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Meri-Rastilantie 3 B, FI-00980 Journal of Food, Agriculture & Environment Vol.8 (2): 1103-1108. 2010 www.world-food.net
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The effect of alkali treatment on the mechanical properties of short pineapple leaf
fibre (PALF) reinforced high impact polystyrene (HIPS) composites
J. P. Siregar 1, S. M. Sapuan 1*, M. Z. A. Rahman 2 and H. M. D. K. Zaman 3
1
Department of Mechanical and Manufacturing Engineering, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor,
Malaysia. 2 Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia. 3 Radiation Processing
Technology Division, Malaysian Nuclear Agency, Bangi 43000 Kajang, Selangor, Malaysia.
*e-mail: sapuan@eng.upm.edu.my, drsapuan@yahoo.com

Received 22 September 2009, accepted 2 April 2010.

Abstract
This paper reported the study of the effect of the alkali (NaOH) treatment on the mechanical properties of pineapple leaf fibre (PALF) reinforced high
impact polystyrene (HIPS) composites. The objective of this study was to investigate the effect of alkali (NaOH) treatment with different
concentration of NaOH (0%, 2% and 4%) solution. The mechanical properties such as tensile strength, tensile modulus, flexural strength, flexural
modulus, notched and unnotched impact and hardness of short pineapple leaf fibre (PALF) reinforced high impact polystyrene (HIPS) composites
were studied and compared. NaOH concentration of 4% that was used for the short PALF treatment showed the highest mechanical properties value
compared to the other concentration.

Key words: Pineapple leaf fibre (PALF), alkali treatment, high impact polystyrene (HIPS).

Introduction
The incorporation of lignocellulosic fibres into a thermoplastics silane treatment, isocyanate treatment, latex coating, permanganate
or thermosetting polymer is often associated with poor fibre treatment, acetylation, monomer grafting under UV radiation, etc.
dispersion due to the large differences in polarity between the have received various levels of success in improving fibre strength
fibres and polymer, and strong intermolecular hydrogen bond and fibre matrix adhesion in natural fibre composites.
between the fibres. To obtain a satisfactory performance from the Alkali treatment of cellulosic fibres, also called mercerization, is
composite, it is necessary to have a good fibre distribution within the usual method that often used by some researches to produce
the matrix. A good distribution implies that the fibres are fully a high quality fibres to reinforce polymer matrix. As seen in Table
separated from each other, and each fibre is fully surrounded by 1, all types of natural fibre, such as hemp, jute, ramie, henequen,
the matrix 1. curaua, flax, etc., have been treated with the sodium hydroxide
The mechanical properties of a natural fibre reinforced composite (NaOH) before mixed together with the polymer (thermoplastics
are determined depending on many parameters, such as fibre or thermosetting) to produce composites 6-27. The concentration
strength, modulus, fibre length and orientation, in addition to the of alkali solution that was used to treat the fibres is in the range of
fibre-matrix interfacial bond strength. A strong fibre-matrix interface 0.5% up to 28%, but most of the researchers used below 10%
bond is very critical for composites to have high mechanical alkali solution. The temperature and soaking time to treat the
properties. A good interfacial bond is also required for effective natural fibre in the solution are in the range of 20-180C and 15
stress from the matrix to the fibre whereby maximum utilization of minutes to 48 h period of time, respectively. The required
the fibre strength in the composite is achieved 2. The interfaces temperature to dry a natural fibre should be below 80C for 24 to
act as a binder and transfers load between the matrix and the 48 h period of time.
reinforcing fibres. Hence the interface plays a key role in Pickering et al. 6 studied the optimising of industrial hemp
controlling the mechanical properties of composites 3. fibre for composites. The hemp fibre was treated with the alkali in
Therefore, to improve the interface and adhesion between the the range of 10% or 15% solution, and the temperature and soaking
fibre and the matrix, a third component, which is called time were in the range of 160C or 180C and 15 or 45 min,
compatibilizer, must be used for matrix modification or the fibres respectively. They found that using the treated alkali with
surface have to be initially modified for the preparation of the concentration 10% for 15 or 45 min period of time and treated
composites 4, 5. Some studies have shown the influence of various alkali with concentration of 15% for 15 min period of time at
types of chemical modifications on the performance of natural temperature of 160C could produce stronger fibres. Therefore, it
fibres and the fibre reinforced composites. The different surface is concluded that with the increase in fibre strength for treatment
chemical modifications of natural fibre such as alkali treatment, has been contributed to the increase of packing density and

Journal of Food, Agriculture & Environment,Vol.8 (2), April 2010 1103


Table 1. The alkali (NaOH) treatment of some natural fibres.
Fibre NaOH Soaking time Soaking Drying Reference
(%) temperature (C)
Hemp 10 or 15 15 or 45 min 160 or 180 80C for 48 h 6
Jute Up to 28 30 min 20 - 7
Ramie 15 2h - - 8
Henequen 2 1h 25 60C for 24 h 9
Curaua 10 - - - 10
Flax 1, 2, 3 20 min Room temperature 80C for 48 h 11
Kenaf 3, 6, 9 3h Room temperature Room temperature for 48h 12
Sisal 2 4h 60 80C 24 h 13
PALF 5 30 min - 60C for 24 h 14
Bagasse 1, 3, 5 2h 25 70C for 72 h 15
Piassava 10 - Room temperature - 16
Oil palm 0.5, 1, 2, 4 - - 70C, until constant weight 17
Coir 5 48 h - - 18
Kenaf 6 48 h 192 110C for 5 h 19, 20
Henequen 2 1h 25 60C for 24 h 21
Hemp 6 48 h 202 60C for 48 h 22
Jute 5 4 and 24 h 25 80C, until constant weight 23
Sisal 10 1h - - 24
Coir 2 1h 70 70C, until constant weight 25
Jute 2 1h 70 70C, until constant weight 26
Hemp 0.8-8 48 h 202 - 27

molecular orientation due to the removal of the cementing materials In this study, treatment of the short PALF was carried out using
(i.e. lignin, pectin and hemicellulose). The decrease in strength in many different concentrations of alkali. The chemical treatment
other treatments was due to the degradation of cellulose with (NaOH) used in this study was expected to be able to improve the
high NaOH concentrations at the temperatures above 160C. mechanical properties of short pineapple leaf fibre (PALF)
Herrera-Franco et al. 9 studied the mechanical properties of short reinforced high impact polystyrene (HIPS) composites.
natural-fibre reinforced composites. The surface henequen fibre
was treated with alkali and silane, and it was found that the tensile Materials and Methods
strength of the HDPE/henequen fibres (80:20 v/v) composites Materials: The pineapple leaf fibre (Ananas comosus) was
with an aqueous NaOH or with the pre-impregnation process did obtained from Pemalang, Central of Java, Indonesia. The size of
not really improve the tensile strength if compared to other pineapple leaf fibre that was used in this research is a 10-40 mesh.
modifications. The high impact polystyrene (HIPS) that has been utilised as the
Rout et al. 25 investigated the effect of alkali treatment of coir matrix polymer is the Idemitsu PS HT 50 that has density of 1.04
fibre in polyester/coir composite system. It was reported that using g/cm3 and is produced by the Petrochemical (M) Sdn Bhd, Pasir
2% alkali-treated coir/polyester composites showed a significant Gudang, Johor, Malaysia. The sodium hydroxide (NaOH) was
improvement of the tensile strength. Valadez-Gonzalez et al. 21 supplied by the Aldrich Chemical Company, Malaysia.
reported that using alkali treatment for henequen fibre improved
the fibre/matrix mechanical interlocking as well as the interaction Alkali (NaOH) treatment: The short pineapple leaf fibre was
between fibre and matrix. soaked in different concentrations (0%, 2% and 4%) of NaOH
Ray et al. 28 have observed the effects of 5% NaOH treatment of solution in the water bath for 1 hour at room temperature. The
jute fibre at room temperature for several varying times (2, 4, 6 and ratio of the fibres and the solution was 1:20 (w/v). After treatment,
8 h). The composite that was prepared with previously treated the fibres were washed and rinsed several times with distilled
fibres showed the maximum improvement for all volume percentage water. Afterwards the fibres were dried in an oven at 80C for 24
of fibre loadings. The flexural strength properties of the composites hours.
at 35% volume fibre loading after being treated for 4 h with alkali
treatment was 238.9 MPa in contrast to the result of 199.1 MPa Compounding: A 50 wt.% untreated and treated fibre content of
that was obtained for composites with untreated fibres. short PALF/HIPS composite was chosen in order to determine the
From the reviews and results of the effect of alkali treatment for effect of using different concentration of alkali for treatments on
natural fibre by previous researchers, it can be concluded that the mechanical properties of short PALF/HIPS composites. The
using alkali (NaOH) solution to treat the natural fibre is one of the short PALF was mixed into the HIPS matrix using a Brabender
chemical treatment methods that can improve the mechanical Plasticorder intensive mixer, model PL2000-6 for 15 minutes at 165C
properties of natural fibre reinforced polymer composite. The alkali and with 50 rpm screw speed.
treatment can lead to the decrease in the spiral angle and the
increase in the molecular orientation of the cellulose chain 7. The Compression molding: The melt compounded mixture that was
alkali treatments generally result in a rougher fibre topography, obtained from the previous process before was placed in the
which can further improve the fibre matrix adhesion in a composite compression molding (Carver hot press) at 165C temperature and
by providing additional sites for mechanical interlocking 21, 26. The endured the process of preheated for 5 min, fully press heated for
alkali (NaOH) is the most common method that has been used for 5 min and followed by cooling for 5 min and afterward was formed
the treatment of natural fibre because this method is inexpensive20. into sheets with the dimensions of 150 mm x 150 mm x 3 mm.

1104 Journal of Food, Agriculture & Environment, Vol.8 (2), April 2010
The specimens for the mechanical test were obtained from the Table 2. The effect of alkali treatment of short PALF on the
composites sheets that were formed according to ASTM standards. mechanical properties of short PALF/HIPS.
Mechanical property NaOH concentration, %
Mechanical testing: 0 2 4
Tensile testing: All tension testing specimens were cut into a Tensile strength (MPa) 22.640 25.717 29.955
dog-bone shape. The tensile test were conducted following the (1.250) (1.251) (1.356)
standard of ASTM D638 type V using Instron (Model 4301) Tensile modulus (MPa) 824.646 1197.751 1284.845
(156.374) (66.431) (133.881)
universal testing machine with load cell of 1 kN and using Flexural strength (MPa) 31.661 34.371 40.789
crosshead speed of 1 mm/min. The test was performed until the (3.251) (1.832) (2.496)
tensile failure occurred. There were seven specimens that have Flexural modulus (MPa) 4294.024 4464.058 4559.339
been tested, but only the result of five specimens was calculated (399.515) (122.408) (280.989)
Notched impact (J/m) 24.39 47.164 52.417
to get the average tensile value.
(1.342) (3.187) (1.580)
Unnotched impact (J/m) 45.460 64.615 76.959
Flexural testing: Three points bend testing was carried out (2.764) (1.124) (5.535)
following the ASTM D790-97. The test methods are for flexural Hardness scale L 84.120 89.260 90.820
properties of unreinforced and reinforced plastics and electrical (0.614) (1.124) (0.709)
Note: Values are average of five samples determinations. Values in parentheses are standard deviations.
insulation materials. The similar Instron universal testing machine
(Model 4301) that has been used for the tensile test was also used
in this experiment for flexural testing. The applied load and the
crosshead speed were specified at 1 kN and 1.3 mm/min,

Tensile strength (MPa)


respectively, while the support span was 48 mm. For flexural test
the samples were prepared and cut into rectangular specimens
with 127 mm (L) x 12.7 mm (W) x and 3 mm (T) dimensions.

Izod impact strength: Izod impact test has been used extensively
to determine the impact resistance of any materials. The Izod
impact test was carried out for the notched and unnotched samples
with dimensions of 63.5 mm x 12.7 mm x 3 mm. The Izod impact
strength is reported as energy per unit notch (J/m). The pendulum
energy that was employed for the testing purpose was 4 Joule.
This test was carried out according to ASTM D256-93. Figure 1. Effect of alkali concentration on tensile strength of PALF/
HIPS composites.
Rockwell hardness strength: Hardness is generally used to
describe a resistance of material to surface indentation, scratching
or marring. The experiment was carried out using the Rockwell
Hardness Tester HA-101 in accordance to ASTM D 785 procedure
Tensile modulus (MPa)

B. The Rockwell hardness was measured using a 0.625 mm ball


and 60 kg of indent force (Rockwell scale L).

Results and Discussion


From the results in Table 2 it can be seen that each of the three
alkali treatment variables had effects on the tensile strength, tensile
modulus, flexural strength, flexural modulus, impact notched,
impact unnotched and hardness of the short PALF reinforced
HIPS composites. The increased concentration of alkali treatment
from 0% to 4% of NaOH increased the mechanical properties of
PALF/HIPS composites. Figure 2. Effect of alkali concentration on tensile modulus of PALF/
HIPS composites.
Effect of alkali treatment on tensile properties: The effects of
alkali treatments (0%, 2%, and 4%) of short PALF fibres on the (2% and 4%) fibre composites is attributed to the improved wetting
tensile strength and tensile modulus were examined using the of alkali-treated short PALF with HIPS.
treated fibre (50% weight) composites. As seen from Figs 1 and 2, Similar results were found by Jacob et al. 29 in case of sisal/oil
the 2% NaOH-treated fibre composites improved the tensile palm hybrid fibre reinforced natural rubber composites. The fibres
strength and tensile modulus by 12% and 31%, respectively, were treated with different concentrations of NaOH (0.5, 1, 2, 4
compared with the untreated fibre composites. With further and 10%) for 1 hour at room temperature. It was found that the
increase of the NaOH concentration to 4%, the tensile strength maximum tensile strength was obtained for the fibres that have
and tensile modulus were also increased to 24% and 35%, been treated previously with 4% NaOH. Nevertheless after the
respectively, in comparison to the untreated fibre HIPS composites. alkali treatment, the diameter and weight of the fibres were
The enhancement in mechanical properties in alkali-treated decreased due to the removal of lignin.

Journal of Food, Agriculture & Environment,Vol.8 (2), April 2010 1105


The superior tensile strength value of alkali-treated could be The effect of alkali treatment on hardness properties: Fig. 7 shows
attributed to the fact that the alkali treatment improved the adhesive the Rockwell hardness results of short PALF/HIPS composite.
characteristics of fibre surface by removing natural and artificial With alkali treatment of 2% and 4% NaOH the hardness value of
impurities which thereby producing a rough surface topography. composites increased. The lowest result of the hardness test,
In addition, alkali treatment leads to fibre fibrillation, i.e. breaking 84.120, derived from the untreated short PALF composite,
down of the fibre bundles into smaller fibres. This has increased meanwhile for the short PALF treated with 2% and 4% NaOH, the
the chance of the effective surface area to be more available for obtained results for the hardness test had better values, 89.260
contact with matrix polymer 30. and 90.260.
Contrary results were found by George et al. 31 with the case of
different alkali concentration to improve adhesion of PALF/PE
composites. The PALF was treated with different concentrations
of NaOH (1% and 5%) and when the PALF was treated with 1%

Flexural strength (MPa)


NaOH, the mechanical properties of longitudinally oriented PALF/
PE composites at different fibre loading were improved. Meanwhile
when using 5% NaOH the tensile strength and tensile modulus
were decreased. It was also concluded that using the higher
concentration of alkali (5%) for treatment will cause the fibre to
lose its characteristics. On the other hand, when using lower
concentration of NaOH for treatment, the complete removal of
lignin on the fibres is not possible. Fibres become thinner upon
alkali treatment. This may be due to dissolution and leaching of
fatty acids and some of the lignin component of the fibre. As the
result, the surface of the fibre becomes rough, and will promote Figure 3. Effect of alkali concentration on flexural strength of PALF/
mechanical anchoring between fibre and matrix. HIPS composites.

Effect of alkali treatment on flexural properties: Figs 3 and 4


show the flexural properties of short PALF/HIPS composites by
alkali-treated fibres. The trend of histogram of flexural strength
Flexural modulus (MPa)

and flexural modulus are similar with the trend of tensile strength
and tensile modulus above. The increased alkali concentration
also increased the flexural strength gradually. The flexural strength
of untreated fibre was 31.661 MPa, meanwhile for the 2% and 4%
of alkali concentration treatments 34.371 MPa and 40.789 MPa ,
respectively. It is also shown that the flexural modulus of untreated
fibre is 4294.515 MPa, whereas for 2% and 4% NaOH concentration
treatments about 4464.068 MPa and 4559.339 MPa, respectively.
Cao et al. 15 reported that for composites composed of the
biodegradable polyester and bagasse fibre, the flexural strength
and flexural modulus were increased when fibre was treated with
1% NaOH solution compared to untreated fibre. Figure 4. Effect of alkali concentration on flexural modulus of
PALF/HIPS composites.
Effect of alkali treatment on notched and unnotched impact
properties: The impact properties could determine the ability of a
material to withstand an impact load, which ability depends on
material toughness. The effect of alkali (NaOH) treatment on the
notched and unnotched impact of short PALF/HIPS composite is
shown in Figs 5 and 6. The untreated fibre has a lower value of
Energy (J/m)

notched and unnotched impact strength compared to 2% and 4%


alkali-treated fibre. The increase of NaOH concentration from 2%
to 4% increased the impact strength of composites from 47.164 to
52.417 J/m for notched impact and from 64.615 to 75.959 J/m for
unnotched impact, respectively. Also Rout et al. 25 found that for
treatment of coir fibre, increasing concentration of NaOH from
2% to 5% increased the impact strength of coir/polyester from
521.9 to 634.6 J/m. Meanwhile, the increased alkali concentration
up to 10% decreased the impact strength of composites. Figure 5. Effect of alkali concentration on notched impact of
PALF/HIPS composites.

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1108 Journal of Food, Agriculture & Environment, Vol.8 (2), April 2010

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