ARTICLE IN PRESS

POLYMER
TESTING
Polymer Testing 26 (2007) 779–787
www.elsevier.com/locate/polytest

Material Properties

Polypropylene-based blends containing waste tire dust: Effects

of trans-polyoctylene rubber (TOR) and dynamic vulcanization
M. Awang, H. Ismail, M.A. Hazizan
School of Materials and Mineral Resources Engineering, Universiti Sains Malaysia, Nibong Tebal, 14300 Penang, Malaysia
Received 26 January 2007; accepted 10 April 2007

Abstract

Blends of polypropylene/waste tire dust (PP/WTD) with and without trans-polyoctylene rubber (TOR) and dynamic
vulcanization were prepared, and the effects of TOR and dynamic vulcanization were investigated. By using WTD of
500–710 mm, five different compositions of PP/WTD blend (i.e. 80/20, 70/30, 60/40, 50/50 and 40/60 wt%) were prepared in
an internal mixer at 180 1C and 50 rpm rotor speed. The results indicate that the incorporation of TOR and dynamic
vulcanization improved the tensile properties of PP/WTD blends. Chemical and oil resistance of the PP/WTD blends with
TOR and dynamic vulcanization was enhanced. Scanning electron microscopy of the fractured surfaces proved that TOR
and dynamic vulcanization promoted good adhesion between the PP matrix and WTD. Thermograms support the finding
that TOR and dynamic vulcanization improved the interaction of PP and WTD and, hence, their compatibility.
r 2007 Elsevier Ltd. All rights reserved.

Keywords: Polypropylene; Trans-polyoctylene rubber; Waste tire dust; Dynamic vulcanization; Blend

1. Introduction between polymers and so forth [6,7]. One of the

Polymer modifications have been carried out in
many ways [1–3] resulting in various properties
depending on factors such as the blend composition,
processing conditions, additives and the temperature
of application. Perhaps this versatility and other
advantages have contributed to 57% of engineering
resins being blended [4] and the fact that polymer
blends constitute more than 30% of overall polymer
consumption [5]. However, a number of setbacks were
reported in polymer modification attempts due to
several constraints, such as diminution of mechanical
properties, lack of thermodynamic compatibility
Corresponding author.
E-mail address: hanafi@eng.usm.my (H. Ismail).
options is to incorporate a suitable third polymeric
component to minimize the constraints [8,9].
Trans-polyoctylene rubber (TOR) is a low-mole-
cular-weight polymer, made from cyclo-octene by
metathesis polymerization, and has been known as a
compatibilizer for incompatible blends as well as a
processing aid. It can provide good processability in
the temperature range of rubber processing
(100–150 1C) as well as good collapse resistance
below the melting temperature, 54 1C, due to re-
crystallization [10]. It has linear and cyclic macro-
molecules which are un-branched and contain one
double bond for every eight carbon atom with
prevalently trans isomeric double bonds [11].
Polypropylene (PP)-based materials are known to
attract attention due to their low cost, processability

0142-9418/$ - see front matter r 2007 Elsevier Ltd. All rights reserved.
doi:10.1016/j.polymertesting.2007.04.007
 ARTICLE IN PRESS
780 M. Awang et al. / Polymer Testing 26 (2007) 779–787

and good balance of properties [12]. One of the Table 1

possibilities is to blend it with abundant waste Characteristics of materials
rubber, and it has attracted a number of researchers Material Description Source
to investigate the properties it has to offer [2,13,14].
Recently, the authors [3] highlighted the effects of Polypropylene (PP) TitanPro 6331 Titan PP Polymers,
Homopolymer Malaysia
waste tire dust (WTD) size and partial replacement MFR at
of PP by WTD on the properties of PP/WTD 230 1C ¼ 14 g/
blends. A number of works have also been reported 10 min

by several researchers on TOR [11,15]. However, no Waste tire dust (WTD) Size: 500–710 mm Mega Makmur
attempt has been made to investigate the effects of Saintifik, Malaysia

TOR and dynamic vulcanization on the properties Trans-polyoctylene rubber Vestenamer 8012 Huls, Germany
of PP/WTD blends. (TOR) ML1+4 at
100 1Co10
In this work, TOR acting as a processing aid and MW ¼ 100,000
a rubber component itself was incorporated into Tm ¼ 51 1C,
PP/WTD blends with the presence of a conventional Tg ¼ 65 1C
Crystallinity at
vulcanization agent, sulfur. The variations of tensile 23 1C ¼ 27%
properties, oil and chemical resistance, morphology
Sulfur, zinc oxide, stearic acid Bayer, Malaysia
and thermal properties are reported and discussed. and CBS
(N-cyclohexyl-2-
2. Experimental benzothiazole-2-sulfenamide)

2.1. Materials and preparation of blend

Table 2
The materials used in this study were PP Summary of mixing sequence
homopolymer, WTD—a recycled product from Time Blends and operation
mechanically ground scrap tires, TOR, sulfur, zinc (min)
oxide, stearic acid and N-cyclohexyl-2-benzothia- PP/WTD without TOR and PP/WTD with TOR and
dynamic vulcanization dynamic vulcanization
zole-2-sulfenamide (CBS). Their characteristics are
illustrated in Table 1. 0 Addition of PP Addition of PP
The PP/WTD blends were formulated based on 2 Addition of WTD Addition of WTD
6 Addition of TORa
80/20, 70/30, 60/40, 50/50 and 40/60 (wt%). The 8 Addition of curativesb
amounts of sulfur, zinc oxide, stearic acid and CBS 9 Remove
were varied accordingly so that all blend composi- 10 Addition of vulcanization
agentc
tions have the same concentration of vulcanization 13 Remove
agent and curatives. The blends were melt-mixed in
a
an internal mixer (Haake Polydrive R600/610) at a TOR (10 phr).
b
Zinc oxide (5 phr), stearic acid (1.5 phr), CBS (1 phr).
temperature of 180 1C and rotor speed of 50 rpm. c
Sulfur (2 phr).
The mixing sequence for blends with and without
TOR and dynamic vulcanization is enumerated in
Table 2. For both systems, PP was melted in the moving platens of an electrically heated hydraulic
mixer for 2 min prior to the addition of WTD. For press to produce a 2 mm sheet. The blends were
the system without TOR and dynamic vulcaniza- preheated for 6 min and compression-molded for
tion, the mixing was continued for another 7 min. In 4 min at 180 1C. The blends were subsequently cooled
the case of the system with TOR and dynamic under running tap water and pressure for 2 min at
vulcanization, additions of TOR, curatives and ambient temperature. Then, dumb-bell-shaped test
vulcanization agent were done at 6 min, 8 min and specimens were punched from the sheets.
10 min, respectively, and the process was considered
complete after a total time of 13 min. Then, the 2.2. Measurement of properties
blends were left to cool down at ambient tempera-
ture prior to molding. Tensile properties were determined using a tensile
About 36 g of PP/WTD blends were placed in a tester (Instron 3366) according to ISO 37. The tests
mold and pressed between smooth sheets and the were performed at a temperature of 2573 1C and

M. Awang et al. / Polymer Testing 26 (2007) 779–787
the specimens were pulled at a constant cross-head
speed of 50 mm/min with the gauge length kept at
50 mm. A minimum of three readings of tensile
strength, elongation at break (Eb) and Young’s
modulus were used to determine the mean values.
The modulus represents stress divided by the
corresponding strain within the proportional limit
of the specimens.
Swelling tests were conducted in accordance with
ISO 1817. The initial weight, W1 was determined
from specimens with dimensions 30 mm  5 mm 
2 mm. Then, the specimens were immersed in IRM
903 oil at ambient temperature for 70 h to reach
equilibrium state. Then, they were taken out and the
adhered oil was immediately removed by blotting
with tissue. The specimens were weighed to deter-
mine the swollen weight, W2. The swelling index was
calculated according to Eq. (1). The same procedure
was applied for swelling test in toluene at ambient
temperature for 46 h.
W2
Swelling index ¼ . (1)
W1
2.3. Morphological observation
Phase morphology of tensile fracture surfaces was
investigated using a scanning electron microscope
(SEM-Leica Cambridge S360). The fractured ends
of the specimens were coated with a thin gold layer
to avoid electrostatic charging.
2.4. Thermal analysis
Thermal analysis of the PP/WTD blends was
performed using a Perkin–Elmer differential scan-
19
17
Tensile Strength (MPa)
15
13
11
5
80/20
Fig. 1. Tensile strength vs. blend composition for the PP/WTD blends.
ARTICLE IN PRESS
781
ning calorimeter (DSC) 6 in nitrogen atmosphere at
a scan rate of 20 1C/min, and a Pyris 6 thermo-
gravimetric analyser at a temperature between 30
and 600 1C, nitrogen airflow of 50 ml/min and a
heating rate of 20 1C/min. The samples were heated
up to 220 1C at the rate mentioned and held for
5 min to eliminate the influence of thermal and
mechanical history. The samples were then crystal-
lized from 220 to 30 1C at the same rate. The melting
temperature (Tm) was determined during the second
non-isothermal heating to 220 1C.
3. Results and discussion
Figs. 1 and 2 show the variations of tensile
strength and modulus of PP/WTD blends with and
without TOR and dynamic vulcanization as a
function of blend composition. An obvious diminu-
tion of both properties is observed as WTD content
increases. This is expected as WTD was poorly
distributed in WTD-rich blends as compared to that
in PP-rich blends. This, in turn promotes high
particle–particle interaction with increasing WTD
content, which at the end contributes to the
reduction in tensile properties. A similar trend was
observed in blends using PP and recycled rubber [2].
As depicted in the figures, incorporation of TOR
and dynamic vulcanization enhanced both tensile
strength and modulus of most PP/WTD blends. The
tensile strength improvement is evident as the WTD
content increases. This observation may be attrib-
uted to a better distribution of WTD in the PP
matrix with the presence of TOR, which acts as a
processing aid, as well as the formation of crosslinks
throughout the PP/WTD blends as a result of
PP/WTD
PP/WTD+TOR+ Dyn. Vulc.
70/30 60/40 50/50 40/60
Composition of PP/WTD (wt %)
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782 M. Awang et al. / Polymer Testing 26 (2007) 779–787

750 PP/WTD
PP/WTD+TOR+Dyn. Vulc.

Young's Modulus (MPa)

650

550

450

350

250

150
80/20 70/30 60/40 50/50 40/60
Composition of PP/WTD (wt %)

Fig. 2. Plots of Young’s modulus and blend composition for the PP/WTD blends.

30
PP/WTD
Elongation at Break, Eb (%)

PP/WTD+TOR+Dyn. Vulc.
25

20

15

10

5
80/20 70/30 60/40 50/50 40/60
Composition of PP/WTD (wt %)

Fig. 3. The relationship between elongation at break, Eb, and blend composition of the PP/WTD blends.

dynamic vulcanization. Being a polymer with low crosslinked WTD [18] coupled with other WTD
viscosity, TOR may also locate at the interfacial contents such as carbon black, zinc oxide and other
area of the PP phase and WTD during the mixing additives, which hinder the flow and mobility of the
process. Previous works revealed that TOR is PP/WTD blends. Carbon black, for example, can
located at the interface of the polymers with higher restrict molecular orientation and mobility of
viscosity [16] and PP/EPDM/NR ternary blends polymer blend molecules [19]. With addition of
[17]. Having some unsaturated chains, TOR is TOR and dynamic vulcanization, all blend compo-
anticipated to participate in dynamic vulcanization sitions exhibit better Eb than the blends without
to become a part of the network structure. The TOR and dynamic vulcanization. This observation
ability of PP/WTD blends with TOR and dynamic was attributed to the formation of interfacial
vulcanization as compared to that of blends without adhesion between PP and WTD as a result of the
TOR and dynamic vulcanization to resist oil and ability of TOR to locate at the interfacial area of the
chemicals, which is elucidated later, confirmed the PP phase and WTD and, hence, co-vulcanizes with
formation of crosslinks in the blends. the elastomer component during the mixing process.
The relationship between elongation at break, Eb, This may promote the formation of interfacial
and blend compositions is shown in Fig. 3. bonding. This is an agreement with the morphology
Generally, Eb increases with increasing WTD of fracture surfaces which shows better encapsula-
content, which is due to the increasing content of tion of WTD and less removal of WTD from the PP
elastomer. However, the Eb of the PP/WTD blends matrix with incorporation of TOR and dynamic
are quite low (o30%) due to the presence of the vulcanization.
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M. Awang et al. / Polymer Testing 26 (2007) 779–787 783

Toluene
2.0
PP/WTD
Swelling Index 1.8
PP/WTD+TOR+Dyn. Vulc.

1.6

1.4

1.2
80/20 70/30 60/40 50/50 40/60

Composition of PP/WTD (wt%)

Fig. 4. Variations of swelling index and blend composition in toluene for 46 h.

Oil: IRM 903

1.30
PP/WTD
1.25 PP/WTD+TOR+Dyn. Vulc.
Swelling Index

1.20

1.15

1.10

1.05

1.00
80/20 70/30 60/40 50/50 40/60

Composition of PP/WTD (wt%)

Fig. 5. Swelling index vs. blend composition in ASTM Oil No. 3 for 70 h.

Figs. 4 and 5 compare the degree of swelling of
blends with and without TOR and dynamic
vulcanization in toluene and oil. The swelling index
is one of the indicators for the degree of cross-
linking. The swelling index increases as the WTD
content increases, which is accounted for by the
increase of elastomer content in the blends. The
ability of blends with TOR and dynamic vulcaniza-
tion is apparent in inhibiting oil and chemical
penetration as compared to blends without TOR
and dynamic vulcanization. This improvement in
resisting oil and chemical penetration into the
blends can be related to the formation of crosslinks
and an increase in crosslink density, as well as
interfacial bonding between PP and WTD as a
result of addition of TOR and dynamic vulcaniza-
tion. The participation of TOR in the vulcanization
process was reported to lead to the variation of the
cure rate and crosslink density [20].
Fig. 6(a)–(c) depicts micrographs of the tensile
fracture surfaces of 80/20, 60/40 and 40/60 PP/
WTD blends, respectively. It can be seen that at
every blend composition, fewer WTD particles were
removed from the matrix in blends with TOR and
dynamic vulcanization than in blends without TOR
and dynamic vulcanization. WTD in the blends with
TOR and dynamic vulcanization was smoothly
covered as shown in Fig. 6(iii), which supports the
notion that TOR tends to help encapsulate the
polymer with higher viscosity during the mixing
process. The introduction of TOR into various
polymer blends is reported to reduce the scale of the
phase morphology, leading to an improvement in
mechanical properties [16,21]. Hence, the above
observation strongly supports the earlier finding
that the addition of TOR and dynamic vulcaniza-
tion in PP/WTD blends helps to create the
interfacial area between the PP phase and WTD,
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784 M. Awang et al. / Polymer Testing 26 (2007) 779–787

Fig. 6. SEM micrographs of the PP/WTD blend (a) without and (b) with TOR and dynamic vulcanization at magnification of 60  :
(i) 80/20, (ii) 60/40 and (iii) 40/60.

and co-vulcanizes with the elastomer component
during the mixing process, which in the end
increases crosslink density and reduces the inter-
facial tension between PP and WTD.
Fig. 7 shows the melting behavior of PP/WTD
blends with and without TOR and dynamic
vulcanization. From the plot, there is very slight
difference in the melting temperature of both
blends. This indicates that the addition of TOR
and dynamic vulcanization did not significantly
interfere with the crystal growth in PP/WTD. It is
reported that rubber particles are present in the
inter and intra-spherulitic region of the crystalline
plastic and have some degree of effect on the
crystallinity and the melting temperature of blends
[22].
Thermograms and derivative thermograms of PP/
WTD blends, with and without TOR and dynamic
vulcanization, are shown in Fig. 8. It can be seen
that there is a slight difference between both blends.
The weight loss for both blends is very low up to
250 1C. Therefore, both blends are considered stable
up to 250 1C in a nitrogen atmosphere. The
degradation of PP/WTD blend, with and without
TOR and dynamic vulcanization, was completed at
about 510 and 500 1C, respectively. The weight loss
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M. Awang et al. / Polymer Testing 26 (2007) 779–787 785

PP/WTD (60/40)
PP/WTD (60/40) + TOR + Dyn. Vulc.

Heat Flow, mW (Endo Up)

114 127 134 140 147 154 160 167

Temperature,° C

Fig. 7. DSC thermograms of PP/WTD without and with TOR and dynamic vulcanization.

a
110
100
90
80
PP/WTD-6040
PP/WTD-6040+TOR+Dyn. vulc.
70
Weight (%)

60
50
40
30
20
10
0
0 100 200 300 400 500 600
Temp (°C)

b
5

0 100 200 300 400 500 600

Derivative Weight % (%/min)

-5

-15

-25
PP/WTD-6040
PP/WTD-6040+TOR+Dyn. vulc.

-35
Temp (°C)

Fig. 8. (a) Thermograms and (b) derivative thermograms of the PP/WTD (60/40) blends.
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786 M. Awang et al. / Polymer Testing 26 (2007) 779–787

cyclic linear

b (CH ) (CH )

s CH CH s
s CH CH s
s s
s
s sx
s

TOR
WTD chain breakdown I
Sulfur+curatives
+ +
s
s sx s
s CH
s CH s CH
(CH ) CH
s CH s CH
s (CH )
(CH )

WTD crosslink bond breakage II

Fig. 9. (a) Structure of TOR and (b) the proposed reaction mechanism between WTD and TOR with the presence of vulcanization agents.

between 250 and 510 1C represents the occurrence of
random chain scission and intermolecular transfer,
which leads to the formation of volatile products
[23]. Fig. 8(b) depicts the degradation of PP/WTD
blends without TOR and dynamic vulcanization,
which occurs in two steps. With addition of TOR
and dynamic vulcanization, the step was smoother
which indicates better interaction between PP and
WTD. This improvement in compatibility between
PP and WTD after addition of TOR and dynamic
vulcanization is in agreement with the morphology
observation and the trend in tensile properties.
Figs. 9(a) and (b) depict the structure of TOR and
the proposed reaction mechanism of TOR with
WTD with the presence of sulfur during dynamic
vulcanization. WTD obtained from mechanical
grinding of scrap tires may contain some degree of
polymer chain breakdown and crosslink bond
breakage [24]. When TOR was added to PP/WTD
blends, TOR tends to encapsulate the polymer
radicals due to its low viscosity compared to that of
PP and WTD. With the presence of curatives and
vulcanization agents during dynamic vulcanization,
broken polymer radicals combined with TOR
through its unsaturated chains to create crosslinks
at the interface as well as entanglements of the
polymer chain and, hence, reduced interfacial
tension between WTD and PP.
4. Conclusions
TOR and dynamic vulcanization improved the
tensile properties of PP/WTD blends as a result of
an increase in crosslink density and the ability of
TOR to locate at the interfacial area of PP phase
and WTD and, consequently, co-vulcanize with the
elastomer component in the presence of a curing
agent. This reaction improved the interfacial adhe-
sion between PP and WTD. The formation of a
better interfacial adhesion between PP and WTD
also accounts for the improvement of the blends in
inhibiting chemical and oil penetration. Micro-
graphs of the tensile fracture surfaces depict that
the addition of TOR and dynamic vulcanization
helped encapsulating WTD, which minimized the
removal of WTD from the PP matrix. There was an
insignificant change in the melting temperature,
indicating that the addition of TOR and dynamic
 ARTICLE IN PRESS
M. Awang et al. / Polymer Testing 26 (2007) 779–787
vulcanization did not significantly interfere with the
crystal growth in PP/WTD. Thermograms support
the finding that TOR and dynamic vulcanization
improve the interaction of PP and WTD and, hence,
their compatibility.
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