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Use of Carboxylated Nitrile Rubber and Natural RubberBlends as Retreading Compound for OTR Tires
Kaushik Pal,1 Tanya Das,2 Samir K. Pal,1 Chapal K. Das21 Department of Mining Engineering, Indian Institute of Technology, Kharagpur 721302, West Bengal, India
2 Materials Science Centre, Indian Institute of Technology, Kharagpur 721302, West Bengal, India
Ore transportation is one of the important unit opera-tions in a mineral industry. In this study, three raw rub-ber compounds are prepared in three different blendratios, and four types of raw rubber samples of pureNR with silica reinforced has been collected from thedifferent tire retreading industries. Blend propertieslargely depend on the blend ratio and on the blendingtechnique. The improvement in the physical propertiessuch as cure characteristics, mechanical characteriza-tion, cross-link density, FTIR, thermal characterization,SEM studies, and dynamic mechanical analysis hasbeen studied in those samples. It has been found thatretread rubber made with 80 phr XNBR and 20 phr NRhas given the better results when compared with theother samples against all the characterization done. Itis also seen that rubber made by the researchers arevery good in tough, rigid and these are extremely ableto withstand for using as a retread rubber for 35Tdump trucks tire when compared with the retread rub-ber made by the tire retreading industries for differentmines in India. POLYM. ENG. SCI., 48:2410–2417, 2008.ª 2008 Society of Plastics Engineers
INTRODUCTION
Tires used in mining vehicles are very costly and need
regular maintenance, because it is impossible to accept its
replacement expense within very short term. The rugged
working conditions in mining industries reduce the life
span of tires on account of cuts, contamination, abrasion,
wear, speed fluctuations, etc. There are several types of
damage occurred in the dump-truck tire such as tread
detachment, sidewall cuts, impact ruptures, bead damage,
etc. For transportation of minerals from one place to
another, the wear and abrasion must be filled by changing
of tire compounds.
Tire industries consume more than 60% of the rubber
product and the prime factors of considerations are safety
and tread life. Thus, 30% of the mechanical work avail-
able from the fuel is dissipated in the tires. A reduction
of 15% in tire rolling resistance may improve fuel con-
sumption by 4.5% [1]. For this problem, Coal India Lim-
ited, India, is spending lots of money every year towards
the tire retreading expenses for increasing the tire life as
well as to reduce the new tire replacing cost, which is
very much expensive one.
Carboxyl groups have also been introduced into rub-
bers in order that reactions characteristic of the carboxylic
functional group might be employed to crosslink the poly-
mer chains or attach them to other molecules or surfaces
[2]. Also, the group is added to significantly improve the
abrasion resistance of NBR while retaining excellent oil
and solvent resistance. XNBR compounds provide high
tensile strength, tough, abrasion resistant, and good physi-
cal properties at high temperatures. Also, XNBR generally
exhibits poor hysteresis properties and reduced cold tem-
perature flexibility, but in regard to chemical resistance
XNBR is considerably superior.
Also, natural rubber (NR) is known to exhibit numerous
outstanding properties, and reinforcing fillers are necessarily
added into NR in most cases in order to gain the appropriate
properties for specific applications. A wide variety of partic-
ulate fillers are used in the rubber industry for various pur-
poses, of which the most important are reinforcement,
reduction in material costs, and improvements in processing
[3]. Reinforcement is primarily the enhancement of strength
and strength-related properties, abrasion resistance, hard-
ness, and modulus [4, 5]. In most applications, carbon black
(CB) and silica have been used as the main reinforcing fill-
ers that increase the usefulness of rubbers by tire retreading
industries. In general, a CB-reinforced rubber has a higher
modulus than a silica-reinforced one. However, silica pro-
vides a unique combination of tear strength, abrasion resist-
ance, aging resistance, and adhesion properties [6]. In tire
treads, silica yields a lower rolling resistance at equal wear
resistance and wet grip than CB [7]. However, NR exhibits
a limited ozone resistance and a high dependence of
dynamic properties on temperature because of damping
derived from high glass transition temperature (Tg) [8].
Correspondence to: K. Pal; e-mail: [email protected]
Contract grant sponsor: Coal India Limited, Kolkata.
DOI 10.1002/pen.21196
Published online in Wiley InterScience (www.interscience.wiley.com).
VVC 2008 Society of Plastics Engineers
POLYMER ENGINEERING AND SCIENCE—-2008
A literature search shows a lack of studies about
XNBR with NR blends alone. With this work, we pretend
to partially fill this gap. Blending of elastomers has been
often used to obtain an optimum number of desirable
combinations, physical properties, processability, and cost.
NR shows very interesting physical properties because of
its ability to crystallize under stretching. These com-
pounds are capable of forming a chemical link between
these dissimilar rubbers to produce a technologically com-
patible blend. The blend vulcanizates thus produced ex-
hibit enhanced physical properties by judicious selection
of the NR:XNBR ratio [9]. The effort toward improving
the efficiency of such transportation system is essential
for reduce running costs and cutting down the end cost
figures by using the XNBR and NR rubber blends.
So, in this study the main goal is to prepare the better
abrasion resistant retread tire than the retreading compa-
nies and maximize the tire life. For this, XNBR and NR
blends with various compositions have been examined for
testing the wear resistance properties.
EXPERIMENTAL
Materials Used in Rubber Preparation
The carboxylated nitrile rubber (XNBR) used was
Nipol N-34 grade, of Nippon Zeon Co., Japan. Its specific
gravity is 0.98, Mooney viscosity at 1008C is 45. Bound
acrylonitrile content is 27%. Natural rubber (NR) of
RMA-1X grade was supplied by the Rubber Board, Kot-
tayam, Kerala. Zinc oxide, stearic acid, N-cyclohexyl-2-benzothiazyl sulfonamide (CBS), and antioxidant (HQ)
was supplied by Bayer (India). Standard rubber grade pro-
cess oil (Elasto 710), carbon black was purchased from
the local market.
Preparation of Raw Rubber
The compounding formulation for the carboxylated
nitrile rubber and natural rubber blends with its various
ingredients were mixed in a two roll mill at a friction
ratio of 1:2 following standard mixing sequence.
Cure Characteristics of Rubber Compound
The cure characteristics of the rubber compound were
studied with the help of a Monsanto Oscillating Disc Rhe-
ometer (ODR-100s), which complies with ASTM D2084
at 1508C. From the graphs, the optimum cure time, scorch
time, and rate of cure [tmax 2 tmin (dN�m)] could be
determined.
Mechanical Characterization (Tensile and Tear)
Vulcanized slabs were prepared by compression mold-
ing, and the dumbbell shaped specimens were punched
out from a molded sheet by using ASTM Die C. The tests
were done by means of a universal tensile testing machine
(Hounsfield H10KS) under ambient condition (25 6 28C),following the ASTM D 412-99 and ASTM D 624-99. The
moduli at 100%, 200% elongation, tensile strength, tear
strength, and elongation at break (%) were measured at
room temperature. The initial length of the specimens was
25 mm and the speed of the jaw separation was 500 mm/
min.
Five samples were tested for each set of conditions, at
the same elongation rate. The values of the tensile
strength, modulus at 100% elongation, 200% elongation,
and elongation at break were averaged. The relative error
was below 5%. The Shore A hardness was measured.
Determination of Crosslink Density
The crosslink density was determined by immersing a
small amount (known mass) of sample in 100 ml toluene
to attain equilibrium swelling. After this, the sample was
taken out from the toluene and the solvent was blotted
from the surface of the sample and weighed immediately.
TABLE 1. Different composition of the rubber.
Ingredients
Sample code (wt. in phr)
MC-1 MC-2 MC-3
Carboxylated nitrile rubber (XNBR) 80 50 20
Natural rubber (NR) 20 50 80
Carbon black 40 40 40
Stearic acid 2 2 2
Process oil-Elasto 710 2 2 2
Antioxidant (HQ) 1 1 1
Sulfur 1 1 1
Accelerator (CBS) 0.7 0.7 0.7
Activator (ZnO) 5 5 5
TABLE 2. Different composition of the collected rubber from the industries.
Basic ingredients
Sample code
PC-1 (%) OC-1 (%) PC-2 (%) OC-2 (%)
NR 60 50 60 60
Carbon black 30 40 30 30
ZnO 2 2 1.5 1.5
Other chemicals 6.5 (Silica 3–4%) 6.5 (Silica 2–3%) 7.5 (Silica 2–2.5%) 7.5 (Silica 2–3%)
Curatives 1.5 1.5 1.5 1
DOI 10.1002/pen POLYMER ENGINEERING AND SCIENCE—-2008 2411
This sample was then dried out at 808C to constant
weight. Then the chemical crosslink density was calcu-
lated by the Flory-Rehner equation [10].
Fourier Transformed Infrared Spectroscopy
Fourier transform infrared spectroscopy was performed
using a NEXUS 870 FT-IR (Thermo Nicolet) instrument
in dry air at room temperature. Spectra were taken in the
range 4000–0 cm21 in transmission mode.
Thermal Characterization (DTA-TGA)
TGA studies were carried out Shimadzu-DT-40 instru-
ment in presence of air at a rate of 108C/min from 25 to
6008C temperature. Degradation temperature of the com-
posites was calculated by TGA plot.
Scanning Electron Microscopy
The tensile fracture surface of the samples were stud-
ied in a scanning electron microscope (JSM-5800 of
JEOL; Acceleration voltage, 20 kV; type of coating, gold)
at 500 and 1000 times zooming.
Dynamic Mechanical Analysis
Dynamic mechanical analysis was performed in tension
mode of a TA instrument DMA 2980 dynamic mechanical
analyzer at a frequency of 1 Hz with a heating rate of
108C/min. The temperature dependence of storage modulus
(E0), loss modulus (E00), and loss tangent (tan d) was meas-
ured from 258C to 1508C with a heating rate 108C/min.
RESULTS AND DISCUSSIONS
Compound Formulation
Compounding formulations based on changing of the
carbo-oxylated nitrile rubber (XNBR) and NR contents
are shown in Table 1. For vulcanization, the amounts of
additives such as sulfur, CB, process oil, CBS were based
on 100 g of rubber.
Two types of raw (unvulcanized) rubbers, such as pre-
mium quality, mainly used in iron ore and uranium mines
for good mileage as well as better service, and general
quality, mainly used in coal mines, have been collected
from tire retreading industries, India. The industry is the
main supplier of retread tire to Uranium Corporation of
India Limited (UCIL), Airport authority, Eastern Coal-
fields Limited (ECL), Steel Authority of India Limited
(SAIL), Tata Iron and Steel Company Limited (TISCO),
and also some Pvt. Company.
Another two types of raw (unvulcanized) rubbers
namely premium quality and general quality have been
FIG. 1. Rheometric plot of the vulcanizates.
TABLE 3. Rheometric parameters of the vulcanizates.
Cure characteristics MC-1 MC-2 MC-3 PC-1 OC-1 PC-2 OC-2
Minimum
torque (dN m) 20 17 12 5 7 17 14
Maximum
torque (dN m) 80 36 53 53 59 84 77
Scorch time
(min) 1 3 3 4 2 4 2
Optimum cure
time (min) 31 8 10 13 10 15 11
Cure rate
index (min21) 3.33 20.00 14.29 11.11 11.11 9.09 11.11
TABLE 4. Mechanical properties of the rubber samples.
Sample
code
Tensile
strength (MPa)
Tear
strength (N/mm)
Elongation
at break (%)
100% modulus
(MPa)
200% modulus
(MPa)
Hardness
(Shore A)
Crosslink density
(moles/g) 3105
MC-1 8.269 42.00 119.2 3.359 6.254 75 10.19
MC-2 3.906 21.70 171.6 1.552 2.640 70 7.081
MC-3 1.388 58.30 76.80 1.482 2.223 64 7.989
PC-1 20.23 26.15 896.0 1.939 3.534 65 7.422
PC-2 4.105 13.33 201.9 1.936 3.320 75 —
OC-1 10.05 57.26 540.0 3.197 7.135 69 6.470
OC-2 9.379 30.37 424.5 2.766 5.349 70 —
2412 POLYMER ENGINEERING AND SCIENCE—-2008 DOI 10.1002/pen
collected from another reputed tire retreading industries in
India. They supply the retread tire to different mines
under Coal India Limited (CIL), Mahanadi Coalfields
Limited (MCL), and Northern Coalfields Limited (NCL).
All the four raw rubber samples have been collected
from those tire retreading companies are depicted in Ta-
ble 2, but the right proportions of the composition is not
found from the companies because of their trade secret.
FIG. 2. (a–g): FTIR plots for rubber samples.
DOI 10.1002/pen POLYMER ENGINEERING AND SCIENCE—-2008 2413
Cure Characteristics of the Rubber Vulcanizates
The torque versus strain curve for all the rubber vul-
canizates are shown in Fig. 1. The optimum cure time for
MC-2 and MC-3 rubber is lesser than PC-1, PC-2, OC-1,
and OC-2 due to the mixing of XNBR with NR and is
shown in Table 3. The optimum cure time of the 80 phr
XNBR and 20 phr NR is much higher than all other rub-
ber vulcanizates. The rate of cure (tmax 2 tmin) always
increased with increasing concentration of NR. This
increase in cure rate may be due to the fact that an
increasing concentration of NR caused the vulcanization
reaction to increase and create more active cross-link sites
in the rubber compound.
In addition, the gradual decrease in scorch time and
cure time for MC-2 and MC-3 might be decreased
because these compounds have experienced greater ther-
mal history during mixing as a result of their higher com-
pound viscosities. For all samples, the scorch time of the
NR is increased.
It is known that the shear heating during mixing
increases when silica loading is increased due to the
increase of compound viscosity [11]. This explanation is
supported by the value of minimum torque determined
from rheometer cure curves.
Mechanical Properties of the Rubber Samples
Tensile strength, modulus, elongation at break, tear
strength, shore hardness, and cross-link density are all
shown in Table 4. The tensile strength of MC-1 is much
higher than MC-2 and MC-3 due to the addition of more
NR with XNBR. But tensile strength of PC-1 and OC-1 is
higher to all other rubber vulcanizates because of the
addition of additives such as silica. Some researchers [11]
found that tensile retention tends to be enhanced when
the silica content is increased. The tear strength of the
MC-1 is moderate than MC-2 and MC-3. Also the tear
strength of PC-1 and OC-1 is higher than OC-2 and PC-2,
respectively.
From the data, it was found that MC-2, MC-3, PC-2,
and OC-2 have lower tensile strength and percentage of
elongation at break compared to MC-1, PC-1, and OC-1.
This can be explained because PC-2 and OC-2 rubber
contains certain amount silica, whereas MC-2 and MC-3
contain lesser amount of XNBR, which causes main chain
degradation and lowers the percentage of elongation and
hence tensile strength. Another factor, which may be re-
sponsible to decrease the tensile strength, is the presence
of greater amount of cross-linked gel in those rubbers
compared with other vulcanizates, which are not dispersed
in the continuous matrix of the rubber.
The module of all the XNBR vulcanizates increased
with an increasing concentration of XNBR. This was for
one or two possible reasons: the restriction of molecular
chain mobility and an increase in the cross-link density.
The latter can be confirmed by the cross-link density data
that is given in Table 4. Addition of large amounts of NR
decreases the cross-link density in vulcanization steps.
Shore hardness of the MC-1 is much higher than all other
vulcanizates. It is clearly visible that addition of more
percentage of NR with XNBR decreases the hardness of
the vulcanized rubber.
FTIR Spectral Analysis
The IR Spectra of the different samples are shown
below in their respective graphs. Figure 2a shows the IR
Spectra of 80 phr XNBR and 20 phr NR (MC-1). Here, a
distinct peak at 3700 cm21 which may be due to the
asymmetric stretching peak of C��H bond of XNBR is
observed. The peak at 2900 cm21 is due to the symmetric
stretching of the C��H bond. The peak at frequency range
of 2500 cm21 may be due to the C��N triple bond.
Similarly from the Fig. 2b, a distinct peak at frequency
2900 cm21 for C��H bond is seen. The peak at 1800
cm21 may be due to the C��H bond of NR. Other peaks
are similar as earlier because of the presence of the
XNBR. The peaks at 1597 cm21 is due to the stretching
frequency of the C¼¼C of the XNBR group.
Figure 2c shows a similar bond frequencies when com-
pared with the above graph because the composition is
same with varying ratios. So, a slightly shift in the band
frequencies is observed from the FTIR plots.
In Fig. 2d, the peak at 2920 cm21 is due to the C��H
bond of NR. The peak at 1600 cm21 is due to the C¼¼C
bond of NR.
The rest figure also shows similar bond frequencies. In
case of Fig. 2d–g, we can see a new peak at 1028 cm21,
which may be due to the incorporation of the silica group
in the matrix.
These observations suggest that silica reacts with the
carbon–carbon double bonds and slower the reversion
reaction rate and hence increases the mechanical proper-
ties of the vulcanizates.
Another important observation was that unlike Padella.
et al. [12] there was no peak in the range of 1730 cm21
FIG. 3. TGA plots of rubber vulcanizates.
2414 POLYMER ENGINEERING AND SCIENCE—-2008 DOI 10.1002/pen
([C¼¼O stretching peak), which indicated that the oxida-
tion of main polymeric chain did not occur at the time of
rubber milling with the help of cracker cum mixing mill
at high temperature.
Thermal Analysis
High temperature TGA (30–7008C) curves for the sam-
ple are shown in Fig. 3. The temperature for the onset of
degradation (T1), the temperature at which 10% degrada-
tion occurred (T10), the temperature at which 50% degra-
dation occurred (T50), and the temperature at which 90%
degradation occurred (T90) were calculated from the TGA
plots and are given in Table 5.
It was observed that the onset degradation temperature
was higher for higher concentration of XNBR rubber than
NR one. The onset degradation temperature thereby prob-
ably decreased in the case of other rubber samples due to
a decrease in cross-link density. Cross linking increased
the rigidity of the system, which in turn increased the
thermal stability. The rate of degradation was almost the
same up to 90% degradation for all the samples.
DMA Analysis
The storage modulus versus temperature curves are
shown in Fig. 4. The storage modulus of the MC-1 was
higher than MC-2 and MC-3, and it increased due to the
increasing concentration of the XNBR rubber, the cross-
link density was found to increase along with its storage
modulus. Storage modulus at 30, 50, 75, 100, and 1258Chas been calculated and all the data are depicted in Table
6. The storage modulus decreases with the increase in the
temperature.
For OC-2, storage modulus is much higher than MC-1
due to the incorporation of silica, but cross-link density is
much lower than MC-1.
However, the increase in the storage modulus at small
strains with increasing silica content is mainly caused by
the increase in strong filler–filler interaction [13, 14].
Others, such as PC-1, PC-2, and OC-1 show the moderate
storage modulus with the change in temperature.
Figure 5 shows the tan d versus temperature of the
rubber samples. The a-relaxations peak of the MC-1 and
MC-2 was shifted to lower temperature side within the
temperature but MC-3, PC-1, PC-2, OC-1, and OC-2 are
shifted to higher temperature side. It seems that NR con-
tain certain chain degradation (evidence from decrease in
cross-link density, Table 4), which restricted the molecu-
lar chain mobility, and hence, the a-relaxations peak tem-
perature shifted toward the higher side.
Also, it has been reported that rolling resistance of
tires is related to tan d value at temperatures of 50–808C[15]. A low tan d value is needed for achieving the low
rolling resistance and saving energy.
FIG. 5. Tan d of the rubber samples as a function of temperature.
TABLE 5. TGA parameters of the samples (8C).
Sample code T1 T10 T50 T90
MC-1 387 396 463 547
MC-2 264 342 449 548
MC-3 258 344 452 547
PC-1 253 314 422 546
OC-1 263 334 412 541
PC-2 261 332 423 535
OC-2 225 346 441 546
FIG. 4. Storage modulus of the rubber samples as a function of temper-
ature.
TABLE 6. Storage modulus of the samples at different temperatures.
Sample Code
Storage Modulus (MPa)
308C 508C 758C 1008C 1258C
MC-1 17.66 14.01 9.10 5.34 4.20
MC-2 7.61 6.54 4.68 3.06 2.40
MC-3 6.29 5.64 4.62 3.42 2.94
PC-1 12.03 10.84 7.91 5.76 4.88
OC-1 7.25 6.89 5.69 4.62 4.20
PC-2 10.36 9.70 7.85 6.23 5.39
OC-2 17.84 16.10 11.91 8.92 7.43
DOI 10.1002/pen POLYMER ENGINEERING AND SCIENCE—-2008 2415
In this experiment, tan d of the vulcanizates having
various filler ratios was determined at 1508C. The result
shows that tan d of the vulcanizates tends to reduce for
MC-1 and MC-2, and subsequently goes up when silica
loading is higher for PC-1, PC-2, OC-1, and OC-2. It
seems that rubber contain certain amount of main chain
degradation (evidence from decrease in cross-link density,
Table 4), which restricted the molecular chain mobility,
FIG. 6. SEM photographs of the (a) MC-1, (b) MC-2, (c) MC-3, (d) PC-1, (e) OC-1, (f) PC-2, and (g) OC-
2 rubber samples.
2416 POLYMER ENGINEERING AND SCIENCE—-2008 DOI 10.1002/pen
and hence, the a-relaxation peak temperature shifted to-
ward higher side [16]. The result obviously suggests the
lowest rolling resistance in the vulcanizates containing
80 phr XNBR and 20 phr NR.
SEM Study
The tensile fracture samples were scanned after gold
coating and are represented in Fig. 6(a–g). The smooth
fracture surfaces observed for all rubber samples. The
micrographs of the 80 phr XNBR and 20 phr NR rubber
(MC-1) shows the smooth filler dispersion and unidirec-
tional tear path oriented along the direction of flow,
which is smooth rubbery in nature, leading to high tensile
strength and high elongation at break than MC-2 and
MC-3. Figure 6b and c is characterized by a smooth, rub-
bery failure (which is a smooth failure in the case of rub-
ber samples without the formation of necking) where the
additives are clearly seen; the appearance is associated
with a low tensile strength. On increasing the silica with
NR (Fig. 6d–g), the fracture mode was completely
changed and it appears that the number of tear paths in
different directions was being constructed by the addi-
tives, giving the samples high tensile and modulus than
all the rubber samples. Figure 6a, d, and e is again char-
acterized by a unidirectional crack path without any fold-
ing making the vulcanizate high tensile and high elonga-
tion at break.
CONCLUSIONS
Preparation of abrasion resistant tires treads rubber
with the help of an open two-roll-mixing mill represent a
novel method for making valuated rubber products. The
XNBR with addition of NR obtained from this process
has very good mechanical properties when compared with
some collected rubbers from different tire retreading
industries.
It is found that the XNBR has potential as an effective
modifier for natural rubber because its incorporation into
rubber enhances the plastication of NR during mastication
in the mill. Vulcanizate properties of NR such as modu-
lus, resistance to abrasion, and compression set are
improved on incorporation of XNBR at a blend ratio of
80 phr XNBR with NR. Data obtained from different rub-
ber characterization in this study show that both modulus
and crosslink density of rubber samples influence their re-
sistance to abrasion, but the former parameter has an
overriding effect.
80 phr of XNBR and 20 phr of NR blends has the
good curing properties and thermal properties than of all
prepared and collected rubber samples. It is also found
that 80 phr of XNBR and 20 phr of NR blends rubber as
retreading tire compound has the ability to withstand with
the mines harsh condition, and also given more tire life
than those of the samples collected from the tire retread-
ing industries.
ACKNOWLEDGMENTS
The authors thank the tire retreading companies for
their immense support and supply of raw retreading com-
pounds. The authors also thank the members of the pro-
ject and key laboratory of Materials Science Centre and
Central Research Facility at IIT, Kharagpur.
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