt% NaClO2 solution (pH ¼
4–5 adjusted by glacial acetic acid) at 75  C for 5 h. The sample
was washed with deionized water and then immediately treated
with 250 mL 2 wt% NaOH at 90  C for 2 h. Thereaer, the
sample was collected and washed with deionized water again
before being treated with 300 mL 1 wt% HCl at 80  C for 2 h.
Finally, the puried cellulose was collected and stored in
Fig. 1 The schematic and preparation process of CBAs. (a) Schematic of the fabrication process, (b) cellulose, (c) PAE, (d) frozen solid, (e) freeze-
dried solid and (f) an ultralight CBA on a flower after cross-linking reaction at 120  C.
98564 | RSC Adv., 2016, 6, 98563–98570
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a refrigerator at 4  C before use. To avoid the generation of
strong hydrogen bonding among the cellulose bers, the
sample was kept in a water-swollen state during the whole
chemical process.
Preparation of the CBAs
The preparation process and a schematic of the CBAs are
illustrated in Fig. 1. A mixture of an aqueous suspension of
cellulose bers (0.35, 0.50, 0.75 and 1.00 wt%) and PAE (20–60
wt% of dry cellulose bers) (Fig. 1a and c) was violently stirred
for 15 min. Next, the suspension was poured into a 150 mL glass
beaker and sealed with a plastic wrap. The samples were then
placed into a low temperature thermostat at
15  C for 24 h to
allow them to form solids. Aerwards, the frozen samples were
freeze-dried at
35  C for 48 h. Finally, the freeze-dried
cellulose-based aerogels were kept at 120  C for 3 h to
strengthen the crosslinking among the cellulose bers.
Hydrophobic coating of CBAs
A tightly sealed glass bottle containing 1 mL MTMS, 1 mL H2O
and the samples was placed in an oven at 80  C for 4 h. Then,
the silanized samples were taken out and placed in a vacuum
oven for 24 h at 60  C to remove any excess MTMS. Aer that,
hydrophobic CBAs were obtained. The CBA synthesized under
different conditions was marked as xCBAy, where x and y denote
the ber content and PAE concentration, respectively.
Characterizations
The surface morphology of the samples coated with Au was
examined using Scanning Electron Microscopy (SEM, SU-1510,
Hitachi Ltd, Japan). The FTIR spectra of the samples were
recorded on a NICOLET-380 spectrometer (Thermo Fisher
Scientic, USA). Contact angle measurements of the samples
treated with MTMS were carried out using a drop of water (3 mL)
or diesel oil (10 mL) (OCA30, Dataphysics, Germany).
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Density and porosity of CBAs

The density (r, g cm
3) and porosity (%) of the unmodied
CBAs were calculated according to the following formula (1)
and (2):

r ¼ m/V (1)

Porosity ¼ (1
r/rc)  100 (2)

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where m and V represent the mass and volume of the CBAs and
rc is the density of crystalline cellulose (1.528 g cm
3).20,23

Oil sorption capacity experiments

To determine the sorption capacity of the MTMS treated aero- Fig. 2 Density and porosity of unmodified CBAs as a function of
gels, this test was performed in various oils (crude oil, diesel oil, cellulose concentration.
soybean oil, lubricating oil and silicone oil) and organic
solvents (toluene, n-hexane, trichloromethane, acetone and
sorption due to the hydrophilicity of the cellulose bers. As
ethanol). A weighed sample (about 0.03 g) was put into a stain-
shown in Fig. 3a, a water droplet was immediately absorbed by
less-steel mesh, and the sample and mesh were immersed
the unmodied CBAs within 0.2 s, and the water contact angle
together into the oil for 5 min. Then, the sample and mesh were
was nearly 0 . On the contrary, the water droplet exhibited
taken out from the oil together and drained for 2 min before the
a typical spherical shape on the outside and remained on the
weight measurement. The oil sorption capacity can be referred
surface of the MTMS-modied CBAs aer 60 s, while the diesel
to as the weight gain dened by the mass of absorbed oil per
oil droplet could immediately penetrate the MTMS-modied
unit mass of dry sample. This measurement was repeated three
CBAs in less than 0.2 s (Fig. 3b–d). Moreover, the water
times and the average value was presented.
contact angle and oil contact angle were 154.8 and 0 (Fig. 3b
and c), indicating the combined superhydrophobic and oleo-
Recyclability of CBAs philic features of the MTMS-modied CBAs. As shown in Fig. 3f,
Aer oil absorption by the CBAs, the absorbed oil was recovered a piece of superhydrophobic CBA could easily absorb chloro-
by simple mechanical squeezing (a 200 g balance weight), and form that was dyed with Sudan III from underwater without any
the remnant oil in the squeezed CBAs was weighed. Then the water being absorbed, further conrming the good hydropho-
squeezed CBAs were allowed to absorb oil again and the oil in bicity of the MTMS-modied CBAs.
the CBAs (adsorbed oil) was measured again. This process was
repeated several times to characterize the recyclability of the
CBAs.

Results and discussion

Characterizations
Light-weight (Fig. 1f) and porous CBAs were successfully
prepared via a green and facile method. Fig. 2 describes the
density and porosity of the CBAs before modication as
a function of the cellulose content and PAE concentration.
Irrespective of the PAE concentration, the density of the CBAs
can reach as low as 0.0055 g cm
3 (i.e., 0.35CBA10), and the
porosity can be as high as 99.6% (i.e., 0.35CBA10) with
decreasing cellulose concentration from 1.00 wt% to 0.35 wt%.
At the same cellulose content, the density of the CBAs increased
with an increase in the PAE concentration, while the porosity
decreased. This shows that the density and porosity were Fig. 3 The wettability of the CBAs. Water contact-angle measure-
inuenced by the cellulose content and PAE concentration. In ments of (a) unmodified CBAs and (b) MTMS-modified CBAs. (c) Diesel
short, the prepared CBAs with high porosity (98.6–99.6%) and oil contact-angle measurements of the MTMS-modified CBA at room
low density (0.0055–0.021 g cm
3) are lightweight materials, temperature. (d) Water and diesel oil were dropped onto the surface of
the MTMS-modified CBA. (e) Water was dropped onto the inner
indicating that the CBAs would be able to oat well on the water
surface of the MTMS-modified CBA. (f) Chloroform was absorbed by
surface aer absorbing oil (see below). the MTMS-modified CBA from underwater (water dyed with copper
The wettability of the CBAs is shown in Fig. 3. Before being sulfate, diesel oil and chloroform dyed with Sudan III, for clear
modied by MTMS, the CBAs could not be directly used for oil presentation).

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Fig. 4FTIR spectra of the (a) unmodified CBA and (b) MTMS-modified CBA, and the EDS spectra of the (c) unmodified CBA and (d) MTMS-
modified CBA.
The FTIR spectra of the unmodied CBAs and modied
CBAs are presented in Fig. 4a and b. Aer modication with
MTMS, the vibrations of the C–H of Si–CH3 groups were iden-
tied at 2964 cm
1.28 The bands at 1270 and 854 cm
1 were
assigned to the Si–C bonds29 and the Si–O–Si stretching vibra-
tion was also observed at 777 cm
1.20,29 The peak intensity of the
O–H stretching at 3336 cm
1 decreased, indicating a successful
silanization reaction between the abundant hydroxyl groups of
the bers and MTMS. The successful silanization on the CBAs
was also conrmed by the energy dispersive X-ray spectrum
(EDS) (Fig. 4c and d). Compared with the unmodied CBAs, the
EDS spectrum of the modied CBAs shows a sharp silicon peak
and the relative silicon atomic weight percentage was 16.21%.
Fig. 5 SEM micrographs of (a) unmodified 0.35CBA40 (500), (b) unmodified 0.35CBA40 (200), (c) MTMS-modified 0.35CBA40 (500) and (d)
MTMS-modified 0.35CBA40 (200).
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Scanning electron microscope (SEM) images show that the
CBAs are porous and have interconnected three-dimensional
network structures with a pore size of around 100–200 mm
(Fig. 5). To avoid the collapse of the structures due to moisture
being absorbed by the cellulose, the freeze-dried CBAs were
modied with MTMS to improve their hydrophobicity and
retain the porous structure of the samples. The morphologies
of the CBAs before and aer hydrophobic modication are
shown in Fig. 5, and there were no signicant changes
observed aer hydrophobic modication. This indicated that
the silanizing modication had little affect on the structures of
the CBAs.
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Fig. 6(a) Effect of cellulose content (0.35, 0.50, 0.75 and 1.00 wt%) on the oil sorption capacities of the CBAs with 40 wt% PAE. (b) Effect of PAE
concentration (10, 20, 40 and 60 wt%) on the oil sorption capacities of the CBAs with 0.35 wt% cellulose.

Effects of the cellulose content and PAE concentration on the
oil sorption of hydrophobic CBAs
The effect of cellulose content (0.35, 0.50, 0.75 and 1.00 wt%) on
the oil sorption capacities of the CBAs with 40 wt% PAE for
crude oil, diesel oil and lubricating oil is shown in Fig. 6a.
Obviously, with an increase in the cellulose content from 0.35 to
1.00 wt%, the oil sorption capacities for crude oil, diesel oil and
lubricating oil decreased signicantly from 62.69 to 39.53 g g
1,

Fig. 7 (a) Compressing–release processes of hydrophobic 0.35CBA40 in the oil system. The diesel oil sorption capacities of (b) 0.35CBA10, (c)
0.35CBA20, (d) 0.35CBA40 and (e) 0.35CBA60 as a function of cycle number.

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78.03 to 46.33 g g
1 and 90.04 to 54.93 g g
1. It could be

concluded that the CBAs with the lowest cellulose content
possessed the highest oil absorption capacities, due to the
lowest density (0.0068 g cm
3) and highest porosity (99.56%)
being obtained at the lowest cellulose content level (i.e.,
0.35CBA40).
The presence of PAE played an important role in facilitating
the formation of the three-dimensional structures of the aero-
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gels, thus impacted the oil sorption capacities. The effect of PAE
concentration (10, 20, 40 and 60 wt%) on the oil sorption
capacities of the CBAs with 0.35 wt% cellulose is depicted in
Fig. 6b. Notably, the oil sorption capacities of 0.35CBA10,
0.35CBA20, 0.35CBA40 and 0.35CBA60 for oil decreased signi-
cantly with increasing PAE concentration from 10 to 60 wt%.
For example, the oil sorption capacities of 0.35CBA10, 0.35CBA20,
0.35CBA40 and 0.35CBA60 for lubricating oil were 106.54, 106.49,
90.04 and 80.10 g g
1, respectively. This showed that the CBAs
with lower PAE concentrations possessed higher sorption
capacities, which could be attributed to the higher porosity and
lower density.

Recyclability
The choice of a suitable material for practical applications not
only depends on the high oil sorption capacity but also the
recyclability of the sorbents. Fig. 7 shows the recyclability of the
CBAs by studying the weight change of saturated absorbed oil.
In this work, a simple squeezing method was selected to recover
the absorbed oil, mainly due to the fact that the oil absorbed by
the CBAs could be easily recovered through squeezing, and the
squeezed CBAs could be reused at once. The rst compression/
release process using the squeezing method is represented in
Fig. 7a, with negligible changes being found on the morphology
of 0.35CBA40, suggesting the excellent mechanical properties
and elasticity of the aerogel. The use of PAE enhanced the
mechanical strength and exibility of the materials, and
increased the reusability of the materials. The sorption capac-
ities of 0.35CBA10, 0.35CBA20, 0.35CBA40 and 0.35CBA60 for diesel
oil as a function of the cycle number are exhibited in Fig. 7b–e.
Aer 16 compression/release cycles, there is still about 50%,
59%, 75% and 77% of the initial sorption capacity remaining
for 0.35CBA10, 0.35CBA20, 0.35CBA40 and 0.35CBA60, and the
Fig. 8 (a) Absorption process of a piece of hydrophobic 0.35CBA40
corresponding sorption quantity capacities were 45.60, 51.88,
with diesel oil. (b) Sorption capacity (g g
1) of hydrophobic 0.35CBA40
58.61 and 51.08 g g
1, respectively. The changes in the sorption for various oils and organic solvents. (c) Sorption capacity (mL g
1) of
capacities of 0.35CBA10, 0.35CBA20, 0.35CBA40 and 0.35CBA60 hydrophobic 0.35CBA40 for various oils and organic solvents.
aer 16 cycles were due to the different mechanical properties
of the CBAs caused by the different PAE concentrations. For
organic pollutants. Fig. 8a shows the sorption process of a piece
a comprehensive consideration of the oil sorption capacities
of hydrophobic CBA with diesel oil that was oating on the
and mechanical properties of the CBAs, the CBAs prepared with
water. It is noteworthy that the oil could be completely absorbed
0.35 wt% cellulose and 40 wt% PAE (0.35CBA40) were the best
within 10 s and without any oil release or water absorption, and
samples. For the convenience of the research, 0.35CBA40 was
the CBAs saturated with oil can oat well on the water surface
selected in the subsequent experiments.
due to their low density and hydrophobicity. Furthermore, the
water contact angle of the CBAs dropped to 113.1–128.8 aer
Oil absorption performance 16 cycles, which means that the recycled CBAs still hardly
The lightweight properties, porous structures, super- adsorbed water in an oil–water mixture.
hydrophobicity and excellent recyclability of the CBAs make For practical applications, an ideal oil sorption material
them an ideal candidate for the sorption of oils and other should be very good at dealing with all kinds of oil pollution.

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The sorption capacity of hydrophobic 0.35CBA40 for a series of
commonly used oils and organic solvents was investigated
(Fig. 8b). Obviously, 0.35CBA40 exhibited a rather high absorp-
tion capacity for the oils and organic solvents, ranging from
58.06 to 101.14 g g
1. For example, the sorption capacities of
hydrophobic 0.35CBA40 for crude oil, diesel oil, soybean oil,
lubricating oil and silicone oil were 62.69, 77.03, 81.32, 88.04
and 94.00 g g
1 respectively. The excellent sorption capacity of
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hydrophobic 0.35CBA40 could be attributed to its high porosity
and low density as well as its uniform superoleophilic and
superhydrophobic properties. However, the sorption capacity of
0.35CBA40 for oils and solvents with different densities was not
the same.14,30 The volume of trichloromethane absorbed was the
lowest, the volume of ethanol, toluene, soybean oil and n-
hexane was average, and the volume of crude oil, diesel oil,
acetone, silicone oil and lubricating oil was the highest.
In general, the sorption capacities of the CBAs were much
higher than those of other cellulose-based aerogels5,18,23,31 and
conventional sorbent materials including natural materials.32,33
It was also observed that their sorption capacity was lower than
that of some superabsorbents, such as MCF aerogel from
microbrillated cellulose bers (88–228 g g
1)20 and graphene
sponge (60–160 g g
1),34 but the method for the manufacturing
process of the CBAs studied here was much simpler and lower
in cost, and its raw material, i.e., Eichhornia crassipes was
a sustainable waste biomass. Thereby, these CBAs could be
promising sorbents used for spilled oil remediation.
Conclusions
Lightweight, porous and exible cellulose-based aerogels were
successfully prepared from Eichhornia crassipes via a facile
process, without the need for special conditions. The superior
CBA with both superior oil absorbency and good mechanical
properties was obtained at 0.35 wt% cellulose and 40 wt% PAE
(i.e., 0.35CBA40). The prepared CBA possessed excellent oil/
solvent sorption capacities and super-hydrophobicity, as well
as superior elasticity. Furthermore, the loss of sorption capacity
of the hydrophobic 0.35CBA40 for diesel oil was only 25% aer
16 cycles. Coupled with the fact that waste biomass is used as
the raw material and the fabrication process is environmentally
friendly, the low density and high porosity CBA is an ideal
alternative for environmental protection.
Conflict of interest
The authors have declared no conict of interest.
Acknowledgements
The work was funded by the National Natural Science Founda-
tion of China (No. 41373097), and Program for Innovative
Research Team in University (No. IRT13078).
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