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Extraction of cellulose and preparation of nanocellulose from sisal fibers

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DOI: 10.1007/s10570-007-9145-9

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Cellulose (2008) 15:149–159
DOI 10.1007/s10570-007-9145-9
Extraction of cellulose and preparation of nanocellulose
from sisal fibers
Juan I. Morán Æ Vera A. Alvarez Æ Viviana P. Cyras Æ
Analia Vázquez
Received: 14 August 2006 / Accepted: 6 July 2007 / Published online: 15 August 2007
Ó Springer Science+Business Media B.V. 2007
Abstract In this work a study on the feasibility
of extracting cellulose from sisal fiber, by means of
two different procedures was carried out. These
processes included usual chemical procedures such
as acid hydrolysis, chlorination, alkaline extraction,
and bleaching. The final products were characterized
by means of Thermogravimetric Analysis (TGA),
Infrared Spectroscopy (FTIR), X-Ray Diffraction
(XRD), Differential Scanning Calorimetry (DSC)
and Scanning Electronic Microscopy (SEM). The
extraction procedures that were used led to purified
cellulose. Advantages and disadvantages of both
procedures were also analyzed. Finally, nanocellulose
was produced by the acid hydrolysis of obtained
cellulose and characterized by Atomic Force
Microscopy (AFM).
Keywords Cellulose
Sisal fibers

Extraction procedures
Characterization

Nanocellulose
J. I. Morán
V. A. Alvarez
V. P. Cyras

A. Vázquez (&)
Research Institute of Material Science and Technology
(INTEMA), National Research Council (CONICET) –
Universidad Nacional de Mar del Plata, Av. Juan B. Justo
4302, 7600 Mar del Plata, Argentina
e-mail: anvazque@fi.mdp.edu.ar
Introduction
Plant fibers are mainly composed of cellulose, hemi-
cellulose and lignin. Cellulose, which awards the
mechanical properties of the complete natural fiber, is
ordered in micro-fibrils enclosed by the other two main
components: hemicellulose and lignin (Vignon et al.
2004; Rong et al. 2001). Cellulose microfibrils can be
found as intertwined microfibrils in the cell wall (2–
20 lm diameter and 100–40,000 nm long depending on
it source) (Itoh et al. 1984; Benziman et al. 1980). As
well as these microfibrils, there exist nanofibers (also
composed by cellulose) with diameters of 5–50 nm and
lengths of several millimeters conformed by nanocrys-
talline domains and amorphous regions. A controlled
acid hydrolysis can separate both regions driving to
crystalline domains with an elastic modulus of 150 GPa,
which is higher than that of the S-glass (85 GPa) and
Aramid fibers (65 GPa) (Samir et al. 2004).
Cellulose is the main component of several natural
fibers such as cotton, flax, hemp, jute and sisal within
others. This natural polymer represents about one-third
of plant tissues and it can be restocked by photosynthesis.
The biosynthesis of this polymer is approximately
1,000 tones by year in the world (Goodger 1976).
Cellulose is a linear polymer of b-(1 ? 4)-D-
glucopyranose units (Fig. 1a). The mechanical prop-
erties of natural fibers depend on the type of cellulose
present. There are several types of cellulose (I, II, III,
IV and V), being type I the one showing better
mechanical properties.
123
150
Fig. 1 (a) Cellulose (b) D-
Xylose; D-Glucose; D-
Glucoronic Acid (c)
Phenylpropane; Guaiacyl;
Syringyl
Hemicellulose is composed of different types of
cycled saccharides such as xylose, mannose and
glucose, among others. It forms a highly branched
random structure. It is mainly amorphous (Fig. 1b).
Lignins are amorphous polymers formed by
phenyl-propane units. They mainly consist of aro-
matic units such as guaiacyl, syringyl and
phenylpropane (Fig. 1c).
There are a great number of potential uses of
cellulose within different industries. As a result, it has
created an important focus for researcher’s interest.
On this field, cellulose production from natural fibers
has become really significant. It generally involves
fibers treatment with alkalis or bisulphites to separate
the lignin and to extract the hemicellulose. In
addition, the extraction processes can be performed
by different kind of procedures. Each method
possesses different advantages and drawbacks related
to the amount/quality of cellulose (composition and
final properties).
In this work, cellulose was extracted from sisal
fibers, which is abundant in South America. Sisal
fibers are composed of cellulose (50–74%), lignin
(8–11%), hemicellulose (10–14%), pectin (1%) and
wax (2%) (Bledzki and Gassan 1999; Hon 1996;
Rowell et al. 1996). Because of its high cellulose
123
Cellulose (2008) 15:149–159
content, cellulose extraction from these fibers could
lead to high quantity of nanofibers.
The aims of this work were to produce cellulose
from sisal fibers through two different procedures and
to perform the characterization of the obtained
cellulose. The cellulose was transformed into nano-
cellulose for its future use as nanofiller for
biodegradable matrices, and it was also characterized
by means of microscopy analysis.
Experimental
Materials
Sisal fibers from Brascorda (Brazil) were used in this
work. Microcristalline cellulose from Sigma Aldrich
(USA) and alkaline lignin from Granit SA (Sweden)
were used as reference materials for the comparative
chemical analysis.
Other reagents used were: toluene (Anedra,
Argentina); ethanol (Anedra, Argentina); sodium
hydroxide (Anedra, Argentina); hydrogen peroxide
(Cicarelli, Argentina), sodium borate (Anedra,
Argentina); nitric acid (Cicarelli, Argentina); acetic
acid (Cicarelli, Argentina), sodium chlorite (Fluka
Cellulose (2008) 15:149–159
Chemie, Germany), sodium bisulphate (Barker,
USA); sulfuric acid (Cicarelli, Argentina); buffer
solution (Anedra, Argentina). All used reagents were
analytical grade.
Cellulose extraction and nanocellulose production
methods
As received sisal fibers were preconditioned before
cellulose extraction took place. The fibers were
washed with distilled water several times and dried
in an oven at 80 °C for 24 h. Then they were chopped
to an approximate length of 5–10 mm. Finally a
de-waxing step was carried out: boiling in a mixture
toluene/ethanol (2:1 volume/volume) in a soxhlet for
6 h. The de-waxed fibers were then filtered, washed
with ethanol for 30 min and dried.
Subsequently, two different procedures were used
for cellulose extraction:
Procedure 1
(I) Pre-treatment with 0.1 M NaOH in 50% volume
of ethanol at 45 °C for 3 h under continuous agita-
tion; (II) Treatment with hydrogen peroxide at
pH = 11.5 (buffer solution) and 45 °C: (a) 0.5%
H2O2, (b) 1.0% H2O2, (c) 2.0% H2O2 and (d) 3.0%
H2O2 for 3 h each one under continuous agitation ;
(III) Treatment with 10% w/v NaOH—1% w/v
Na2B4O7
10 H2O at 28 °C for 15 h, under continuous
agitation; (IV) Treatment with HNO3, 70% + HAc,
80% (1/10 v/v) at 120 °C for 15 min (V) Washing
with 95% ethanol; washing with water and washing
again with 95% ethanol; (VI) drying at 60 °C in oven
until constant weight. This procedure was adapted
from the work done by Sun et al. (Sun and Sun 2002;
Sun et al. 2004).
Procedure 2
(I) Treatment with 0.7 w/v.% sodium chlorite Na-
ClO2: holocellulose (a-cellulose + hemicellulose)
production by the gradual removal of lignin; at pH
4 (buffer solution) boiling for 2 h using a fiber to
liquor ratio of 1:50 and treatment with sodium
bisulphate solution 5% w/v.; (II) treatment of
151
holocellulose with 17.5 w/v.% NaOH solution; (III)
filtering, washing with distilled water and drying at
60 °C in a vacuum oven until constant weight. This
procedure was adapted from the works of Chatto-
padhavay and Sarkar (Chattopadhyay and Sarkar
1946; Sarkar et al. 1948).
Nanofibers production
Nanofibers were prepared by the acid hydrolysis of
obtained celluloses (procedures I and II). The acid
hydrolysis was carried out with sulphuric acid
(H2SO4) solution 60 wt.% at 45 °C, 30 min under
continuous agitation.
Characterization methods
TGA
Dynamic thermogravimetric measurements were per-
formed by using a Shimadzu TGA-DTG 50
instrument. Temperature programs for dynamic tests
were run from 25 °C to 700 °C at a heating rate of
10 °C/min. These tests were carried out under
nitrogen atmosphere (20 ml/min) in order to prevent
any thermoxidative degradation.
DSC measurements
Runs were carried out in a Shimadzu DSC-50 from
room temperature to 400 °C at a heating rate of 2 °C/
min under nitrogen atmosphere.
FTIR spectra
DRIFT method was followed in order to obtain FTIR
spectra. 64 scans were carried out on wavenumber
from 4,000 cm1 to 600 cm1. The equipment used
was an FTIR Genesis II.
SEM examination
Scanning Electronic Microscopy (SEM) photographs
of fibers and microfibrils surfaces were taken with a
123
152 Cellulose (2008) 15:149–159

scanning electron microscope, JEOL JSM-6100
instrument.
AFM examination
A Digital Instruments NanoScope III controller with
a MultiMode Atomic Force Microscopy (AFM) head
was used to image the cellulose crystals, using the
supplied liquid cell filled with water. Images were
acquired in contact mode.
XRD
In all cases, a small weight loss was found in the
range of 25–150 °C due to the evaporation of the
humidity of the materials or low molecular weight
compounds remaining from the isolation procedures.
Decomposition of the untreated sisal fibers shows
several stages, indicating the presence of different
components that decompose at different
temperatures.
Decomposition of celluloses obtained by proce-
dures I and II starts around 255 °C. In both cases,
solid residues at 700 °C are close to 15–18 wt.%. On
the other hand, commercial cellulose has a sharp
weight loss starting at 305 °C and it was almost

A PW1710 Diffractometer equipped with an X-ray

generator (k = 0.179 nm) was used. Powder X-Ray
diffractometry was carried out. Samples were
scanned in 2h ranges varying from 5° to 40° (1°/min).

Results and discussion

TGA

Due to the differences in the chemical structures

between hemicellulose, cellulose and lignin, they
usually decompose at different temperatures. Many
studies related to the decomposition of lignocellulosic
materials can be found in specific literature. For
example, Yang et al (Yang et al. 2007) showed that
in the thermal analysis, cellulose decomposition started
at 315 °C and persisted until 400 °C. Maximum weight
loss rate was reached at 355 °C. At 400 °C almost all
cellulose was pyrolyzed, and the solid residuals were
relatively small (6.5 wt.%). Hemicellulose started its
decomposition at 220 °C and continued up to 315 °C.
The decomposition peak reached the maximum mass
loss rate at 268 °C, showing a 20 wt.% of solid
residuals at 700 °C. Finally, they showed that lignin
decomposition extended to the whole temperature
range, starting well below 200 °C and persisting above
700 °C. The solid residue left from lignin pyrolisis was
the highest one (46 wt.%).
The thermal gravimetric analysis permits to study
the decomposition of the obtained celluloses (Proce-
dures I and II). As a reference, commercially
Fig. 2 (a) Thermal analysis of obtained cellulose, sisal fiber,
available lignin and cellulose were also studied.
commercial lignin and commercial cellulose (b) DTGA curves
Figure 2a shows the residual mass (wt%) as a of lignin, sisal fibers, commercial cellulose and obtained
function of the temperature. celluloses

123
Cellulose (2008) 15:149–159 153

completely pyrolyzed at 700 °C, with a residual mass Table 1 Absorption bands for functional groups of cellulose,
of 1.6 wt.%. hemicellulose and lignin
Regarding lignin decomposition, it started at Fiber Wave Functional Compounds
200 °C and showed a continuous mass loss over the component number (cm1) group
whole range. At 700 °C, the remaining solids were
Cellulose 4,000–2,995 OH Acid, methanol
close to 35 wt.%. The wide temperature range
2,890 H–C–H Alkyl, aliphatic
observed during lignin decomposition is due to the
1,640 Fiber–OH Adsorbed water
different activities of the chemical bonds present on
1,270–1,232 C–O–C Aryl-alkyl ether
its structure (Yang et al. 2007).
1,170–1,082 C–O–C Pyranose ring
The differential mass loss (in wt.%/°C) as a skeletal
function of temperature for the same samples is 1,108 OH C–OH
shown in Fig. 2b. Presenting the data this way allows
Hemicellulose 4,000–2,995 OH Acid, methanol
the identification of the maximum mass loss rate, as
2,890 H–C–H Alkyl, aliphatic
well as the presence of different peaks during the
1,765–1,715 C=O Ketone and
decomposition of the samples. carbonyl
During the decomposition of the untreated sisal 1,108 OH C–OH
fibers, a small peak appears at 296 °C, close to the Lignin 4,000–2,995 OH Acid, methanol
main one (348 °C). This peak was attributed to the 2,890 H–C–H Alkyl, aliphatic
decomposition of hemicellulose by other authors 1,730–1,700 Aromatic
(Alvarez and Vazquez 2006). 1,632 C=C Benzene
Celluloses obtained from Procedures I and II also stretching
showed a small broadening or shoulder on the left ring
side of the main peak (348 °C). It could be due to a 1,613, 1,450 C=C Aromtic
broad distribution of molecular mass from cellulose skeletal
mode
or a residual content of hemicellulose. In the case of
1,430 O–CH3 Methoxyl–
commercial cellulose, it showed a sharp peak with a
O–CH3
maximum decomposition rate at 348 °C. In this case
1,270–1,232 C–O–C Aryl-alkyl
there were no signs of any broadening or shoulders on ether
the left side of the peak. 1,215 C–O Phenol
Regarding lignin decomposition, it could be seen 1,108 OH C–OH
that the rate was lower than the other materials, with 700–900 C–H Aromatic
the peak starting at 200 °C and continuing up to hydrogen
700 °C.
Celluloses obtained from procedures I and II
started decomposing at lower temperatures than FTIR
commercial cellulose. In addition, they showed
higher amounts of residual solids. This could be an Fourier Transform Infra Red spectroscopy was car-
indicator of the presence of small amounts of ried out. Samples analyzed included untreated sisal
hemicellulose or lignin which withstood the extract- fibers, commercial cellulose, commercial lignin and
ing procedures. However, the differences in the celluloses obtained in this work. The FTIR lets
starting temperature for decomposition could be due characterize the chemical structure by identifying the
to a higher degree of order of the commercial functional groups present in each sample.
cellulose when compared to the ones obtained in this The infrared spectra of cellulose, hemicellulose
work (size distribution, molecular weight among and lignin were studied in the literature (Yang et al.
others). Furthermore, the differences in residual mass 2007; Alvarez and Vazquez 2006; Oh et al. 2005;
could be due to the chemical procedures used, which Nelson and O’Connor 1964). The typical functional
could induce higher char formation (1.6 wt.% and groups and the corresponding bands for each com-
15–18 wt.%). This was in accordance to the results ponent are shown in Table 1 (Oh et al. 2005; Nelson
obtained by Sun et al. (2004). and O’Connor 1964). The three materials are mainly

123
154
Fig. 3 FTIR Spectra for
obtained celluloses,
commercial cellulose and
commercial lignin
composed of alkanes, esters, aromatics, ketones and
alcohols, with different oxygen-containing functional
groups observed in Fig. 1a, b, c.
All samples presented two main absorbance
regions. The first one at low wavelengths in the
range 700–1,800 cm1, and the second one at higher
wavelengths corresponding to the range 2,700–
3,500 cm1 approximately. However specific absorp-
tion peaks could be identified for each particular
component (Fig. 3).
Lignin presented characteristic peaks in the range
1,500–1,600 cm1 corresponding to the aromatic
skeletal vibration. In addition, due to the presence
of functional groups such as methoxyl –O–CH3,
C–O–C and aromatic C=C, absorbance in the region
between 1,830 cm1 and 1,730 cm1 was observed
(Reddy et al. 2005).
Commercial cellulose and cellulose from Procedure
II presented an absorption band at 1,652 cm1. On the
other hand, cellulose from Procedure I presented a peak
at 1,728 cm1. Regarding the assignation of these
Fig. 4 Colour of
commercial celluloses and
celluloses obtained by
Procedures I and II
123
Cellulose (2008) 15:149–159
peaks, many possibilities arise from the literature. Some
authors (Sun and Sun 2002; Alvarez and Vazquez 2006;
Cyras et al. 2004) showed that acetylation can be found
by the presence of acetyl ester bands at 1,745 cm1.
Taking into consideration that Procedure I required the
use of acetic acid as a crucial step for obtaining
cellulose, there was a possibility for some acetylation to
take place. However, this band is not present in the
spectrum corresponding to the cellulose obtained by this
procedure.
The peak present at 1,728 cm1 in the spectrum
corresponding to the cellulose obtained by Proce-
dure I could be due to the presence of small
amounts hemicellulose, which contain higher C=O
linkage at 1,765–1,715 cm1. Another possibility it
that carboxyl or aldehyde absorption (1,728 cm1)
could be arising from the opened terminal glyco-
pyranose rings or oxidation of the C–OH groups,
and also the 1,620 cm1 band corresponds to
carbonyl groups. The presence of the peak at
1,728 cm1 could be attributed to oxidation due to
Cellulose (2008) 15:149–159
the yellow color of cellulose obtained by Procedure
I (Fig. 4).
Lojewska et al. observed OH bending of adsorbed
water at 1,640 cm1 (Lojewska et al. 2005). All the
FTIR spectra were developed after the same carefully
drying process, however the water adsorbed in the
cellulose molecules is very difficult to extract due to
the cellulose-water interaction, as it was explained by
Baird et al in the computational analysis done on
cellulose molecules (Baird et al. 2006).
Analyzing the spectra, it is evident that there was no
remaining lignin in the obtained celluloses. This arises
from the absence of the absorption bands related to
aromatic ring vibrations (1,500–1,600 cm1).
X-Ray diffraction
In order to analyze the crystallinity of the celluloses
obtained in this work, X-Ray diffractometry was
carried out. Celluloses from Procedures I and II as
well as the commercial cellulose were analyzed. The
results are shown in Fig. 5. It could be noticed that
cellulose was present in the form of cellulose I, and
not cellulose II, which arises from the fact that there
is no doublet in the intensity of the main peak
(Bhatnagar and Sain 2005; Deraman et al. 2001).
The crystallinity index (IC) can be determined by
using the following equation (Mwaikambo and
Ansell 2002):
Fig. 5 XRD of commercial cellulose, and celluloses obtained
by Procedures I and II
155


Ið002Þ  IðamÞ
Ic ¼  100
Ið002Þ
where I(002) is the counter reading at peak intensity at
a 2h angle close to 26° representing crystalline
material and I(am) is the counter reading at peak
intensity at a 2h angle close to 18° representing
amorphous material in cellulosic fibers.
The results show that the crystallinity was similar
for the three celluloses (Crystallinity Index IC = 75
± 1). Considering that hemicellulose has a random,
amorphous structure, it is concluded that the samples
prepared by means of Procedures I and II could have
a small quantity or no hemicellulose remaining from
the original fibers.
Differential scanning calorimetry
The Differential Scanning Calorimetry (DSC) tech-
nique was used to compare the thermal behavior of
commercial cellulose and the celluloses obtained by
Procedures I and II. Results are shown in Fig. 6.
In all the thermograms, from 30 °C to 140 °C an
endothermic peak appeared due to water evapora-
tion. Commercial cellulose showed a sharp
endothermic peak at 330 °C, corresponding to the
fusion of its crystalline part. Celluloses obtained
from Procedures I and II did not show a clear fusion
Fig. 6 DSC Thermograms for obtained celluloses and comer-
cial cellulose
123
156 Cellulose (2008) 15:149–159

peak. However the cellulose obtained by Procedure SEM and AFM

II showed an endothermic peak at 190 °C. In
previous works (Mwaikambo et al. 2002), the
decrease in the position of the peak has been
related to an increase in the amount of amorphous
cellulose and a reduction in the cellulose crystallite
length. It was found that the crystallinity index was
almost the same; as a consequence, the shift of the
peak was more likely due to the wider molecular
weight and size distribution of cellulose crystals. As
a result, the fusion (endothermic peak) could be
superimposed to the degradation reaction (exother-
mic peak). The mass loss during the DSC analysis
was similar for all the samples (71 ± 3%). As it was
expected, considerable degradation took place dur-
ing the tests.
Figure 7 shows the SEM micrographies of the
original sisal fibers and its products after different
steps of both procedures.
The diameter of original sisal fibers was around
100–500 lm (Fig. 7a). Each fiber is composed by
several microfibrils with diameters in the range of
8–12 lm. Each elementary fiber shows a compact
structure; exhibiting an alignment in the fiber axis
direction with some non-fibrous components in the
fiber surface (Doraiswammy and Chellamani 1993;
Garcı́a-Jaldon et al. 1998).
It was previously shown that after completion of
the selected chemical treatments (Procedures I and
II), most of the lignin and hemicellulose were

Fig. 7 SEM micrographies

at different stages of the
cellulose extraction
process: a) Sisal Fiber;
b) Treatment I, Procedure 1;
c) Treatment II,
Procedure 1; d) Treatment
III, Procedure 1;
e) Treatment I, Procedure 2
and f) Treatment II,
Procedure 2

123
Cellulose (2008) 15:149–159 157

Fig. 8 Diameter distribution

of extracted cellulose microfibrils and
untreated sisal fibers

Table 2 Average diameter of sisal fibers and cellulose

microfibrils obtained by Procedures I and II
Sisal Cellulose Cellulose
Procedure I Procedure II

Diameter (lm) 220.5 ± 105 22.0 ± 9.2 9.1 ± 2.1

removed. Fiber diameter was reduced until almost

pure cellulose was obtained. Cellulose microfibrills
of the original fibers were separated from each other
to produce fibrils with diameters around 7–31 lm
(Fig. 8).
The average diameter of the cellulose microfibrils
obtained by Procedures I and II is shown in Table 2.
From the plant, natural fibers are extracted by
mechanical methods. As it was previously mentioned, Fig. 9 AFM image of obtained cellulose
these fibers have diameters in the micron range. After
that; chemical procedures conduct to the partial note that this kind of procedures affect the total
removal of different fibers components generating a integrity of fibers.
diameter reduction (by separating the macro into After cellulose was prepared, acid hydrolysis was
micro fibrils) as well as a change in the fibers carried out in order to produce cellulose nanofibers.
composition (cellulose purification). Elementary Figure 9 shows the AFM micrographs of the obtained
fibers show a helicoidal structure (related to cellulose nanocellulose.
ordered chains) that appears evident after the total This Figure shows that after the acid hydrolysis,
extraction procedure took place. It is possible that the diameter of the cellulose fibers was in the range of
these fibers were formed by nano-ordered chains that the nanometer with an average size of
can be separated by acid hydrolysis. It is important to 30.9 ± 12.5 nm (Fig. 10).

123
158
Fig. 10 Size distribution of nanocellulose obtained after acid
hydrolysis
Comparison between Procedures I and II
When comparing the two procedures, important
differences are noticed in terms of productivity,
environmental impact, fiber quality and size distri-
bution, among others. Whereas Procedure I involves
more steps and requires more time than Procedure II,
it is an environmentally friendly treatment due to the
fact of being completely chlorine-free. Therefore
higher production cost is balanced by the lower
pollution involved. The fibers obtained using Proce-
dure II showed a narrower size distribution, as well as
a lower amount of surface defects. Therefore, more
effort should be focused on achieving higher quality
cellulose fibers as in Procedure II, but with less
harmful process such as those in Procedure I.
Conclusions
In this work, two different procedures for cellulose
extraction from sisal fibers were evaluated. By means
of TGA, FTIR, DSC and XRD, it was possible to
characterize the obtained cellulose and analyze the
presence of lignin and hemicellulose. No component
extraction could be ensured after TGA analysis. FTIR
spectra confirmed the removal of hemicelluloses and
lignin; these results were based on the characteristic
peaks of lignocellulosic materials. Furthermore, XRD
tests showed that the crystallinity was the same for all
the celluloses studied, confirming the previous
123
Cellulose (2008) 15:149–159
conclusions. DSC curves showed the superposition
of the peaks corresponding to the fusion and the
degradation. These techniques allowed concluding
that the obtained material was cellulose with no
significant quantities of hemicellulose or lignin.
When comparing Procedures I and II in terms of
productivity, environmental impact, fiber quality and
size distribution, many differences showed up. It was
noticed that the first one was less environmentally
aggressive, while the second one involved less
process time and drove to fibers with more homoge-
neous diameter distribution.
From scanning electron microscopy; different
morphologies were observed at every stage of each
procedure. After cellulose was obtained, a simple
acid hydrolysis conducted to nanofibers, which was
confirmed by AFM images. These fibers will be used
in future works in the production of biodegradable
nanocomposites with enhanced properties.
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