Original article

Journal of Reinforced Plastics and

Composites
Mechanical properties of PP/kenaf 0(0) 1–8
! The Author(s) 2018
core nanocomposites made from Article reuse guidelines:
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nanocrystalline cellulose as an additive DOI: 10.1177/0731684418804882
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Fatimah Athiyah Sabaruddin1, Paridah Md Tahir1,2 and

Seng Hua Lee1

Abstract
Kenaf core contains a fairly high amount of cellulose and lignin; hence, any attempt to use both components would be
beneficial. In this study, kenaf core was used as reinforcement in PP/kenaf core nanocomposites. The core was prepared
in two forms: (i) as micron-size reinforcement and (ii) as nanocrystalline cellulose. The bleaching process for nanocrys-
talline cellulose was conducted at different intensities in order to retain different amounts of lignin in the pulp. Then, the
nanocrystalline cellulose was prepared via hydrolysis reaction. Both the micron-size kenaf core pulp and the nanocrys-
talline cellulose of different bleaching intensity were loaded in the polypropylene matrix with the aid of maleic anhydride
grafted polypropylene coupling agent. The mixtures were then hot pressed at 180
C for 8 min to form into standard
testing size sample according to standard ASTM D638 (dumbbell shape for tensile test) and D790 (for flexural and
impact test). The chemical, mechanical and morphological properties of the composites were evaluated. The results
revealed that composites added with unbleached nanocrystalline cellulose (11.48% lignin content) had lowered the
tensile and flexural strength. On the contrary, the impact strength was increased when unbleached nanocrystalline
cellulose was added.

Keywords
Kenaf core, nanocellulose, lignin, chemical analysis, scanning electron microscopy

Introduction
Kenaf fibre is one of the well-known natural fibres that
possess the ability as reinforcement. It contains high cel-
lulose content, and thus has high tensile strength, good
ductility properties and is not brittle.1 Many researchers
have reported the use of kenaf fibre, especially in PP
matrix to improve the mechanical strength of the com-
posite. In most studies, kenaf bast is chosen over kenaf
core due to its length and mechanical strength and there-
fore more suited for high mechanical strength applica-
tion as reinforcement in composites.2–5 However, kenaf
core which comprises almost 60–65% (w/w) of the
whole kenaf stem has low density (approximately 100
kg/m3), porous structure and comparable cellulose con-
tent to that of wood (almost 45%) which make it a good
prospect for the biochemical source of cellulose deriva-
tives.6,7 Lignin is another important chemical compo-
nent after cellulose in most plants. In the pulping
process, lignin has been considered as an unwelcome
component as it influences the severity of the pulping
process. In the production of nanocrystalline cellulose
(NCC), it usually commences with the production of
pulps. Bleaching is needed in order to remove the resid-
ual lignin. This bleaching process, however, generates
waste usually in the form of liquid. Regardless of the
method of bleaching, the effluent may have a certain
characteristic which can damage the environment
because some by-products from the delignification pro-
cess cannot be broken down and discharge into the envi-
ronment.8 Nowadays, lignin by-products have been
1
Institute of Tropical Forestry and Forest Products (INTROP), Universiti
Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia
2
Faculty of Forestry, Universiti Putra Malaysia, 43400 UPM Serdang,
Selangor, Malaysia
Corresponding author:
Paridah Md Tahir, Institute of Tropical Forestry and Forest Products
(INTROP), Jalan Asam Jawa, Selangor 43400, Malaysia.
Email: parida@upm.edu.my
2 Journal of Reinforced Plastics and Composites 0(0)
utilised for many applications instead of being disposed
of including resin adhesives for polymer blending, and
for the preparation of low-molecular weight fuel addi-
tives.9,10 Lignin also has the potential to act as a com-
patibilizer since it contains both polar hydroxyl groups
and non-polar hydrocarbon and benzene rings thus
make it eligible to play the role as compatibility enhanc-
er between matrix and reinforcement and improve the
mechanical properties of a composite.11 These applica-
tions of lignin, however, are in the form of isolation or
extraction products.
Therefore, in this study, the lignin was let to remain
in the pulps by limiting the bleaching intensity and
analyzed to compare its function with isolated lignin.
This study was then focused on the production of
PP/KC/MAPP nanocomposites loaded with NCC
(bleached and unbleached). The objective of this
study is to determine the effects of NCC with different
bleaching intensity on the mechanical properties of PP/
KC/MAPP composites.
Experimental
Materials
Raw kenaf core fibres (Hibiscus cannabinus) were sup-
plied by the National Kenaf and Tobacco Board
(LKTN), Kota Bharu, Kelantan, Malaysia.
NCC preparation
Kenaf core chips (200 g) of 2–3 cm long were placed in a
twin digester with 20% NaOH and 0.1% anthraquinone
(AQ). The ratio of cooking liquid was 1:10 and was
cooked at 170
C for 1 h 30 min. The kenaf pulp was
later bleached through three-stage bleaching to generate
pulps of different lignin content. Table 1 shows the
bleaching conditions employed in the study which cor-
responds to the types of pulp produced: (a) B1, for pulps
bleached using stage D1 only, (b) B2, for pulps bleached
following stages D1, Ep and D2 and (c) UB, for pulps
without undergoing bleaching sequence.
The NCC was then prepared by treating the kenaf
core pulps (types UB, B1 and B2) with sulfuric acid.
The pulps were stirred vigorously in the sulfuric acid
solution of different concentrations for 60 min at 45
C
and rinsed using multiple centrifugations until the solu-
tion becomes a cloudy suspension. The concentration
Table 1. Bleaching conditions used in the study.
Bleaching stage Chemical charge
D1 2% sodium chlorite þ 3% acetic acid
EP 1.5% NaOH þ 1% H2O2
D2 1.5% sodium chlorite þ 3% acetic acid
of acid sulfuric used for each type of pulp was varied
depending on the lignin content (60%, 62% and 64%
of H2SO4 for UB, B1 and B2 pulps, respectively). The
process was continued with dialysis using cellulose
membrane until the pH changed from acidic to neutral.
The suspensions were then sonicated for 30 min before
they were freeze dried.
Nanocomposites preparation
A specific amount of NCC (0.5 or 1% w/w) was blend-
ed with 40% w/w kenaf core fibre and 59% w/w poly-
propylene matrix; 1% w/w of MAPP was added as the
compatibilizer. All materials were mixed using the
internal mixer at rotor speed and temperature of 50 r/
min and 170
C, respectively. Solid mixture products
from the mixing were crushed using the crusher to
make sure the homogeneity of the mixture before
being pressed using the hot press. The crushed products
were placed into a mould and were pressed at 180
C for
a total of 8 min: 3 min for melting to take place and 5
min for curing. A set of composites using 40% w/
w kenaf core fibre, 59% w/w PP matrix and 1% w/
w of MAPP without the addition of NCC was pro-
duced to serve for comparison purpose. The control
samples were denoted as PP/KC/MAPP.
Testing methods
Chemical analysis. Lignin determinations for kenaf pulp
before and after bleaching process were analysed using
TAPPI T222 om-02. The sample was hydrolysed in 72
wt.% H2SO4 at 20
C for 2 h and boiled for 4 h. The
precipitate was cooled, filtered and dried. The mass of
dried lignin was analysed.
FTIR test. FTIR tests were done using Perkin Elmer
(Spectrum-100) machine at frequencies range of 500–
4000 cm1 and the results were plots according to their
IR transmission over frequency.
Mechanical tests. For the mechanical test, the tensile and
flexural tests were done according to ASTM D638M
and ASTM D790 standard, respectively. Impact test
was performed according to ASTM D256 standard
using CEAST impact tester.
Reaction time (min) Temperature (oC) Consistency (%)
120 70 10
90 70 10
90 60 10
Sabaruddin et al.
Morphological test. The morphological characterization
was established using JSM-6400 scanning electron micros-
copy (SEM) upon sample that coated with carbon coating.
Results and discussion
Chemical content determination
Table 2 shows the lignin percentage of raw kenaf core,
alkaline-treated kenaf core and bleached kenaf core.
Generally, the amount of lignin in wood varies from
ca. 12% to 39% according to Klason lignin analysis.9
The lignin content of raw kenaf core shows that the
amount of 33.69% falls within this range. The lignin
content was observed to drop from 33.69% to 11.48%
and contributed to the effectiveness of sodium hydrox-
ide as the alkaline agent to remove the lignin content.
The content of lignin continued to drop after the first
and second stages of bleaching to 9.16% and 2.23%,
respectively and indicates that the amount of lignin
was expelled in stages according to the bleaching steps.
The lignin that still intact within the fibre, however,
impedes the function of acid to hydrolyse the amor-
phous region during the acid hydrolysis process.12
Therefore, modification of acid sulfuric intensity is
needed to assist the production of NCC.
Fourier transform infra-red
FTIR analysis. Figure 1 shows the spectra for PP/KC/
MAPP with and without the addition of different type
of 1% w/w NCC, NCC-UB and NCC-B2. The absorp-
tion peaks in the range of 3400–3300 cm1 were refer-
ring to stretching and bending of hydroxyl (O–H)
groups of cellulose and absorbed water on fibres.
Meanwhile, peaks at 2920 cm1 correspond to CH
stretching and ether linkages from the pyranose ring of
the cellulose.13–16 All nanocomposites samples share
these same peaks which may be attributed to the pres-
ence of kenaf core fibres. After the addition of NCC,
peaks at 1727 and 1729 cm1 appear for both samples,
PP/KC/MAPP/NCC-B2 and PP/KC/MAPP/NCC-UB
Table 2. Lignin content of kenaf core before and after blech-
ing process.
Sample Bleaching stage % Lignin
Raw kenaf core – 33.69
Unbleached kenaf – 11.48
core – UB
Bleached kenaf D1 9.16
core (once) – B1
Bleached kenaf D1, Ep, D2 2.23
core (twice) – B2
3
respectively, which refers to the stretching of the carbon-
yl group (C = O) of acetyl acid group in hemicellulose.
Besides, the peaks in the range of 1609–1631 cm1
correspond to stretching and bending of hydroxyl
groups of absorbed water on fibres, while the peaks at
1237 cm1 correspond to C–O stretching of aryl group in
lignin. The intensity of the peaks increased after the addi-
tion of NCC and continued to increase with the addition
of NCC with the least lignin content. According to
Zainuddin et al.,16 these peaks represent the important
functional groups of hemicellulose and lignin was
completely absent. Intense peaks were observed for all
samples at 1037 cm1 which represent the C–O stretching
and C–H rocking vibrations of the pyranose ring skeleton
of the cellulose in both kenaf core fibres and NCC.16–18
The last peak at 823 cm1 refers to COC, CCO and CCH
deformation and stretching vibration.19 This peak only
appears on spectra of the sample without NCC addition.
All the above characteristic absorption peaks prove the
existence of three polymeric constituents in kenaf core,
cellulose, lignin and hemicellulose, as well as the NCC in
nanocomposites. Other than peaks that represent kenaf
core and NCC in the spectra, there are also a few spec-
trum peaks that denote pure PP as the matrix in the nano-
composites. For example at peak 2920 cm1, this peak
corresponds to PP characteristic bands of C–H stretch-
ing.20 On the other hand, peaks at 1455 cm1 and 1373
cm1 represent asymmetric vibrations of H atoms of CH2
and symmetric vibration of H atoms of CH2 of the ethyl
functional group, respectively.21
Tensile properties
Figure 2 compares the tensile strength of PP and the
hybrid composites produced in this study. The tensile
Figure 1. The IR spectroscopy of PP/KC/MAPP with and
without NCC.
MAPP: maleic anhydride grafted polypropylene; NCC: nano-
crystalline cellulose.
4 Journal of Reinforced Plastics and Composites 0(0)
Figure 2. The tensile properties of PP and PP/KC/MAPP with and without NCC loading.
MAPP: maleic anhydride grafted polypropylene; NCC: nanocrystalline cellulose.
strength of the composite increases with the addition of
40% w/w kenaf core fibres with the addition of 1% w/
w of MAPP as coupling agent. The 9.8% increment can
be attributed to the much higher strength and stiffness in
kenaf fibre as compared to the matrix,22 as well as the
presence of MAPP that improved the fibre–matrix inter-
action results in better adhesion and interfacial strength
that eventually increased the strength.23. The effect of
NCC addition revealed a mix result on the tensile
strength. For instance, there is slight decrement from
21.98 MPa to 20.97 MPa which occurred when PP/
kenaf core was added with 0.5% of unbleached NCC
(NCC-UB). Increasing the NCC-UB content to 1%
reduced the tensile strength even further. However, the
addition of 0.5% NCC of different levels of lignin con-
tent (NCC-B1 and NCC-B2) had resulted in slight incre-
ment of the tensile strength. Similar situation was
observed when the NCC content was increased to 1%.
Comparable values of tensile strength were observed for
composites added with 0.5 and 1% NCC-B2 with values
22.2 MPa and 21.8 MPa, respectively.
NCC-UB contains a relatively high amount of
lignin, 11.48% as compared to both NCC-B1 and
NCC-B2 (9.16 and 2.23%, respectively) due to the
absence of the bleaching process. It is known that
bleaching process does not only remove the lignin sub-
stances in the pulp but also other amorphous materials
including hemicellulose. This hemicellulose is responsi-
ble for moisture absorption of the fibres. It is known
that high moisture absorption can cause deterioration
in the mechanical properties.24–26 Even though lignin
has the potential of being a natural compatibilizer due
to its structure that has both polar hydroxyl group and
nonpolar hydrocarbon and benzene rings,11 this
application is very limited due to the presence of hemi-
cellulose. Therefore, due to this matter, composites that
incorporated with NCC-UB show lower tensile
strength as compared to composite loaded with NCC-
B1 and NCC-B2. The fact that NCC possesses higher
surface area has given more significant impact upon the
properties of the composites than that of kenaf core
fibre because this fibre also has high amorphous mate-
rials within the fibre itself. Agglomeration of the NCC
filler also can cause the deterioration of the mechanical
properties especially when high loading was applied.
The effect of kenaf core addition is more prominent in
tensile modulus of PP/KC/MAPP composites as shown
in Figure 2. A notable increase in stiffness was seen in PP/
kenaf core tensile modulus with an addition of 40% (w/
w) kenaf core. Additions of NCC at different lignin con-
tents also show some effects on the tensile modulus. It
appears that the tensile modulus slightly decreases when
added with NCC-UB but continues to increase gradually
after being added with NCC-B1 and NCC-B2. It is sug-
gested that the presence of lignin in the NCC reduced the
composite compatibility due to the reduction in polarity
in the interphase, which results in increased adhesion
towards PP.10,27 As a result, it lowered the strength and
stiffness of the composites. This result obtained is in line
from what has been reported by Morandim-Giannetti
et al.,27 claiming that the presence of lignin in the com-
posites does lower the tensile strength especially with the
sample that compatibilized with MAPP.
Flexural strength
Figure 3 shows the flexural properties of PP and the
hybrid composites. No significant changes in the
Sabaruddin et al. 5

Figure 3. The flexural properties of PP and PP/KC/MAPP with and without NCC loading.
MAPP: maleic anhydride grafted polypropylene; NCC: nanocrystalline cellulose.

flexural strength were detected either with the additions

of 40% (w/w) kenaf core, 1% (w/w) MAPP or 0.5/
1.0% (w/w) NCC. Nonetheless, a reverse effect was
seen in the flexural modulus. It appears that the addi-
tion of MAPP has improved the interfacial adhesion
and kenaf distribution in the polymer matrix so much
that the superior toughness of the kenaf fibre has been
continuously transferred to PP matrix across the thick-
ness of the specimens resulting in a much higher flex-
ural stiffness. Compared to neat PP composite,
the flexural modulus improved almost 126% with
40% (w/w) addition of kenaf core. This value, however,
decreased around 14.18% with additions of NCC irre-
spective of the amount of lignin content. Apparently,
0.5% of NCC addition is sufficient to retain the flexural
modulus to be above 1900 MPa. A slight decrease in Figure 4. The impact properties of PP and PP/KC/MAPP with
flexural strength upon 1% NCC addition can be and without NCC loading.
MAPP: maleic anhydride grafted polypropylene; NCC: nano-
ascribed to agglomeration of the fibre reinforcement
crystalline cellulose.
and 1 wt.% of MAPP was not enough to aid the dis-
tribution effect upon the reinforcements.
of MAPP, therefore, may not be enough to control
Impact strength
the compatibility between PP matrix and kenaf core
The impact strength of the PP and the hybrid compo- fibre. Saad28 reported in their study that the impact
sites are shown in Figure 4. PP alone shows the highest strength of the composites decreased especially at
impact strength of 0.244 J. As expected, the impact higher filler loading (>30% w/w), whether it is treated
strength decreased markedly (0.077 J) after adding or untreated with MAPP, which may be caused by the
40% w/w of kenaf core. It is suggested that high a- agglomeration of fillers that weakened the interfacial
mount of kenaf core filler may increase the moisture regions and consequently weakened the impact
absorption because of the fact that natural plant strength. The impact strength was then observed to
like kenaf core contains high amount of hydroxyl slightly increase when added with NCC indicated
groups which make them hydrophilic in nature. This increase in strength. It is suggested that NCC can
hydrophilic nature can lead to poor dispersion of fibre help to fill up the space between fibre filler and transfer
filler thus causing the agglomeration and thus lowered the strength to the composites due to its high sur-
the impact strength of the composites.24 The 1% (w/w) face area.
6 Journal of Reinforced Plastics and Composites 0(0)

Figure 5. The morphological depiction of tensile fracture surface of (a) PP/KC/MAPP (b) PP/KC/NCC-UB/MAPP (c) PP/KC/NCC-
B2/MAPP.
MAPP: maleic anhydride grafted polypropylene; NCC: nanocrystalline cellulose.

Morphological properties the agglomeration problem also may lead to

The comparative study of morphology was taken using
SEM on the fracture surfaces of the tensile sample for
PP/KC/MAPP, PP/kenaf core added with NCC-UB
and NCC-B2 are depicted in Figure 5. The morphology
images show a strong interaction between kenaf core
fibre and PP matrix except for the image shown in
Figure 5(b) where there is the formation of cracks
(show in red circle) as a proof of low tensile properties
of this sample. It is suggested that high amount of
lignin, especially from the NCC, had caused incompat-
ibility of the composites. It is known that lignin has
polar and nonpolar groups structure, and therefore it
is assumed that this lignin structure had to be impaired
with the MAPP structure, hence forming a third phase
or separated lignin phase like that has been reported in
Morandim-Giannetti et al.27 Albeit the amount of
lignin in NCC is small in this study as compared to
additional isolated lignin, but the fact that NCC is
having high surface area had caused major affect
towards the properties of nanocomposites. In addition,
this formation of crack. For image shown in Figure 5
(a) and (c), the fracture type can be classified as trans-
granular fracture which indicates a strong bonding
between matrix and reinforcement material.
Conclusion
NCC (0.5 wt.% and 1 wt.%) from kenaf core with
different lignin content (NCC-UB, NCCB1 and
NCC-B2) was successfully loaded in PP/KC/MAPP
composites. The FTIR analysis shows slight changes
in the functional group characteristic of all materials
when NCC was added in the composites especially at
peak around 1237 cm1, 1727–1729 cm1 and 823
cm1. Incorporation of NCC in the PP/KC/MAPP
composites was observed to slightly decrease the tensile
and flexural strength of the composites. However,
slight improvements were observed for impact strength.
The presence of lignin in the NCC, particularly in
unbleached NCC (NCC-UB), had led to the
Sabaruddin et al.
deterioration of the mechanical properties of the nano-
composites due to its incompatibility between PP
matrix. The high surface area of NCC also plays a
major role to prominently expose the effect of lignin
towards mechanical properties of the nanocomposites.
The formation of crack shown by NCC-UB proves the
effect of incompatibility of lignin in the nanocompo-
sites which might be due to the formation of separated
lignin phase. Therefore, NCC with the least lignin con-
tent gives better mechanical properties to the PP/KC/
MAPP composites.
Declaration of conflicting interests
The author(s) declared no potential conflicts of interest with
respect to the research, authorship, and/or publication of
this article.
Funding
The author(s) disclosed receipt of the following financial sup-
port for the research, authorship, and/or publication of this
article: The authors would like to thank The Ministry of
Higher Education Malaysia (KPT) for the financial support
to carry out this study. This study is funded under Higher
Institutional Centre of Excellence (HICoE) Grant
No. 6369109.
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