Polymer Testing 30 (2011) 784790

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Polymer Testing
journal homepage: www.elsevier.com/locate/polytest

Material properties

The effect of chitosan loading on the curing characteristics, mechanical

and morphological properties of chitosan-lled natural rubber (NR),
epoxidised natural rubber (ENR) and styrene-butadiene rubber (SBR)
compounds
H. Ismail*, S.M. Shaari, N. Othman
Division of Polymer Engineering, School of Materials & Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal,
Penang, Malaysia

a r t i c l e i n f o a b s t r a c t

Article history: Chitosan-lled rubber compounds were prepared using a laboratory sized two-roll mill.
Received 29 May 2011 The effect of chitosan loading on three different types of rubber (STR 5L, ENR-25 and SBR)
Accepted 6 July 2011 was investigated. The results indicate that, overall, the scorch time (tS2), cure time (t90),
tensile strength and elongation at break (Eb) decrease with chitosan loading, whereas an
Keywords: increment was observed in the maximum torque (MH) and the tensile modulus (M100 and
Chitosan
M300) of all three types of rubber. At a similar chitosan loading, the cure characteristics of
Natural rubber
SBR were found to be longer (for tS2 and t90) and higher (for MH) than those of STR 5L and
SBR
ENR-25 ENR-25. The tensile properties of SBR were found to be the lowest of the three rubbers at
a similar chitosan loading. The rubber-ller interaction for all three types of rubber
decreases with chitosan loading. Morphological studies of the tensile fractured surface of
the vulcanisates using scanning electron microscopy (SEM) indicated that chitosan inter-
acts less well with SBR than STR 5L and ENR-25.
2011 Elsevier Ltd. All rights reserved.

1. Introduction regarding the disposal of these materials at the end of their

Natural rubber is one of the most important elastomers
widely used in industrial, technological and engineering
elds due to its superior and unique mechanical properties
that make it an important and irreplaceable material in
certain applications, such as in tires, mountings, gaskets
and seals. Reinforcing rubbers with commercially obtain-
able llers has been a common practice to yield properties
required for intended applications. In recent years, there
have been many studies on nano-sized reinforcing llers
due to great demand for improved material properties.
However, there is also growing environmental awareness
* Corresponding author. Tel.: 60 4 599 6113; fax: 60 4 594 1011.
E-mail address: hana@eng.usm.my (H. Ismail).
useful life.
The incorporation of reinforcing llers from renewable
resources into polymeric materials can result in new
materials with enhanced properties and biodegradability.
This approach has become of major interest in recent years
with the utilization of renewable resources such as cuttle-
bones [1], rice husks [24], oil palms [5], bamboo [6], starch
[7] and chitin [810] in place of commonly used carbon
black, silicates, hard clays and synthetic bres. One of the
advantages of these llers, apart from being biodegradable,
is that they are readily available at low cost compared to
traditional commercial llers.
Chitosan is a linear polymer of a (1 / 4)-linked 2-
amino-2-deoxy-b-D-glucopyranose obtained from the N-
deacetylation of chitin, a common structural polymer
found in exoskeletons [11]. The primary source of chitin

0142-9418/$ see front matter 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymertesting.2011.07.003
 H. Ismail et al. / Polymer Testing 30 (2011) 784790
and chitosan are crustaceans such as crabs, shrimp and
lobsters, which are highly abundant biomasses due to the
food and beverage and canning industries. Due to its
physical and chemical properties, chitosan has received
much attention as a functional biopolymer and is being
used in a wide range of applications ranging from
biomedical engineering, pharmaceutical and cosmetic
products to water treatment and plant protection [12].
Despite the efforts made in these elds, there are few
studies that have been reported on the incorporation of
chitosan into rubber, especially natural rubber
compounds. However, attempts have been made to blend
chitosan with natural rubber latex [1316]. In this study,
we have concentrated on incorporating chitosan as a new
type of ller in rubber compounds. One of the most
important requirements for chitosan to be successfully
employed as a ller is ensuring good interaction with the
rubber at a reasonable loading level. Therefore, the effect
of chitosan loading on the curing characteristics, tensile
properties and morphology of chitosan-lled natural
rubber (NR), epoxidised natural rubber (ENR) and
styrene-butadiene rubber (SBR) are reported.
2. Experimental
2.1. Materials
Natural rubber grade STR 5L, purchased from Zarm
Scientic & Supplies Sdn. Bhd., Penang, epoxidised
natural rubber with 25 mol% epoxidation (ENR-25)
supplied by the Rubber Research Institute Malaysia
(RRIM) and styrene-butadiene rubber (SBR), Taipol 1502,
purchased from TSRC Corporation, Taiwan were used as
the matrices. Chitosan powder with an average particle
size of 90 mm was obtained from Hunza Nutriceuticals
Sdn. Bhd., Penang. The chitosan was dried in a vacuum
oven at 70  C for 3 h prior to use to expel moisture. The
other compounding ingredients used were zinc oxide,
stearic acid, N-cyclohexyl-2-benzothiazole sulphonamide
(CBS), 6-tert-butyl-4 methyl-phenol (BKF) and sulphur,
which were all were purchased from Bayer (M) Ltd and
used as received. Toluene was purchased from Baker
Aldrich (M) Ltd.
2.2. Mixing and cure assessment
The mixing and compounding of chitosan with STR 5L,
ENR-25, SBR and the other ingredients, as shown in Table 1,
were performed using a laboratory sized two-roll mill
model XK-160. The curing characteristics of the compounds
were determined with a Monsanto Rheometer MDR 2000
according to ISO 3417 at 150  C. The compounds were later
compression moulded at 150  C according to the respective
t90 values.
2.3. Measurement of tensile properties
Dumbbell shaped test pieces were cut from moulded
sheets previously conditioned for 24 h at room tempera-
ture. Tensile tests were performed using an Instron IX3366
machine at a crosshead speed of 500 mm/min according to
785
Table 1
Composition of rubber compounds.
Materials Compounds (phr)d
Rubber a
100
Zinc oxide 5
Stearic acid 3
BKFb 1
CBSc 0.5
Sulphur 2.5
Chitosan 0, 10, 20, 30, 40
a
STR 5L, ENR-25 or SBR.
b
6-tert-butyl-4 methyl-phenol.
c
N-cyclohexyl-2-benzothiazole sulfonamide.
d
parts per hundred rubber.
ISO 37. The tensile modulus (M100 and M300), tensile
strength and elongation at break (Eb) were obtained from
the tests.
2.4. Measurement of rubber-ller interactions
The rubber-ller interaction was determined by
swelling the cured compounds in toluene according to ISO
1817. Test pieces with dimensions of 30 mm  5 mm
 2 mm were prepared from the moulded sheets. The
initial weights were recorded prior to testing. The test
pieces were then immersed in toluene and conditioned at
25  C in a dark environment for 72 h. After the conditioning
period, the weights of the swollen test pieces were recor-
ded. The test pieces were then dried in an oven at 70  C for
15 min and allowed to cool at room temperature for
another 15 min before the nal weights were recorded. The
Lorenz and Park equation has been applied in this study
[17]. The swelling index was calculated according to
Equation (1):
Q f =Q g aez b (1)
where the subscripts f and g refers to lled and gum
vulcanisates, respectively, z is the ratio by weight of the
ller to the rubber hydrocarbon in the vulcanisates and
a and b are constants. Higher Qf/Qg values reect weaker
interactions between the ller and matrix. In this study, the
weight of toluene uptake per gram of rubber hydrocarbon
(Q) was calculated according to the following relation:
Q swelled weight  dried weight=initial weight
 100=formula weight
2.5. Scanning electron microscopy observation of the tensile
fractured surfaces
The tensile fracture surfaces of the vulcanisates were
investigated with a ZEISS SUPRA 35VP scanning electron
microscope with a GEMINI eld-emission column. The
main purpose of this evaluation was to observe the degree
of dispersion of chitosan in the rubbers and to evaluate the
bonding between the chitosan and different types of
rubber. The fractured test pieces were coated with a thin
layer of gold-palladium to eliminate electrostatic charge
build-up during examination.
786 H. Ismail et al. / Polymer Testing 30 (2011) 784790
Fig. 1. Effect of chitosan loading on the scorch time of rubber compounds.
3. Results and discussion
3.1. Curing characteristics
Figs. 13 show the effect of chitosan loading on the
curing characteristics of chitosan-lled rubber compounds
as determined with a Monsanto Rheometer. It can be
observed from Figs. 1 and 2 that there is a signicant
decrease in scorch and cure times with the addition of
chitosan in all three types of rubber, and the values further
decrease as chitosan loading increases. The observed
reduction in scorch and cure times is an indication of the
enhancement of the cure rate. In most cases, cure
enhancement is a consequence of ller parameters such as
surface area, surface reactivity, particle size, moisture
content and the presence of metal oxides [18]. However, in
this study, the cure enhancement was possibly attributed to
the formation of bonds due to the interaction between the
chitosan functional groups (OH and NH2 groups in chi-
tosan) and the compounding additives. Such observation
has been reported by El-Helan et al. [19] in their studies of
chitosan and agar.
Another important factor is the longer mixing time
required to homogeneously blend higher loadings of chi-
tosan with the rubber. A shearing force is applied to the
Fig. 2. Effect of chitosan loading on the cure time of rubber compounds.
Fig. 3. Effect of chitosan loading on the maximum torque of rubber
compounds.
materials during the compounding process. This force
results in friction, which then generates heat. The extra
heat accumulated from longer compounding time will
cause the compounds to undergo premature curing [21]
and, therefore, result in shorter scorch and cure times.
At similar chitosan loading, Figs. 1 and 2 show the scorch
time and cure time of chitosan-lled SBR compounds to be
the longest compared to STR L and ENR-25. Such an
observation for SBR may be due to the higher overall
apparent activation energy of the vulcanisation rate of this
compound. Chough and Chang [22] reported that the
vulcanisation rate of rubber increases in proportion to the
number of allylic hydrogen atoms in the statistical repeat
unit, whereby a higher content of allylic hydrogen resulted
in a lower overall apparent activation energy of vulcani-
sation. In general, a statistical repeat unit of natural rubber
(STR 5L and ENR-25) and SBR have 7 and 3.3 allylic
hydrogen atoms, respectively [22]. This fact explains the
higher scorch and cure time of SBR as compared with STR
5L and ENR-25. Natural rubber has the same reactivity as
ENR-25, but the presence of epoxide groups in ENR-25,
which activate the adjacent double bonds, make it more
susceptible to vulcanisation and, therefore, lowers the
scorch and cure times.
Fig. 4. Effect of chitosan loading on the tensile strength of rubber
compounds.
 H. Ismail et al. / Polymer Testing 30 (2011) 784790
Fig. 5. Effect of chitosan loading on the modulus at 100% elongation of
rubber compounds.
Fig. 3 shows that the maximum torque (MH) values for
all three types of rubber increase as the chitosan loading
increases. The increment in the maximum torque values
indicates that the presence of llers in the compounds
tends to reduce the mobility and exibility of the macro-
molecular chains of the rubber [2326].
At a similar chitosan loading, the maximum torque
values assume the following order: SBR > ENR-25 > STR 5L.
This is due to the properties exhibited by the different types
of rubber. In SBR, the presence of styrene pendant groups
along the rubber chains hinders the movement of the
rubber chains due to their bulkiness and, therefore, the
torque is higher compared to that of ENR-25 and STR 5L.
3.2. Tensile properties
Figs. 47 show the effect of chitosan loading on the
tensile properties of chitosan-lled rubber compounds
measured with an Instron machine. It can be observed in
Fig. 4 that the tensile strength of all three compounds drops
with the addition of chitosan. This may be due to the size
and geometrical factor of the ller, whereby irregular sha-
ped llers tend to decrease the strength of composites due
Fig. 6. Effect of chitosan loading on the modulus at 300% elongation of
rubber compounds.
787
Fig. 7. Effect of chitosan loading on the elongation at break of rubber
compounds.
to the inability of the llers to support the stress trans-
ferred from the matrix [27]. Large particle sized ller
provides a smaller surface area, which gives rise to
a weaker interaction between the ller and rubber matrix
[20]. SEM observation of the chitosan particles (Fig. 8)
revealed that they had these characteristics.
However, at a similar loading, the tensile strengths of
the compounds assume the following order: STR 5L > ENR-
25 > SBR. The highest tensile strength was exhibited by the
STR 5L compounds due to the ability of the natural rubber
chains to undergo strain-induced crystallisation. The
lowest tensile strength was exhibited by the SBR rubber,
which may be attributed to the presence of bulky side
groups that hinder the crosslinking process.
As shown in Figs. 5 and 6, overall, the tensile moduli of
the rubber compounds at 100% and 300% elongation
increase with the addition of chitosan and increase further
as chitosan loading is increased. This indicates that the
addition of chitosan reduces the elasticity of the rubber
chains [2426]. The increase in tensile modulus can be
associated with the maximum torque values of the rubber
compounds, which increased with ller loading.
At a similar loading, the tensile moduli at 100% and 300%
elongation of ENR-25 showed higher values than STR 5L and
Fig. 8. Micrograph of chitosan particles taken at magnication of 50.
788 H. Ismail et al. / Polymer Testing 30 (2011) 784790
Fig. 9. Effect of chitosan loading on the rubber-ller interactions of rubber
compounds.
SBR. This might be due to the presence of ether crosslinks
stemming from acid-catalysed ring-opening reactions in the
ENR-25 compounds, which increase the stiffness of these
compounds above that of the others. This is in perfect
agreement with the observation of Ismail et al. [28].
The elongation at break (Eb) observed in Fig. 7 gradually
decreases with chitosan loading. The reduction of the
elongation at break is mainly caused by the increasing
brittleness of the composite as a result of the transition
from a rubber to a plastic phase with increasing chitosan
loading [29]. The increase in ller loading will tend to
restrict the exibility of the rubber chains and, therefore,
cause the rubber vulcanisates to fail at a lower elongation.
At a higher loading of chitosan, the elongation at break
decreases further as a result of the increasing dominance of
ller-ller interactions in the compound [18].
Fig. 10. (a) SEM Micrographs of unlled compounds of STR 5L taken at magnication of 300. (b) SEM Micrographs of unlled compounds ENR-25 taken at
magnication of 300. (c) SEM Micrographs of unlled compounds of SBR taken at magnication of 300.
At a similar loading, the elongation at break (Eb)
exhibited by chitosan-lled SBR compounds showed the
lowest values. This might be due to the presence of bulky
side groups, which restrict the exibility of the rubber
chains and produce a stiffer rubber compound.
3.3. Rubber- ller interactions
The rubber-ller interactions (Qf/Qg) of chitosan-lled
STR 5L, ENR-25 and SBR compounds with different chito-
san loading are shown in Fig. 9. It can be observed that,
overall, the Qf/Qg increases with increasing chitosan
loading. The increase in Qf/Qg indicates that the rubber-
ller interaction weakens with the addition of chitosan
and weakens further with higher chitosan loading. The
poor interaction between chitosan and STR 5L, ENR-25 and
SBR might be attributed to the incompatible nature of the
constituents: rubber exhibits hydrophobicity and chitosan
exhibit hydrophilicity. A similar observation was reported
by Ismail and Haw [27] for palm ash and natural rubber.
However, at similar chitosan loading, the SBR compounds
exhibited the highest Qf/Qg values compared to STR 5L and
ENR-25. This indicates that the rubber-ller interaction is
much weaker in chitosan-lled SBR compounds, which is in
agreement with the tensile strength results.
3.4. Morphological studies of tensile fractured surface
Fig. 10 shows SEM micrographs of unlled STR 5L, ENR-
25 and SBR compounds taken at a magnication of 300-x.
The micrographs reveal that the fracture surface exhibits
greater matrix tearing in STR 5L (Fig. 10a) compared to the
ENR-25 (Fig. 10b) and SBR (Fig. 10c) compounds. The
rougher surface observed in the STR 5L compound (Fig. 10a)
 H. Ismail et al. / Polymer Testing 30 (2011) 784790 789

Fig. 11. (a) SEM Micrograph of chitosan lled compounds of STR 5L at 10 phr chitosan loading taken at magnication of 150. (b) SEM Micrograph of chitosan
lled compounds of ENR-25 at 10 phr chitosan loading taken at magnication of 150. (c) SEM Micrograph of chitosan lled compounds of SBR at 10 phr chitosan
loading taken at magnication of 150. (d) SEM Micrograph of chitosan lled compounds of STR 5L at 40 phr chitosan loading taken at magnication of 150.
(e) SEM Micrograph of chitosan lled compounds of ENR-25 at 40 phr chitosan loading taken at magnication of 150. (f) SEM Micrograph of chitosan lled
compounds of SBR at 40 phr chitosan loading taken at magnication of 150.

indicates that the matrix tearing has contributed to 4. Conclusions

a higher tensile strength.
The SEM micrographs in Fig. 11 show the fractured
surfaces of STR 5L, ENR-25 and SBR compounds with 10 phr
(Fig. 11ac) and 40 phr (Fig. 11df) chitosan taken at
magnication of 150-x. With increasing chitosan loading,
the fractured surfaces show poor dispersion and adhesion
of chitosan to STR 5L, ENR-25 and SBR (Fig. 11ac), whereby
there were agglomerations and signicant detachment of
chitosan from the lled compound. Greater detachment (as
circled) can be seen in the rubber compounds with 40 phr
chitosan (Fig. 11df). The formation of holes indicates that
the resulting chitosan detachments have contributed to the
reduction in tensile strength with increasing chitosan
loading. However, at a similar loading, the SEM micro-
graphs show that more signicant detachment occurs in
SBR compounds as a result of the poor interaction between
the chitosan and rubber which contributes to the lower
strength of these compounds.
From this study, the following conclusions can be drawn.
1. Overall, the scorch time (tS2), cure time (t90), tensile
strength and elongation at break (Eb) decreased with
chitosan loading, whereas the maximum torque (MH)
and the tensile modulus (M100 and M300) increased for
all three types of rubber compound.
2. At a similar chitosan loading, the characteristic cure
values of SBR were found to be longer (for tS2 and t90) and
higher (for MH) than those of STR 5L and ENR-25. The
tensile properties of SBR at a similar chitosan loading
were found to be the lowest of the three materials.
3. The rubber-ller interactions for all three types of rubber
decreased with increasing chitosan loading.
4. Morphological studies of the tensile fractured surfaces of
the vulcanisates indicated that chitosan interacts less
well with SBR than with STR 5L and ENR-25.
790 H. Ismail et al. / Polymer Testing 30 (2011) 784790
Acknowledgements
Shazlin Mohamed Shaari (S.M. Shaari) wishes to thank
Universiti Sains Malaysia for the nancial support under
the USM fellowship scheme in pursuing her PhD study.
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