Industrial Crops and Products 72 (2015) 54–59

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Industrial Crops and Products

journal homepage: www.elsevier.com/locate/indcrop

Mechanical properties and water absorption of glass fibre reinforced

bio-phenolic elastomer (BPE) composite
Umar Adli Amran, Sarani Zakaria ∗ , Chin Hua Chia, Sharifah Nabihah Syed Jaafar,
Rasidi Roslan
School of Applied Physics, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia

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

Article history: In this study, bio-phenolic resin (BPR) was synthesised using liquefied oil palm empty fruit bunch (EFB)
Received 29 August 2014 fibres. Epoxidised natural rubber (ENR) was added to provide elastomeric properties and improve the
Received in revised form 27 January 2015 phenolic resin brittleness. Three different types of NR/glass fibre prepregs using SMR-L, ENR-25 and ENR-
Accepted 29 January 2015
50 were prepared and used in the fabrication of the bio-phenolic elastomer (BPE) glass composites. The
Available online 13 February 2015
composites were made by using hand lay-up technique. The ENR-50 showed the best compatibility with
the BPR. The impact strength of the composites increased as much as 77.7% with the addition of 35 wt%
Keywords:
of ENR-50. Flexural test results indicated that the BPE composites possessed elastomeric properties. The
Liquefaction
Bio-phenolic composite
ENR acted as a compatibiliser that helped in improving the wettability of the BPR on the surface of the
Compatibility glass fibres. Furthermore, approximately 47% of water absorbed by the BPE composites was reduced as
Mechanical properties the ENR-50 composition increased up to 35 wt%.
Water absorption © 2015 Elsevier B.V. All rights reserved.

1. Introduction nol, as lignin contains phenolic derivatives, such as sinapyl alcohol,

Phenolic resin is a thermosetting resin produced from the poly-
condensation of phenol and formaldehyde (Pilato, 2010). The resins
are divided into two types, novolac and resol, based on the concen-
tration of phenol to formaldehyde ratios and type of catalyst used.
For novolac resin, the formaldehyde to phenol (F/P) ratio is less
than one and the catalyst used is acidic, whereas the resol resin
is produced with F/P ratio greater than one in the presence of a
basic catalyst (Effendi et al., 2008). Phenolic resins are widely used
in many applications due to their high strength, modulus, thermal
and chemical resistance. However, phenolic resin is known to be
brittle, which limits its use in high-performance applications.
Concerns about the depletion of fossil fuels, environmental
pollutions, and fluctuations in the prices of petroleum-based
chemicals have led to numerous studies devoted to replacing phe-
nol with renewable feedstocks, such as lignocellulose biomass and
woods. Lignocellulose biomass and woods are abundantly available
throughout the world, and they can serve as a continuous supply of
raw materials. Lignocellulose material is composed of three main
compounds; cellulose, hemicellulose, and lignin. The presence of
lignin in lignocellulose materials enables it to be liquefied in phe-
∗ Corresponding author. Tel.: +60 3 8921 3261; fax: +60 3 8921 3777.
E-mail address: szakaria@ukm.edu.my (S. Zakaria).
coumaryl alcohol, coniferyl alcohol, etc (Effendi et al., 2008).
Over the last few decades, several studies have been carried
out to utilise wood and biomass as raw material in the synthe-
sis of phenolic resin via a liquefaction process (Lin et al., 1994;
Alma et al., 1998a,b; Lee et al., 2002). Liquefaction of biomass, as
well as cellulose and wood, in the presence of phenol and acid
(organic and inorganic) as catalysts, has been intensively studied
(Alma et al., 1995a,b). Most biomass liquefaction reactions are car-
ried out in the presence of an acid catalyst, which can significantly
increase the conversion yield. Liquefaction under alkaline condi-
tions indeed provides lower biomass residue content; however, it is
not an effective catalyst to achieve a high amount of combined phe-
nol (Alma et al., 1998a). During the liquefaction process,by using
organic solvent, macromolecule compounds in biomass decom-
pose into reactive small molecules via several processes, such as
dehydration, dehydrogenation, deoxygenation, and decarboxyla-
tion (Lin et al., 2001, 2004). However, these small molecules will
then re-polymerise through condensation, cyclisation, and poly-
merisation.
Investigation into the liquefaction of oil palm empty fruit bunch
(EFB) fibres with phenol in the presence of sulphuric acid has been
carried out by Ahmadzadeh et al. (2008). In their study, they found
that high liquefaction yield can be obtained with the phenol to
EFB fibre weight ratio of 3:1. The study allowed them to obtain
optimum parameters for satisfactory yield as follows: liquefaction

http://dx.doi.org/10.1016/j.indcrop.2015.01.054
0926-6690/© 2015 Elsevier B.V. All rights reserved.
 U.A. Amran et al. / Industrial Crops and Products 72 (2015) 54–59
time 60–90 min, temperature range of 130–150 ◦ C and catalyst con-
centration of 3–5%. In addition, the liquefied EFB (LEFB) was used
as a phenolic precursor to prepare novolac type resin for mould-
ing application. Meanwhile, Roslan et al. (2014) used the LEFB to
prepare resol type phenolic resin and study its physical, chemi-
cal, and mechanical properties. From the chemical analysis, they
found that LEFB at para position is more favoured for the reaction
with formaldehyde when compared to the ortho position due to
the steric effect. The plywood shear strength of the resol resin is
also in compliance with the JIS K-6852 standard.
Epoxidised natural rubber (ENR) is a chemically modified nat-
ural rubber which has epoxide groups grafted onto its polymeric
chains by the epoxidation process (Ruamcharoen et al., 2011).
These epoxides make ENR susceptible to various chemical reactions
that involve hydrogen-donor molecules, such as alcohols, car-
boxylic acids, and amines (Phinyocheep et al., 2005). Commercially,
there are two types of ENR, ENR-25 and ENR-50. The designated
integers represent the mole percentage (%) epoxidation of the
natural rubber. Miscibility of blends or compounds is attributed
by molecular interactions, for example a donor–acceptor type of
weakly acidic hydrogen or dipole–dipole interaction. Theoretically,
ENR should be compatible with proton-donating polymers, such as
phenolic resin (Kallitsis and Kalfoglou, 1989).
Phenolic resin requires a toughening mechanism to improve its
brittleness. An example of a phenolic resin toughening mechanism
is the incorporation of rubber. The most common rubber used is
nitrile rubber due to its compatibility (Kaynak and Cagatay, 2006).
It is expected that the introduction of ENR will provide elastomeric
properties and improve the impact resistance of the phenolic com-
posites. However, little literature has reported on the topic of the
utilisation of natural rubber as toughening agent in phenolic com-
posites. Hence, the aim of this study is to investigate the mechanical
properties and water absorption of ENR-toughened glass fibre rein-
forced bio-phenolic resin composites, which are referred to as
bio-phenolic elastomer (BPE) composites.
2. Experimental
2.1. Materials
Oil palm EFB fibres and E-glass fibres (woven and non-woven)
were supplied by Szetech Engineering Sdn. Bhd and RTG Intech
Sdn. Bhd., respectively. Natural rubbers with three different grades,
SMR-L (Standard Malaysian Rubber Light), ENR-25 and ENR-50,
were purchased from the Malaysian Rubber Board. The rubber
grades represent 0%, 25% and 50% mole epoxidation, respectively.
SMR-L (0% epoxidation) is a natural rubber before epoxidation was
used as a control to study the effect of rubber epoxidation. Industrial
grade phenol (98%) was supplied by Chemzone Sdn. Bhd. Ana-
lytical grade sulphuric acid (98%), formalin (37% formaldehyde),
sodium hydroxide (NaOH), methanol and toluene were procured
from Sigma–Aldrich.
2.2. Liquefaction of EFB fibres
Liquefaction of the EFB fibres was performed according to pro-
cedures reported upon in the previous studies (Ahmadzadeh et al.,
2009 Zakaria et al., 2014) with slight modification. First, the EFB
fibres were dried in an oven at 105 ◦ C for 24 h. The weight ratio of
phenol to EFB fibres (P/EFB) of 3:1 and sulphuric acid (3% based on
the phenol weight) were used in the liquefaction reaction. Lique-
faction was carried out in an oil bath at a temperature of 150 ◦ C
for 90 min. Black and viscous liquid was produced at the end of
the reaction. This liquid was then diluted with 400 ml methanol.
The mixture of black liquid and methanol was filtered with filter
55
paper (Whattman no. 1) to remove the residues. Later, the methanol
added was evaporated from the mixture by using a rotary evapo-
rator to obtain liquefied EFB (LEFB).
2.3. Resinification process
A resinification reaction was carried out by reacting forma-
lin with the LEFB to prepare BPR. The LEFB was reacted with
formalin (37% formaldehyde solution) as the crosslinking agent
with the formalin/LEFB weight ratio of 1.2 in an alkaline medium.
Sodium hydroxide (40 wt%) aqueous solution, used to obtain alka-
line medium, was added in two-steps process. During the first
60 min of the reaction, 5 wt% (based on LEFB weight) of NaOH solu-
tion was added, and the reaction temperature was set at 65 ◦ C.
Following this, the reaction temperature was increased to 85 ◦ C and
20 wt% (based on LEFB weight) of NaOH solution was added, where
it was held for another 60 min. All of the reactions were conducted
in a reflux system.
2.4. Preparation of natural rubber (NR) and epoxidised natural
rubber (ENR) solutions
Ten grams of natural rubber (SMR-L) and epoxidised natural
rubber (ENR-25 and ENR-50) were dissolved in 100 ml of toluene,
separately, to produce rubber solutions with 10% solid rubber con-
tent. The process was conducted in a 1000 ml round bottom flask
attached to a reflux condenser system equipped with an overhead
stirrer to stir the mixture. The process was carried out at 80 ◦ C for
6 h in an oil bath.
2.5. Preparation of rubber/glass fibre prepregs
To study the effects of the natural rubber degree of epoxida-
tion on the properties of the composite, three prepregs with 5 wt%
(from the weight of the woven glass fibres) of each SMR-L, ENR-25
and ENR-35 were prepared. An additional three prepregs with 15,
25 and 35 wt% (from the weight of woven glass fibres) of ENR-50
were prepared to study the effect of different rubber compositions
on the composite properties. The rubber solution was applied on
both sides of the woven glass fibres. During the application of the
rubber solution, care was taken to match the exact required weight
and thickness on each side of the prepregs to maintain a balanced
composite design. Later, the rubber-coated glass fibres were dried
in an oven at 60 ◦ C overnight to remove toluene. The thickness of
the prepreg was measured and controlled by using an electronic
micrometre.
2.6. Preparation of bio-phenolic elastomer (BPE) composites
Composite boards were prepared by using a hand lay-up tech-
nique, followed by compression moulding. Total glass fibre loading
Fig. 1. Lay-up arrangement.
56 U.A. Amran et al. / Industrial Crops and Products 72 (2015) 54–59
Table 1
Effects of natural rubber types on the mechanical properties of BPE composites.
Types of rubber Impact strength
(kJ/m2 ) (±SD)
Ref. 72.40 ± 2.12
SMR-L 56.01 ± 4.06
ENR-25 71.59 ± 3.59
ENR-50 74.04 ± 2.64
used was 40 wt% of total composite weight. The other 60 wt% com-
prised the total weight of resin and rubber solid content used. Each
composite consisted of five layers of GF mats and two layers of
NR/GF prepregs, as shown in Fig. 1. These lay-ups were kept in an
oven at 60 ◦ C for 14 h to reach semi-cure stage. The semi-cured
lay-ups were then hot-pressed at 105 ◦ C for 15 min in a rectangle
mould with a dimension of 150 mm × 150 mm × 3 mm. The sam-
ples with 5% SMR-L, 5% ENR-25, and 5% ENR-50 were later referred
to as composites SMR-L, ENR-25 and ENR-50, respectively. The
same arrangement of composite without NR was fabricated as a
reference sample and labelled as “Ref.”.
2.7. Mechanical tests
Izod impact and flexural tests were carried out in accordance
with ASTM D256 and D790, respectively. The impact test was
performed on an Instron CEAST 9050 machine using notched spec-
imens (notch depth: 2.5 mm) with an impact speed of 3.46 m/s
and incident energy of 5.0 J. For the flexural test, three-point bend-
ing with a nominal specimen dimension of 90 mm × 13 mm × 3 mm
was carried out by using a Universal Testing Machine (Testomet-
ric M500-50CT). The span between supports was 50.0 mm and the
crosshead speed was 10 mm/min. Each value obtained represents
the average of five specimens.
2.8. Morphological analysis
The morphological structure of the BPE composites was inves-
tigated by using a scanning electron microscope (SEM Supra 55 VP
Zeiss) to observe the fractography of the surface of the BPE com-
posites and the interaction between glass fibres, ENR, and BPR. The
impacted specimens were cut cross-sectionally at the notched parts
using a sample cutter and coated with a thin gold layer prior to SEM
analysis.
2.9. Water absorption
Composite specimens with a dimension of 15 mm × 15 mm ×
3 mm were used for the water absorption test. The specimens were
then immersed in distilled water at a temperature of 25 ◦ C. Period-
Fig. 2. Scheme of probable crosslinking between BPR and ENR.
Flexural strength Flexural modulus
(MPa) (±SD) (MPa) (±SD)
50.87 ± 1.59 6212.30 ± 325.97
21.32 ± 1.13 1259.28 ± 58.70
21.69 ± 1.59 2949.03 ± 402.62
22.55 ± 1.07 1475.24 ± 126.19
ically, the specimens were taken out and wiped with absorbent
paper to remove the water on the specimen surfaces and then
reweighed. The water absorptions of the samples were calculated
by using Eq. (1):
W2 − W1
Water absorption(%) = × 100 (1)
W1
where W1 is the initial weight of the sample before the immersion
(g) and W2 is the weight of the sample after the immersion (g).
3. Results and discussion
3.1. Effects of types of natural rubber
Table 1 demonstrates the effects of natural rubber types (SMR-
L, ENR-25, and ENR-50) on the mechanical properties of the BPE
composites. In this case, the rubber composition was fixed at 5 wt%
based on the weight of woven glass fibres. From the result, the
impact strength of the Ref. sample is 72.40 kJ/m2 . After 5 wt%
of SMR-L loaded, the impact strength of the SMR-L composite
decreased to 56.01 kJ/m2 . This phenomenon occurred due to the
incompatibility between the resin (polar material) and SMR-L nat-
ural rubber (non-polar materials). Similar results were observed
in a study conducted by Thongnuanchan et al. (2007), when NR
latex adhesives used as a binder for particleboards demonstrated
that a transetherification reaction of methoxymethyl groups from
hexamethoxymethylmelamine did not occur in the non-polar
NR system. After the introduction of ENR-25 and ENR-50, the
impact strength of the composites increased to 71.59 kJ/m2 and
74.04 kJ/m2 , respectively. Although the results have no significant
effect if compared to the Ref. sample due to the large standard devi-
ation, they show that the presence of the epoxides group allows the
reaction between OH from the BPR and the ENR to take place. Again,
this result is in a strong agreement with the previous finding in the
literature on ENR-based adhesives (Thongnuanchan et al., 2007).
Phenolic resin consists of an aromatic ring and two ortho- and para-
positions for reactions in every phenol molecule. Besides, abun-
dance of OH groups in BPR is capable to crosslink with the oxirane
ring of the ENR molecules. Fig. 2 shows the scheme of probable
crosslinking mechanism between BPR and ENR.
 U.A. Amran et al. / Industrial Crops and Products 72 (2015) 54–59
Fig. 3. Fractographs of composites with different types of NR (a) Ref. (b) SMR-L (c) ENR-25 and (d) ENR-50.
Composites at different amounts (15%, 25%, and 35%) of SMR-L,
ENR-25 and ENR-50 were prepared to study the effects of different
rubber compositions. Unfortunately, as the composition of SMR-
L and ENR-25 increase, delamination occurs before the composite
specimens are tested (there is no result shown). Delamination hap-
pens as SMR-L and ENR-25 show incompatibility with the resin
as their compositions increase. Thus, both rubbers are not suit-
able to be used in the prepreg application. Nevertheless, ENR-50
showed strong compatibility with resin and formed rigid samples
as its composition increased. The effects of ENR-50 composition are
discussed in Section 3.2.
SEM fractographs of composites with different types of natural
rubber are shown in Fig. 3. For the Ref. sample in Fig. 3(a), it is
observed that there is no BPR wetted on the glass fibre surface.
Fig. 3(b) shows that the SMR-L remains on the glass fibre surface,
but the resin does not attach to the rubber after impact force is
applied. This is due to the incompatibility between SMR-L and BPR.
It is noted that, the resin begins to wet the ENR-25 and ENR-50, as
shown in Fig. 3(c) and (d), respectively. The compatibility between
rubber and resin is solely dependent on the epoxides present in the
ENR. As the mole % of epoxidation increases, the ability of the resin
to wet the glass fibre prepreg also increases.
Table 1 shows the flexural strength and modulus of the BPE com-
posites produced with different types of rubber. From the results,
Table 2
Effects of ENR-50 compositions on the mechanical properties of BPE composites.
ENR-50 composition (%) Impact strength
(kJ/m2 ) (±SD)
Ref. 72.40 ± 2.12
5 74.04 ± 2.64
15 96.51 ± 1.72
25 114.27 ± 2.95
35 128.65 ± 5.07
57
all BPE composites show reduction in both flexural strength and
modulus in comparison with the Ref. sample. Flexural strength
indicates an ability of a material to resist deformation under bend-
ing force whereas the modulus is heavily dependent on the ratio
of stress over strain of that material. Elastomers possess elastic-
ity that enables them to absorb forces while deforming. The results
indicate that the BPE composites have turned out to be less rigid. As
the composition of the rubber is constant, the flexural strength does
not differ much. Nonetheless, there is a slight difference in modu-
lus of the ENR-25 sample. Chemical and physical properties of the
ENR change depending on the extent of the mole % of epoxidation.
Flexural strength of ENR is decreased as the mole % of epoxidation
increases (Baker et al., 1985).
3.2. Effects of rubber composition
Table 2 shows the effects of the ENR-50 compositions on the
mechanical properties of BPE composites. From the table, it can be
seen that the impact strength of the BPE composite increases from
72.40 kJ/m2 to 128.65 kJ/m2 with the addition of 35 wt% of ENR-50.
A significant increment on the impact strength can be observed at
15 wt% of ENR-50. The increase in the ENR-50 composition allowed
more impact force to be absorbed through stress distribution by
rubber particles present in the composite. In addition, more epox-
Flexural strength Flexural modulus
(MPa) (±SD) (MPa) (±SD)
50.87 ± 1.59 6212.30 ± 325.97
22.55 ± 1.07 1475.24 ± 126.19
29.59 ± 1.11 1555.13 ± 98.11
25.65 ± 0.82 1235.12 ± 111.57
24.64 ± 1.15 1386.36 ± 110.07
58 U.A. Amran et al. / Industrial Crops and Products 72 (2015) 54–59
Fig. 4. Fractographs of composites with different composition of ENR-50 (a) Ref (b) 5 wt% (c) 15 wt% (d) 25 wt% and (e) 35 wt%.
ides exist in the composites when the rubber composition increases
which allows for greater interaction between the ENR-50 and BPR,
resulting in greater rubber-resin compatibility.
Fractographs in Fig. 4 portray the condition of the BPE compos-
ites at different ENR-50 compositions after being impacted. From
the images, it can be clearly seen that more resin wets the surface
of the glass fibre as the ENR-50 composition increases. This has
proven that the ENR-50 has acted as a compatibiliser between the
glass fibre and BPR. Furthermore, higher amounts of ENR-50 cause
more rubber particles to squeezed into the voids formed through
solvent evaporation during hotpressing, thereby, reducing the for-
mation of voids. Lesser void content in the composites improves
their impact strength.
Flexural strength and modulus of the BPE composites at
different compositions of ENR-50 are shown in Table 2. The flex-
ural strength and modulus of all BPE composites samples are
decreased when compared to Ref. sample when the ENR compo-
sition increases. The elasticity and resilient properties of rubber
have altered the overall composite rigidity and provide an elas-
tomeric property. This leads to a reduction in the composites’
flexural strength and modulus. There is no pattern or significant dif-
ference in flexural properties of the composites associated with the
addition of different amounts of ENR because they are anisotropic
material. So, the flexural load applied to the samples is unequal
at different axes where it is measured. However, the results show
that 15% ENR composition possesses the highest flexural strength
and modulus, which is 29.59 MPa and 1555.13 MPa, respectively. It
may be at this point that the amount of rubber affords the highest
rigidity and optimum compatibility for the ENR-50 BPE composites.
3.3. Water absorption test
Fig. 5 presents the water absorption of BPE composites at
different ENR-50 compositions. Curing of phenolic resin leaves
microvoids that contribute to the sites for water absorption in
composite material. Absorbed water trapped in a composite body
may deter its performance for a period of time. It is very crucial to
reduce the water intake of the composite to prevent this problem
from occuring. In the Ref. composite sample, total water uptake is
11.25%. The water absorption by the BPE composites decreases as
the ENR-50 composition increases. At 35 wt% of ENR-50, the total
water absorbed by the composite sample is 5.95%. Approximately
 U.A. Amran et al. / Industrial Crops and Products 72 (2015) 54–59
Fig. 5. Water absorption of composites with different composition of ENR-50.
47% water uptake has been reduced by the addition of 35 wt% of
ENR-50, when compared to the Ref. sample. This happen as many
microvoids are lost due to the formation of a compact composite
structure and the ENR-50 prepregs have also protected some areas
from allowing water to diffuse in the composite sample.
4. Conclusions
In this study, BPE composites were prepared by using BPR with
the incorporation of natural rubber and different types of epox-
idised natural rubber (ENR) prepregs. ENR was added to provide
an elastomeric property to the brittle thermosetting resin. The
results demonstrated that the addition of SMR-L into the com-
posite decreased its impact strength due to the incompatibility
between the rubber and the resin. However, after the introduc-
tion of ENR-25 and ENR-50, the impact strength of the composites
was increased. In addition, investigation into the effects of different
ENR-50 compositions showed similar results as the impact strength
increased from 72.40 kJ/m2 to 128.65 kJ/m2 . These findings proved
that the epoxides group in the ENR backbone can provide com-
patibility by allowing the rubber-resin interaction. This was also
supported by the results obtained via SEM images. Flexural prop-
erties of the BPE composites were found to be decreased when
rubber was introduced. This indicated that the fabricated com-
posites possessed elastomeric properties. Meanwhile, the water
absorption test showed that the addition of ENR has a great effect
in reducing the total percentage of water absorbed by the BPE
composites.
59
Acknowledgements
We acknowledge the financial support from research grants
PHI-2013-001, UKM-ST-07-FRGS0232-2012 and UKM-DIP-2014-
013.
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