Composites: Part B 52 (2013) 233238

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Composites: Part B
journal homepage: www.elsevier.com/locate/compositesb

Structural and thermal characterization of Moroccan sugar cane bagasse

cellulose bers and their applications as a reinforcing agent in low
density polyethylene
Amine Moubarik a,, Nabil Grimi b, Nadia Boussetta b
a

MAScIR-INANOTECH, ENSET, Avenue de lArme Royale, Madinat El Irfane, 10100 Rabat, Morocco
Universit de Technologie de Compigne, Unit Transformations Intgres de la Matire Renouvelable (TIMR, EA4297), Centre de Recherche de Royallieu, BP 20529,
60205 Compigne Cedex, France
b

a r t i c l e

i n f o

Article history:
Received 29 December 2012
Received in revised form 8 April 2013
Accepted 11 April 2013
Available online 19 April 2013
Keywords:
A. Fibers
A. Polymermatrix composites
B. Fiber/matrix bond
B. Mechanical properties
B. Strength

a b s t r a c t
Cellulose bers were isolated from Moroccan sugar cane bagasse by using three distinct stages. Firstly
bagasse was subjected to (1) a hot water (70 C) treatment to eliminate hemicellulose, then to (2) an alkaline aqueous solution (15% of sodium hydroxide (NaOH), 98 C) treatment to eliminate lignin, and nally
to (3) a bleaching stage. Sugar cane bagasse cellulose bers were analyzed by different complementary
analysis (FT-IR; 13C NMR and TG). The reinforcing capability of cellulose bers extracted from sugar cane
bagasse was investigated using low density polyethylene as matrix. The cellulosic preparations were free
of bound lignin. The intrinsic viscosity, the viscosity average and the molecular weight were respectively
511 ml/g, 1769 and 286578 g/mol. An enhance on mechanical properties of composites was found, a gain
of 72% in Youngs modulus at 25 wt.% ber loading and a gain of 85% in exural modulus at 25 wt.% ber
loading, as a results of a good interface adhesion between cellulose bers and matrix.
2013 Elsevier Ltd. All rights reserved.

1. Introduction
Bagasse is the by-product obtained after sucrose extraction
from the sugar cane plant. It has a high proportion of cellulose,
which can be readily isolated by pulping from the other components namely lignin and hemicellulose. About 4050% of bagasse
is the glucose polymer cellulose, much of which is in a crystalline
structure. Another 2535% is hemicelluloses, an amorphous polymer usually composed of xylose, arabinose, galactose, glucose,
and mannose. The remainder is mostly lignin plus lesser amounts
of mineral, wax, and other compounds [1,2]. This characteristic
suggests the possibility of using the bagasse as a source of cellulose
bers.
To obtain different products from sugar cane bagasse it is necessary to submit the biomass to separation process of its constituents. However, it is a challenge to isolate original cellulose from
sugar cane bagasse. A variety of methods such as organosolv fractionation [3,4], steam explosion [5,6] and enzymatic hydrolysis [7]
have been developed in an attempt to isolate and identify cellulose.
One of the most suitable methods for the extraction and separation
of cellulose is that based on the alkaline delignication [6,8,9].
Corresponding author. Address: INANOTECH-MAScIR (Moroccan Foundation for
Advanced Science, Innovation and Research), ENSET, Avenue de lArme Royale,
Madinat El Irfane, 10100 Rabat, Morocco. Tel.: +212 6 63 52 81 58.
E-mail address: amine.moubarik@yahoo.fr (A. Moubarik).
1359-8368/$ - see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesb.2013.04.040

Chemically, cellulose is a linear natural polymer of anhydroglucose units linked at the one and four carbon atoms by b-glycosidic
bonds. Cellulose is present in an amorphous state, but also associated with crystalline phases through both intermolecular and
intramolecular hydrogen bonding for which cellulose does not
melt before thermal degradation [10,11]. There are several types
of celluloses (I, II, III, IV, and V) and type I shows the best mechanical properties. Cellulose I consists of two phases, Ia and Ib.
Cellulose Ia has one-chain triclinic structure and cellulose Ib has
two-chain monoclinic structure [12], and they differ in hydrogen
bonding [13]. Thermodynamically, the cellulose Ib format is found
to be more stable than the Ia, and cellulose Ia was converted to Ib
by annealing at around 200 C in a number of different solvent
media [14,15].
Interest in natural bers has increased worldwide due to their
low cost, low density, hardness, good thermal and mechanical
resistivity [16] and to their environmental friendliness [17]. The
main disadvantages of natural bers are low permissible processing temperatures, the tendency to form clumps, and their hydrophilic nature. The substitution of nonnatural bers by vegetable
bers has a lot of advantages that can be justied through ecological balances. Some research works were developed using thermoplastic polymers/natural bers showing excellent results for many
applications, especially in interior components for automotives.
Thermoplastics such as polyethylene (PE) [18,19], polypropylene

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A. Moubarik et al. / Composites: Part B 52 (2013) 233238

(PP) [2022], poly(lactic acid) (PLA) [23] and poly(vinyl chloride)

(PVC) [24] have been compounded with natural bers (such as sisal, jute, and sugar cane bagasse cellulose) to prepare composites.
The aim of this work was to valorise the sugar cane bagasse biomass. The study discusses the isolation and characterization of cellulose bers from Moroccan sugar cane bagasse and the possibility
to incorporate them as a reinforcing component in low density
polyethylene. The effect of ber content on the mechanical properties has been investigated in terms of tensile strength, Youngs
modulus and exural modulus.

2. Experimental methods
2.1. Materials
Sugar cane bagasse was obtained from a local sugar factory
(Guangzhou, Morocco). The bagasse was stored indoors while the
experiments were conducted. The bagasse was air-dried for three
days at ambient temperature (up to 810% equilibrium moisture
content) and then cut into small pieces (12 cm). The cut bagasse
was ground to pass a 1.0 mm size screen. All chemicals used were
of analytical or reagent grade (SigmaAldrich, France). The Low
Density Polyethylene (LDPE, Riblene MP 31 from Polimeri europa
france, density of 0.924 g/cm3 and a melting temperature of
109.8 C) was used as the matrix.

2.2. Isolation and purication of cellulose from bagasse

The procedure for isolation of cellulose with hot water and
aqueous solution of sodium hydroxide is illustrated in Fig. 1.
Twenty grams (oven-dry matter) of sugarcane bagasse were treated with a hot water at 70 C for 2 h. The solid-to-liquid ratio used
was 1:10 (w:w). The treatments were carried out in a steel reactor
with a Parr 4836 temperature controller (Parr Instrument Company, Moline, IL). At the end of the reaction the pre-treated sugarcane bagasse was cooled (25 C), washed with water (S:L
ratio = 1:10; w:w) and centrifuged (2000 rpm, t = 10 min) to separate the solubilized hemicelluloses.
Lignin was then extracted from the pretreated sugar cane bagasse using alkaline treatment. Sugar cane bagasse was placed in
a reactor with an aqueous alkaline (15% NaOH (m/v)) solution.
The solid-to-liquid ratio was 1:10. The suspension was maintained
under agitation (250 rpm) for 90 min at 98 C. At the end of the
reaction the delignied material was ltered to obtain the black liquor without any brous materials. The residue was washed with
water until the pH was neutral. The alkali extracted bers were airdried under ambient laboratory conditions and stored until the
time of bleaching.
Because of persistent discoloration the cellulose bers were
subsequently bleached with a sodium chlorite/glacial acetic acid
mixture to remove any residual lignin and hemicellulose that
may have been present. The bleached cellulose bers were washed

Sugar cane
bagasse
Extracted with hot water at 70C during
2 hours (solid:liquid ratio; 1:10, w/w).

Separated
sample
Extracted with 15% NaOH (w/v)
aqueous solution at 98 C for 90 min
(solid:liquid ratio; 1:10, w/w)

Cellulose
fibers

Filtrate:
lignin

Washing with water and air-drying

Cellulose
fibers
Sodium chlorite/glacial acetic acid

Bleached
cellulose fibers
- Washing with 5% NaOH (w/v)
- Washing with water and air-drying

Cellulose
fibers
Fig. 1. Scheme for extractions of original celluloses from Moroccan sugar cane bagasse.

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A. Moubarik et al. / Composites: Part B 52 (2013) 233238

repeatedly, initially with an aqueous sodium hydroxide (5%; w/w)

and subsequently deionized water in order to attain a neutral pH
and air-dried under ambient laboratory conditions.
2.3. Cellulose characterization
The chain length of cellulose is generally expressed as the degree of polymerization (DP), which is dened as the average number of anhydroglucose units in the chain of the cellulose molecule.
Viscosity of the cellulosic preparations was measured by British
Standard Methods for determination of limiting viscosity number
of cellulose in dilute solutions, Part 1. Cupriethylenediamine
(CED) method (BS 6306: Part 1: 1982) [25]. The viscosity average
(DP) of the cellulose samples was determined from their intrinsic
viscosity [g] in cupriethylenediamine hydroxide (cuene) solution,
P0.9 = 1.65 [g] (ml/g), where P is an indeterminate average DP
[26]. Molecular weight of the cellulosic preparations was then calculated from their P value multiplied by 162, molecular weight of
an anhydroglucose.
Fourier transform infrared spectroscopy (FT-IR) measurements
were performed in an ABB Bomem FTLA 2000-102 instrument by
direct transmittance using KBr pellet technique. Each spectrum
was recorded over 20 scans, in the range from 4000 to 200 cm 1
with a resolution of 4 cm 1. Background spectra were collected before every sampling. KBr was previously oven-dried to avoid interferences due to the presence of water. The characteristic bands of
cellulose were assigned according to the literature.
Solid-state Cross Polarization/Magic Angle Spinning (CP/MAS)
13
C NMR measurements were obtained at ambient temperature
by using a Bruker 400 MHz spectrometer. Powdered samples were
packed in a 4-mm zirconia rotors, sealed with Kel-FTM caps and
spun at 7 kHz and at a contact time of 3.5 ms. Chemical shifts were
determined relative to tetramethyl silane (TMS) used as control.
Thermogravimetry (TG) was used to determine the thermal stability and degradation of the cellulose samples using a TGA Q50
thermogravimetric apparatus. Ten milligrams of each cured sample
were placed on a balance located in the furnace and heat was applied over the temperature range from room temperature to 800 C
at a heating rate of 5 C/min in air. Mass losses vs. temperature
thermograms were obtained showing the different decomposition
processes. Three replicates were used for sugar cane bagasse and
pure cellulose.

of 170, 170, 165 and 165 C from hopper to the die respectively.
The extruded composites were cooled in a water bath and then pelletized into granules of 2 mm length. The granular materials were
subsequently compression molded into samples for mechanical
testing.
2.5. Composites testing
The mechanical strength of composites was determined using
an INSTRON universal-testing machine (model 33R4204). Tests
were carried out according to ISO 527-3 [27] with 2 mm/min crosshead speed. Tensile strength and modulus values are average results of fty tested specimens. The resulting load was measured
using a 50 kN load cell.
Flexural properties of the samples were measured on an INSTRON 33R4204 equipment in accordance to ASTM D790-03 standard [28]. The measurements were performed at ambient
conditions (23 C). The crosshead speed for the exural tests was
set at 2 mm/min. The resulting load was measured using a 50 kN
load cell.
Scanning electron microscopy (SEM) was used to probe the dispersion of the cellulose bers in the polymer matrix. SEM of the
composite sample was performed with a Jeol. JSM-7000 F BRUKER
instrument operating at 15 kV. The specimens were frozen under
liquid nitrogen, fractured, coated with palladium to prevent electrical charging.
Effects of water absorption on bagasse cellulose bers reinforced LDPE composites were investigated in accordance to ASTM
D570 standard [29]. Samples for mechanical tests containing different ber fractions of reinforcement were evaluated after water
absorption to evaluate the effect on mechanical properties.
2.6. Statistical analysis
The tests experiments concerning the composite characterization were repeated 50 times. Means and standard deviations of
data were calculated. The analysis of variance (ANOVA) was applied for the analysis of the results of Table 1. For each analysis, signicance level of 5% was assumed. All statistical analyses were
carried out using the software Statgraphics Plus 5.1 (Stat-point
Technologies, Inc.).
3. Results and discussion

2.4. Composites preparation

3.1. Yield of cellulose
The LDPE in form of granules and dried sugarcane bagasse cellulose with various weight percents (10, 15, 20 and 25 wt.%) were
extruded altogether using an extruder screw, marks IMACOM
equipped with four heating zones operating at a screw rate of
125 rpm. The extruder barrel was heated with the following prole

Alkaline treatment is usually an effective method to isolate cellulose bers from agricultural residues. Sodium hydroxide, one of
the most common alkaline reagents, has been applied to treat a
variety of agricultural residues [30,31]. In this study, cellulose

Table 1
Mechanical properties of the composites before and after water absorption. Fifty replicates of each composites. S.D.: standard deviation.
Materials

Low density polyethylene (LDPE)

Cellulose (10%)/LDPE composites
Cellulose (15%)/LDPE composites
Cellulose (20%)/LDPE composites
Cellulose (25%)/LDPE composites

Before water absorption

After water absorption

Tensile Strength
(MPa)
Mean S.D

Youngs Modulus
(MPa)
Mean S.D

Flexural Modulus
(MPa)
Mean S.D

Tensile Strength
(MPa)
Mean S.D

Youngs Modulus
(MPa)
Mean S.D

Flexural Modulus
(MPa)
Mean S.D

14 0.9a
10 0.4b
9 0.2c
11 1.5b
7 1.8b

236 21a
263 11b
310 9c
360 17d
407 12e

194 12a
230 8b
260 15c
310 16d
360 11e

13 0.7a
9 0.9b
9 0.5b
8 1c
6 1.1e

207 11a
249 14b
289 10c
333 12d
378 18e

186 10a
214 13b
233 11c
286 20d
308 18e

a, b, c, d, e values with the same superscript letters were not signicantly different.
S.D.: standard deviation.

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A. Moubarik et al. / Composites: Part B 52 (2013) 233238

was isolated with 15% NaOH at 98 C for 90 min. Yields of cellulose

are calculated on a dry weight basis. The obtained yields of cellulose are 42%. These values are in perfect consistency with the literature, which reports cellulose percentages of 50% [3234]. The
two-stage treatments with hot water and 15% NaOH, totally released 84% of original cellulose from sugar cane bagasse. This
sequential treatment enabled the isolation of original cellulose
from sugar can bagasse.
3.2. Cellulose characterization
FT-IR spectroscopy has been extensively used in cellulose research, since it presents a relatively easy method of obtaining direct information on chemical structure of cellulose. Fig. 2
illustrates FT-IR spectra of cellulose isolated from sugar cane bagasse. The absorptions bands are attributed to the functional
groups that are present in the cellulose. In the spectra of cellulosic
preparations obtained by a single alkaline extraction with 15%
NaOH, the absorptions at 3370, 2870, 1628, 1436, 1373, 1320,
1211, 1172, 1113, 1026, and 896 cm 1 are associated with the typical values of cellulose [6,35]. The absence of the band at
1726 cm 1 and the band relating to lignin aromatic ring vibrations
at 1513 cm 1 revealed that the treatments of sugar cane bagasse
by delignication with NaOH (15%) under the used conditions
completely removed lignin from the cell wall of sugar cane bagasse, resulting in the cellulosic preparations, which are free of
lignin.
Solid-state CP/MAS 13C NMR spectroscopy is capable of providing detailed information directly on the characteristics of the bagasse cellulose bers. Fig. 3 illustrates the CP/MAS 13C NMR
spectra of the pure cellulose derived from bagasse. It can be seen
that the most intense signals are those from cellulose carbons that
appear between 60 and 110 ppm. The signals from 60 to 70 ppm
are attributed to C-6, from 70 to 80 ppm to C-2, C-3, and C-5, from
80 to 90 ppm to C-4 (88.1, C-4 of crystalline cellulose; 82.6, C-4 of
amorphous cellulose), and from 98 to 110 ppm to C-1 [36,37]. The
absence of the signals at 56 and 110160 ppm relating to methoxyl
and aromatic groups of lignin conrmed that the cellulosic preparations were free of the associated lignin [35].
The viscosity average (DP) of a cellulose sample is conveniently
estimated from the intrinsic viscosity by applying the equation
DP0.9 = 1.65 [g] (ml/g). The molecular weight (Mw) of the cellulose
was estimated by multiplying by 162, a molar mass of anhydroglucose. The intrinsic viscosity, the DP and the Mw are respectively
511 ml/g, 1769 and 286,578 g/mol. These values showed that cellulose preparation isolated from sugar cane bagasse had higher
intrinsic viscosity and molecular weight compared to the results
found in the literature [6,9] indicating that treatment of sugar cane

Fig. 2. FTIR spectra of the sugar cane bagasse cellulose bers.

Fig. 3. CP/MAS

13

C NMR spectra of the sugar cane cellulose bers.

bagasse with hot water and NaOH (15%) under the used condition
does degrade the macromolecule of cellulose.
The thermal decomposition of organic polymers is commonly
determined by thermogravimetry (TG) analysis under nitrogen or
air atmosphere. TG and DTG curves of sugarcane bagasse and pure
cellulose derived from bagasse (after removal of lignin and hemicellulose) are shown in Fig. 4 a and b, respectively. The initial
weight losses starting at 36 C for both native ground bagasse
and pure cellulose may be attributed to the evaporation of loosely
bound moisture on the surfaces of these materials. The second degradation occurred at around 100130 C and is ascribed to the
evaporation of absorbed water. The degradation of untreated bagasse ensues at 180 C and the maximum rate of degradation
was observed at 270 C (revealed by DTG curve) while that of the
alkali treated cellulose occurred at 210 C and the rate of degradation becoming maximum at 320 C (according to DTG curve). The
presence of other macromolecules (hemicellulose, lignin) which
are decomposed at low temperatures help to cause early onset of
degradation of the bagasse. Similar observations were reported
by Mandal and Chakrabarty [38].
3.3. Cellulose valorization
The values of mechanical properties (tensile strength, Youngs
modulus and exual modulus) of the composites after and before
water absorption are summarized in Table 1. Addition of cellulose
bers to LDPE, yield a composite material with a higher Youngs
modulus and a higher exural modulus compared to neat LDPE.
This improvement corresponds to an increase of 72% and 85% for
the Youngs modulus and the exural modulus, respectively. The
ANOVA analysis showed a signicant difference between cellulose
bers/LDPE composites and neat LDPE. This is due to the high cellulose bers tensile modulus compared to neat PP and to a good
interaction between cellulose bers and matrix [39]. The results
obtained for tensile strength showed a decrease in the tensile
strength with increasing cellulose ber loading. This could be explained by the cellulose ber length and the decohesion between
the matrix and bers under stress. This decohesion generates a
stress concentration which accelerates the sample break. In this
work, 20 wt.% bagasse cellulose ber reinforced LDPE matrix was
the optimum percentage to make the best composites. Therefore
the mechanical properties obtained after water absorption were
slightly affected. The slight decrease in mechanical properties after
water absorption may be caused by formation of hydrogen

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A. Moubarik et al. / Composites: Part B 52 (2013) 233238

Sugar cane
bagasse

Pure
cellulose

Pure
cellulose

Sugar cane
bagasse

Fig. 4. TG (a) and DTG (b) curves of untreated sugar cane bagasse and pure cellulose bers derived from sugar cane bagasse (after removal of lignin and hemicellulose).
Analysis in air atmosphere, heated at 5 C/min.

Sugar cane
bagasse

Cellulose
fibers

Fig. 5. SEM images of the tensile fractured surface of optimal cellulose bers (20%)/
LDPE composites.

bonding between the water molecules and cellulose bers, which

change the structure and properties of the bers, matrix, and the
interface between them. The cellulose bersmatrix interface can
also play a signicant role in the rate of water absorption in composites and the deterioration of mechanical properties due to
water effects [4042].
SEM was used to monitor the fracture surface of the composites
after quenching the samples in liquid nitrogen. The SEM observations of the fractured surface of cellulose (20%)/LDPE composites
are presented in Fig. 5. These gures show a better berLDPE
interfacial adhesion. Fig. 5 shows that the bers were covered by
the LDPE to a larger extent. In addition, there were almost no signs
of ber pull-outs and most of the bers were fractured. It was difcult to make certain conclusions regarding to the dispersion of
the bers in the LDPE from the SEM micrographs. However, there
was no evidence of large agglomerates of bers on the studied fracture surfaces.

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4. Conclusion
In summary, the adopted extraction methodology seems to be
able to isolate cellulose bers from sugar cane bagasse. The hot
water treatment of bagasse followed by the alkaline treatment
were found to be a promising alternative separation process since
it resulted in the removal of most of the lignin and hemicelluloses
without any signicant damage of the macromolecules of cellulose
structure. Furthermore, FT-IR spectroscopy and 13C NMR spectrometry of the cellulose bers conrm that all the lignin and hemicelluloses were eliminated during the separation process.
The present results reveal that cellulose bers can be used as
reinforcing ller in LDPE. The results show a signicant increase
of the mechanical properties of composites with the addition of
cellulose bers, reaching 72% increases from neat LDPE in Youngs
modulus at 25 wt.% cellulose bers reinforcement, while the exural modulus increased by 85% at 25 wt.% cellulose bers reinforcement when compared to neat LDPE.

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[22]

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[25]

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