Composites Part B 150 (2018) 277e283

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

Fabrication and characterization of olive pomace filled PP composites

N. Kaya a, M. Atagur b, *, O. Akyuz a, Y. Seki c, M. Sarikanat d, M. Sutcu b,
M.O. Seydibeyoglu b, K. Sever e
a _
Izmir Katip Çelebi University, Institute of Science, Material Science and Engineering Department, Çig _
li, Izmir, Turkey
b _
Izmir Katip Çelebi University, Engineering and Architecture Faculty, Material Science and Engineering Department, Çig _
li, Izmir, Turkey
c _
Dokuz Eylül University, Science Faculty, Chemistry Department, Buca, Izmir, Turkey
d _
Ege University, Engineering Faculty, Mechanical Engineering Department, Bornova, Izmir, Turkey
e _ _
li, Izmir,
Izmir Katip Çelebi University, Engineering and Architecture Faculty, Mechanical Engineering Department, Çig Turkey

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

Article history: The aim of this study is to investigate the filling properties of an agricultural waste, olive pomace powder
Received 7 March 2017 (OP), for polypropylene (PP) matrix material. Different weight fractions of OP (from 10 to 40 wt %), which
Received in revised form has a median particle size of 21.36 mm (D50) mm, were loaded into PP by high-speed thermo kinetic
21 July 2017
mixer. In this research, the effects of weight fraction of OP within PP on mechanical, viscoelastic, thermal,
Accepted 28 August 2017
chemical, crystallographic, and morphological properties of PP composites were investigated by tensile
Available online 1 September 2017
and three point bending test, dynamic mechanic analysis, thermogravimetric analysis and differential
scanning calorimetry, Fourier transform infrared analysis, X-ray diffraction analysis, and scanning elec-
Keywords:
Olive pomace
tron microscopy. When 40 wt% OP filler was loaded into PP, the Young's modulus and flexural modulus of
Mechanical properties PP increased by about 62.5% and 19%, respectively. The storage modulus and thermal stability of PP were
Thermal properties remarkably enhanced with increasing OP weight fraction.
© 2017 Elsevier Ltd. All rights reserved.

1. Introduction side products can be easily utilized in polymer matrices to create

Along with the fast growing developments in polymeric mate-
rials, the need for green and sustainable materials is ever increasing
very fast [1e3]. As the new concept of “Circular Economy” states,
utilization of the products in a circular and recycling way is very
critical [4]. Moreover, the industry revolution 4.0 also strongly states
that the using of sustainable materials is very important for a better
environment [5]. The increased use of biocomposites and eco-
friendly composites is very important for the developing countries
as the agricultural products more produced bring wealth to rural
areas [6]. Biocomposites utilize many industrial agricultural fiber in
the form either reinforcement or filler in polymer materials [7e16].
Within the context of circular economy, the utilization of plant
residues and agricultural fibers play a key role for green composites
and affordable materials. From the engineering perspective, besides
creating novel materials, the production method should be also
cost effective. Circular economy tries to utilize the side product of
many industrial products in a value added application. Agricultural
wastes are generally incinerated to obtain energy. However, these
* Corresponding author.
E-mail address: metehan26mmz@gmail.com (M. Atagur).
much more wealth and eco-friendly materials [17,18].
For agricultural wastes and fibers, each country tries to utilize
the plants that grow in their land. Mediterranean area is full of olive
trees and olive plants. Olive is quite healthy and has many benefits
for the human body [19]. It is consumed in large quantities in Italy,
Greece, France, and Turkey. As people consume olive, the olive
stone is not considered as a product for polymer matrices. Espe-
cially, there are big olive oil manufacturers in Aegean region and the
olive pomace (OP) and olive stone arise in large quantities. The
farmers are trying to find suitable application areas for these OP
materials to obtain value added products.
In this study, OP powder, which was obtained from olive oil
producers, was mixed with polypropylene (PP) in order to obtain
new green composites by using melt mixing techniques. This study
aims to demonstrate that whether OP, the side products of the olive
industry, can be utilized in a novel polymer composite or not.
2. Materials and methods
2.1. Materials
The matrix material PP (MH 418) having a density of 0.90 g/cm3

http://dx.doi.org/10.1016/j.compositesb.2017.08.017
1359-8368/© 2017 Elsevier Ltd. All rights reserved.
278 N. Kaya et al. / Composites Part B 150 (2018) 277e283
and a melt flow index of 5 g/10 min was supplied from Petkim-
SOCAReTurkey. OP was obtained from Altan olive oil factory
(Saruhanlı-Manisa in Turkey). Then, OP was ground with a labo-
ratory grinder (Retsch RS 200 vibratory disc mill). Then, particles
were passed through a 100 mesh sieve (particles smaller than
0.150 mm) and dried at 70
C for 48 h to remove moisture.
2.2. Characterization OP powder sample
The particle size distribution of OP powders was analyzed by a
laser particle size analyzer (Mastersizer 2000, Malvern) in water as
a dispersant. Sonic pulse was applied to dispersant in the course of
measurement. X-ray diffraction (XRD) analysis of OP powder
sample was performed using a Panalytical Emperian model (with
CuKa radiation at 45 kV and 40 mA).
2.3. Manufacturing of composite materials
PP matrix composites at various weight fractions with 10, 20, 30,
and 40% of OP (PP-10OP, PP-20OP, PP-30OP, and PP-40OP, respec-
tively) were produced by using a laboratory type high-speed
thermo kinetic mixer. In order to produce OP filled PP compound,
a blend of OP and PP at about 70 g was processed in the mixer at
2000 rpm. The composite plates were produced by the help of
hydraulic hot and cold press at 170
C for 210 s between 40 and
120 bar pressure in hot press, then composite plates were cooled at
20
C for 120 s at 120 bar pressure in cold press.
2.4. Characterization of composite materials
Tensile tests were performed by using a universal testing ma-
chine having a 5-kN load cell (Shimadzu Autograph AG-IS, Japan).
The tensile tests of the composites were carried out according to
the ASTM D-638 standard, and the crosshead speed was selected to
be 50 mm/min. The tests were repeated at least five times for each
type of composite to check for repeatability. The flexural strength
and modulus of the composites were determined using a three-
point bending test according to the ASTM D-790 standard. The
tests were conducted with the universal testing machine using a
crosshead speed of 1 mm/min and a span length of 32 mm. The
tests were repeated at least five times. The dynamic mechanical
analysis (DMA) of PP and OP filled composites was carried out on a
Dynamic Mechanical Analyzer (TA Instruments Inc., DMA Q800).
The storage and loss moduli of PP and its composites were deter-
mined. Single cantilever was used and multi frequency-strain
modulus mode was selected to analyze all specimens between
the temperatures of 25 and 140
C in air atmosphere. Differential
Scanning Calorimetry (DSC) analysis was conducted by using dif-
ferential scanning calorimeter (TA Instrument Q2000). In order to
erase the thermal history, the samples were firstly heated to 200
C
at a heating rate of 10
C/min and held for 3 min. Then the samples
were cooled to 90
C and held for 1 min. Afterwards, the samples
were heated to 190
C at a heating rate of 10
C/min. FTIR analysis
was conducted by using Fourier Transform Infrared Spectrometer
(Thermo 50i) in attenuated total reflection (ATR) mode. FTIR
spectra, which are ranged between 4.000 and 650 cm1, were
recorded with a resolution of 4 cm1 and with an accumulation of
16 scans. Thermal stabilities of samples were investigated by
Thermogravimetric analysis (TGA) using a STA 8000 instrument
from Perkin Elmer. The samples were heated from room tempera-
ture to 600
C at a heating rate of 10
C/min under nitrogen at-
mosphere. X-ray diffraction (XRD) analysis was performed using a
Panalytical Emperian model (with CuKa radiation at 45 kV and
40 mA) to determine the characteristic peaks of the raw materials
and the crystallinity of the produced composites. The fracture
surfaces of the composites were observed using a scanning electron
microscope (SEM) (Carl Zeiss 300VP, Germany) operated at 2.5 kV.
A thin layer of gold was coated on the fractured surface of the
composites by using an automatic sputter coater (Emitech K550X)
to reduce the extent of sample arcing during SEM observation.
3. Results and discussions
3.1. Particle size analysis
Particle size distribution of OP is shown in Fig. 1. According to
Fig. 1, the particle volume distribution of OP powder sample shows
a gauss distribution. The mean size of powders is 21.36 mm (D50)
based on a volume distribution and 50% of the particles are smaller
than 21.36 mm. Besides, D10 and D90 were obtained to be 4.28 mm
and 58.47 mm, respectively. The curve also shows the presence of
some particles smaller than 1 mm and larger than 100 mm.
3.2. Tensile testing
Fig. 2 shows the effect of filler weight fraction on the tensile
properties such as tensile strength and Young's modulus of PP and
OP filled PP composites. As shown in Fig. 2, tensile strength and
Young's modulus values of PP were obtained to be 35.2 and
893 MPa, respectively. The tensile strength of PP composites con-
taining OP filler was lower than that of PP. Moreover, the tensile
strength of the composites decreased with increasing P weight
fraction up to 40%. It is observed that after incorporation of OP into
PP, tensile strength of PP decreased from 35.2 to 18.4 MPa. Fillers
having an irregular shape do not contribute to the stress transferred
to the polymer matrix. In this manner, the incorporated material
acts as a filler rather than a reinforcement [20]. The decrease in
tensile strength of composite compared to virgin polymer can be
associated with inadequate wetting of the filler with the matrix,
poor dispersion of fillers, presence of agglomerates, and poor
adhesion between the filler and matrix [21,22].
It can be also seen that the Young's modulus of the PP increases
with the addition of OP filler into PP in the studied weight fraction
range (10, 20, 30, and 40%). Shumigin et al. point out that the
Young's modulus of the filler is higher than the that of the matrix
material and this case leads to an increase in Young's modulus of PP.
Increased Young's modulus of composites can be due to the
restricted macromolecular mobility and deformability in the pres-
ence of filler particles [21]. When 40 wt% OP filler was added into
PP, the Young's modulus of PP increased by 62.5%. In general, par-
ticle fillers are more rigid compared to the polymer matrix so filler
addition causes an increase in the rigidity of the polymer matrix
Fig. 1. Particle size distribution of OP powder.
 N. Kaya et al. / Composites Part B 150 (2018) 277e283 279

Fig. 2. Tensile strength and Young's modulus of PP and OP filled PP composites.

[22]. It can be said that with increasing the weight fraction OP filler
in PP, PP become stiffer.
3.3. Three point bending test
Fig. 3 shows the effect of filler weight fraction on the flexural
strengths and moduli of PP and OP filled PP composites. As illus-
trated in Fig. 3, the flexural strength values of the composites were
lower than that of PP. Moreover, flexural strength decreased
continuously from 58.49 MPa for PP to 48.49 MPa, 39.82 MPa,
37.84 MPa, and finally to 33.93 MPa for 10, 20, 30, and 40% filler
weight fractions, respectively. In Fig. 3, it can be seen that, the
flexural modulus of OP filled PP composites enhanced with an in-
crease in filler loading. The highest flexural modulus value was
obtained to be 2160.3 MPa for PP-40P. Moreover, the flexural
modulus of the PP-40OP composite was approximately 19% higher
than that of PP. The reasons for these behaviors can be explained by
using the same reasons as previously mentioned above.
3.4. Dynamic mechanical analysis (DMA)
Viscoelastic properties of PP and OP filled PP composites were
investigated by DMA technique. Variation of storage and loss
modulus of PP and OP filled PP composites as a function of tem-
perature is shown in Fig. 4. DMA results indicate that the storage
modulus values of OP filled PP composites are higher than that of PP
at the whole temperature range. This point outs that the stiffness of
OP filled PP composites is increased with the addition of OP
particles.
The storage modulus values are also tabulated in Table 1. DMA
results show that 10, 20, 30, and 40 wt% OP fillings into PP led to
10.6%, 15.4%, 28.9%, and 54.7% increases in storage modulus,
respectively, when compared to that of PP at 30
C. The increase in
storage modulus was due to mechanical limitation posed by
increasing filler content embedded in the viscoelastic polymer
matrix. It can also be seen from Table 1 that with increasing tem-
perature, the storage modulus values of OP filled PP composites
decreased due to the softening of the matrix and initiation of the
relaxation process [23].
The retention ratio is known as the ratio of the storage modulus
at 130
C to that at 30
C. The retention ratios of PP, PP-10OP, PP-
20OP, PP-30OP, and PP-40OP were obtained to be 0.18, 0.20, 0.19,
0.21, and 0.22, respectively. It can be seen from the retention ratios
that the OP filled PP composites possess improved mechanical
properties compared to PP at high temperatures.
The variation of the loss modulus, E00 , of the PP and OP filled PP
composites against temperature are presented in Fig. 4. Loss
modulus represents energy loss as heat or molecular rearrange-
ments during the loading cycle, which indicates the viscous nature
of the polymer [24,25]. As shown in Fig. 4, the loss modulus of

Fig. 3. Flexural strength and flexural modulus of PP and OP filled PP composites.

280 N. Kaya et al. / Composites Part B 150 (2018) 277e283

Fig. 4. Storage and Loss modulus values of PP and OP filled PP composites.

Table 1 (Tc), crystallization enthalpy (DHc), melting enthalpy (DHm), and

Storage modulus values of OP filled PP composites at various temperature. the degree of super-cooling (DT), are presented in Table 2. The de-
Storage modulus 30
C 50
C 75
C 100
C 130
C gree of crystallinity (Xc) of PP composites was estimated using
equation (1) [26].
PP 1682.06 1384.82 844.69 540.50 303.38
PP-10OP 1860.77 1562.64 1003.83 653.10 379.07 
PP-20OP 1940.75 1604.92 1005.62 645.42 366.39 DHm fpp
Xc ð%Þ ¼  100 (1)
PP-30OP
PP-40OP
2168.94
2601.73
1845.06
2250.86
1203.46
1501.62
787.43
997.04
455.98
581.86
DHm0

where DH
m is the melting enthalpy of 100% crystalline PP assumed

composite with 10 wt% OP was almost close to PP at low temper-
ature. However, the loss modulus of composite with 10 wt% OP was
much higher than that of PP at high temperature. On the other
hand, the loss modulus of composites with 20, 30 and 40 wt% OP
was much higher than that of PP in the whole temperature range.
The relaxation transition peak presented in Fig. 4 represents the
transition region from the glassy state to the rubbery state [25]. a
relaxation peaks of PP, PP-10OP, PP-20OP,PP-30OP, and PP-40OP
composites were obtained to be at 66.2, 69.5, 68.2, 71.9, and
73.7
C, respectively. It can be noted a relaxation peak of PP was
increased with increasing the weight fraction of OP into PP.
to be (209 J/g) and fPP is PP weight fractions in the composite [27].
Table 2 shows that the melting temperatures of PP slightly
changed after the incorporation of OP, which indicates that the
crystal size of PP did not change considerably. Besides, OP filling
into PP improved the crystallization of PP because of the fact that
the crystallization temperature enhanced by 2e3
C. As can be seen
from Table 2, OP adding increased the degree of crystallinity of
PP by 4e8%. PP-20OP exhibited the greatest crystallinity in the
Table 2
DSC data of PP and OP filled PP composites.

Sample Tc(
C) Tm (
C) DHc(J/g) DHm(J/g) DT(
C) Xc (%)

3.5. Differential scanning calorimetry (DSC) analysis PP 116 167 94.8 74.1 51 35
PP-10OP 119 165 90.6 76.8 46 41
DSC curves of PP and OP filled PP composites are shown in Fig. 5. PP-20OP 118 166 82.9 72.1 48 43
PP-30OP 118 166 70.5 57.2 48 39
DSC melting and crystallization parameters for PP and its compos-
PP-40OP 118 164 57.8 51.3 46 41
ites such as melting temperature (Tm), crystallization temperature

Fig. 5. DSC curves of PP and OP filled PP composites.

 N. Kaya et al. / Composites Part B 150 (2018) 277e283 281

composite samples. The degree of super-cooling was decreased by
filling of OP, which can be explained by the fact that filling of OP
into PP enhanced the rate of crystallization of PP.
3.6. Thermogravimetric analysis (TGA)
TGA curves of PP and OP filled PP composites can be seen in
Fig. 6. The results obtained from TG curves for the samples are
summarized in Table 3. As can be seen from Table 3, there are two
decomposition steps in the OP filled PP composites. First one is due
to OP decomposition and the second one is due to PP decompo-
sition. From TG curves, the decomposition temperatures at 5%
mass losses for PP, PP-10OP, PP-20OP, PP-30OP, and PP-40OP were
determined to be 382, 381, 306, 308, and 282
C, respectively.
10 wt% OP filling into PP did not affect the decomposition tem-
perature of PP at 5% mass loss. However 40 wt% OP loading
decreased the temperature by 100
C. Initial and maximum
decomposition temperatures of PP were considerably increased by
filling of OP into PP. The initial and maximum decomposition
temperature of PP was obtained to be 420 and 453
C respectively.
20 wt% OP filling into PP increased the initial and maximum
decomposition temperatures to 445 and 464
C, which indicates
increases of 25 and 11
C, respectively. The residual weight values
at 600
C for PP, PP-10OP, PP-20OP, PP-30OP, and PP-40OP were
obtained to be 99.8, 95.6, 80.2, 68.2, and 58.3%, respectively. Filling
of OP into PP increased the remaining residues due to charring of
OP. It can be noted that char yield which is related with material
flame resistance was increased by OP filling into PP. This may be
due to the ring structures of cellulose and phenolic structures of
lignin having greater char yield [28,29]. From TGA analysis, it can
be claimed that the thermal stability of PP was markedly improved
by filling of OP into PP.
3.7. X-ray diffraction (XRD) analysis
The XRD pattern of OP powder is shown in Fig. 7. From the
pattern, it can be reported that OP powder sample has a charac-
teristic peak of cellulose (2q ¼ 22.5
). This residue includes amor-
phous and some crystalline phases such as quartz and calcium
carbonate.
The XRD patterns of PP and OP filled PP composites show a
number of characteristic peaks due to their crystalline structure, as
shown in Fig. 8. According to the result, PP has an isotactic poly-
propylene crystal structure. The results show that the filling of OP
into PP has some effects on the crystallinity of the PP, as seen
from Fig. 8a. The lower peak intensities for the composites as
compared to PP imply decreasing the crystallinity of the composite.
Furthermore, the lowest intensity values in PP-40OP composite is
due to presence of amorphous OP powder in the PP matrix and
reduced crystallinity of composites. It can be seen from Fig. 8 that
the peak intensity of PP at 28.5
disappeared with increasing up to
40%OP addition. The peaks at about 26.6 and 29.3
, which are due
to quartz and calcite within OP, can be seen in the diffraction
pattern of the composite samples. This proves the existence of OP
within the composites.
3.8. Fourier transform infrared (FTIR) analysis
FTIR spectra for PP and its composites are seen in Fig. 9. The peak
at 1623 cm1 in the spectra of OP was observed due to carboxyl
groups present in the components of composites [30]. Besides, the
band at 1030 cm1 in the spectrum OP probably corresponds to C-O
groups of lignin, hemicelluloses, and cellulose components in
composites [30]. As can be seen from Fig. 9, the peaks at about
1620 cm1 in the spectra of composites exhibited the availability of
OP within the composite. Additionally, one of the prominent vari-
ations in the spectra of PP and its composites is the existence of the
peaks at about 1030 cm1 in the spectra of OP filled composites. It
can be reported that the FTIR spectra of composites confirm the
presence of OP within PP matrix material.

3.9. Scanning electron microscopy (SEM) analysis

Fracture surfaces of PP containing OP are shown in Fig. 10. It can

be seen from Fig. 10 that fillers left from the matrix after the tensile

Fig. 6. TG curves of PP and OP filled PP composites.

Table 3
TGA data for PP and OP filled PP composites.

Sample Td(
C)a at 5% mass loss Ti (
C)a Tm(
C)a Mass loss (600
C) %

PP 382 420 453 99.8

PP-10OP 381 432 460 95.6
PP-20OP 306 445 464 80.2
PP-30OP 308 440 461 68.2
PP-40OP 282 439 463 58.3
a
Td: Decomposition temperature, Ti: Initial decomposition temperature, Tm:
Maximum decomposition temperature. Fig. 7. XRD pattern of OP residue powder.
282 N. Kaya et al. / Composites Part B 150 (2018) 277e283

Fig. 8. XRD patterns of PP and OP filled PP composites.

tests. Cavities were observed throughout the matrix. The result

indicated a poor interfacial bonding between OP filler and PP ma-
trix. The stress cannot be efficiently transferred from the matrix to
the fillers. Thus, tensile and flexural strengths of the composites
decreased. Orientation of PP matrix after fracture exhibited simi-
larities in the direction of matrix in PP-10OP and PP-20OP com-
posites, but matrix fracture of PP-30OP and PP-40OP composites
seems to be omnidirectional. This irregularity could be attributed to
demonstrating lower matrix strength under stress. Mechanical test
results were obtained to be in harmony with the SEM images of
composites.

4. Conclusion

The production and characterization of OP filled PP composites

Fig. 9. FTIR spectrums of P, PP and OP filled PP composites. were carried out in this study. The main conclusions obtained from
this study are as follows:

Fig. 10. SEM images of the composites. a) PP-10OP, b) PP-20OP,c) PP-30OP, d) PP-40OP.
 N. Kaya et al. / Composites Part B 150 (2018) 277e283
 Tensile and flexural strengths of the composites decreased as
the filler loading increased. However Young's modulus and
flexural modulus increased with increasing filler loading.
 The crystallinity of PP increased with increase of OP loading into
PP. The super-cooling decreased by filling of OP because of the
fact that filling of OP into PP enhanced the rate of crystallization
of PP.
 The storage modulus of PP increased with increasing OP weight
fraction in the whole temperature range. The loss modulus of
10 wt %OP was almost close to PP at low temperature. On the
other hand, the loss modulus of the composite with 10 wt% OP
was much higher than that of PP at high temperature. OP filled
PP composites possess improved mechanical properties
compared to PP at high temperatures.
 Maximum decomposition temperatures of PP were remarkably
increased by filling of OP into PP.
 This study demonstrated that that OP, the side products of the
olive industry, can be utilized as a filler material for poly-
propylene matrix material.
Acknowledgements
Financial support for this study was provided by TUBITAK-The
Scientific and TechnologicalResearch Council of Turkey, Project
Number: 214M350.
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