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The Free Library > Business and Industry > Business > Rubber World > April 1, 2006
The Free Library > Business and Industry > Chemicals, plastics and rubber > Rubber World > April 1, 2006
The Free Library > Date > 2006 > April > 1 > Rubber World

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Improving rolling resistance of NR tread formulations.
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Energy conservation is of interest on both a national and rubber industry level. High oil prices
will increase the desire for conservation. A major source of energy loss in tires is the motive
(kinetic) energy that is converted to heat in the tire tread as the tire rolls down the road. Low
rolling resistance can result in significant energy savings.

Many manufacturers of passenger car tires have adopted the partial replacement of carbon
black by silica, the so-called "green" tire, to lower rolling resistance. A key to the successful use
of silica in automobile tire tread stock is the use of a silane coupling agent to improve bonding of
the silica to the rubber. Another factor is the creation of special solution styrene-butadiene
rubbers with exact control of microstructure.

Truck tires are based primarily on natural rubber (NR) because of its exceptional resistance to
heat build-up and low cut and chip properties. NR is the polymer of choice for truck tire treads
because it runs cooler and has lower rolling resistance, which translates to reduced fuel
consumption. Furthermore, a decrease in running temperature yields better tire aging resistance
and therefore improved retreadability.

At the present time, truck tire treads use highly reinforcing carbon black for maximum
reinforcement and excellent resistance to abrasion. A truck tire is expected to last over 400,000
km (250,000 miles). The replacement of carbon black by silica in truck applications has been
hampered by incomplete coupling of the silica to the polymer chain ends of the NR. In addition
to not obtaining sufficiently lower rolling resistance, abrasion resistance also typically suffers.

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A survey of global truck tire manufacturers, retread makers and freight haulers was conducted
to obtain a "voice of the customer," to learn customer needs and the important parameters Precured urethan

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necessary for the adoption of more energy-efficient tires.


innovations)
End users regard cost per mile as the most important criteria, specifically cost per 0.7 mm (0.03 Increase truck tire
in.) of tread wear. Tires are the second highest capital expense for trucking companies. Average modifications.
fuel economy is 2-1/2 to 3-1/2 km/L (6-8 miles/gal.), and it is felt an improvement of 0.1 km/L
(0.2 miles/gal.) would be significant. Silica/silane
Article)
Tire manufacturers indicate wear and rolling resistance are the most important parameters. The challenge ah
One-third of fuel cost for trucking companies is simply to roll the tires. A 3% reduction in rolling (Tech Service).(ru
resistance results in a 1% improvement in fuel costs. Some sacrifice in tread wear would be
Patent news.(inclu
acceptable to realize a fuel economy benefit; there are more potential savings in lowering rolling
resistance than in increasing tread wear. Development of H
properties, perform
Measuring loss factor as an indication of rolling resistance
Vulcanizable rubb
vehicle tires. (Pat
Dynamic mechanical testing can be used to measure loss factor as tangent delta, which is the Coordinamento P
ratio of viscous response (loss modulus) divided by the elastic response (storage modulus).
Tired of rolling res
Loss factor can be used as an indication of relative rolling resistance, with lower tangent delta
values indicative of lower rolling resistance. The storage modulus is also important, because it
determines how much the tread will deform under a given load as the tire rotates through the
footprint.

Laboratory test data for compounds based on either solution SBR or NR are shown in table I to
illustrate the differences in dynamic mechanical properties. In the SBR/BR passenger tread
compound, the data show a large improvement in loss factor by the addition of precipitated
silica, from about 0.20 to 0.12. The NR truck tread compound shows less reduction in loss factor
by the addition of precipitated silica, from about 0.18 to 0.14.

Effect of silica level

Precipitated silica was tested as a partial replacement for N220 carbon black in the NR base
formulation, and test results are shown in table 2.

Higher levels of precipitated silica lead to slightly lower abrasion resistance and modulus. The
loss factor of the compounds containing silica is significantly lower than the black-filled
compound, with the 60 phr silica compound exhibiting less than half the loss factor of the black-
filled compound at 4% double strain amplitude.

The initial addition of silica yields a compound with lower tear strength and shorter scorch and
cure times. Increasing levels of silica provide improved tear strength with longer scorch and cure
times, becoming comparable to carbon black at the highest silica level.

Effect of silane level

Holding the silica level constant at 60 phr (with 5 phr N220 carbon black), the level of TESPT
silane was varied from 2.4 to 6.0 phr. Formulas and test data are shown in table 3.

The results in figures 1-3 show that higher silane levels lead to lower scorch and cure times with
higher modulus and abrasion resistance. Loss factor appears to be optimum between 3.6 and
4.8 phr.

[FIGURES 1-3 OMITTED]

Effect of accelerator type and level

In the base formulation with 60 phr silica, DPG was compared as a secondary accelerator to
Royalac 150 (R-150) with activator. Table 4 contains the formulas and test results, including a
black-filled compound as a control. Overall, DPG yields poorer abrasion resistance than the R-
150 system. As shown in figures 4-6, higher levels of either secondary accelerator system lead

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to lower loss factor, shorter scorch and cure times and higher tensile modulus. Although figure 6
shows that the loss factor of DPG is similar to the R-150 system by RPA torsional shear results,
the MTS results in compression of table 4 indicate that the R-150 system is superior to DPG for
dynamic properties.

[FIGURES 4-6 OMITTED]

Effect of activator components

The activator is a mixture of several components. The effect of three components was studied in
a [2.sup.3] factorial design. The formulas and test results are contained in table 5. A low level of
component A and a high level of component B gave a desirable combination of scorch and cure
times with the best loss factor and abrasion resistance.

Regression analysis indicated no highly significant interaction or quadratic effects. The main
linear effects are shown in table 6. The high level of component C gives improved abrasion
resistance with no highly significant effect on other properties. As indicated in table 6,
component A detracts from abrasion resistance and lengthens cure time. Component B lowers
scorch and cure times and provides the most significant improvement in loss factor.

It was felt that the initial activator blend, although providing good technical performance, was in
need of improvement. Odor and worker health and safety were specific issues of concern.
Therefore, alternatives for components A and B were sought. After several analogues were
tested, a new blend composition was selected--designated Activator 2. Figures 7 and 8 compare
these two activators for dynamic properties, and a good match for loss factor is indicated.

[FIGURE 7 OMITTED]

Tire build results

A tire test was undertaken to evaluate the R-150 system with each activator. A black-filled
formulation was used as a control. The three compounds were prepared at a custom mixer, and
pre-cured treads were extruded and cured. Sixty drive position tires, size 285/80-R22.5, were
purchased and buffed. Twenty tires of each compound were retreaded. The specific
formulations and laboratory results are shown in table 7. Tire tests found:

* Compound AC yielded a rolling resistance of 18.3 kg (40.4 lbs.).

* Compound AD yielded a rolling resistance of 15.8 kg (34.9 lbs.), a 13.6 % reduction.

* Compound AE yielded a rolling resistance of 17.6 kg (38.9 lbs), a 3.8 % reduction.

Based on the fastest wearing groove from on-tire fleet trials, the projected distance to wear-out
showed:

* Compound AC gave a tread wear of 417,010 km (259,130 miles).

* Compound AD gave a tread wear of 356,600 km (221,590 miles), a 14.5% reduction.

* Compound AE gave a tread wear of 377,070 km (234,310 miles), a 9.6% reduction.

Assuming a sales price of $450 per tire and a diesel fuel cost of 79 cents/L ($3/gal.), compound
AD results in a cost savings of $8,684 in 402,320 km (250,000 miles); compound AE, $2,574.
These calculations do not take into account the effect of any raw material cost differences and
the possible need to adjust the tire sales price.

The unexpectedly poorer rolling resistance results for compound AE were verified by laboratory
measurement of loss factor, as shown in figure 9.

Comparing figure 9 to figure 8, it is clear that neither factory compound with silica, R-150 and

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activator achieved the 0.1 loss factor of the laboratory mixed compounds. Why the poorer
factory results were obtained is being examined. Our working hypothesis is volatility of one or
more of the components, because all three factory compounds required hot remilling to bring
viscosity down to a workable range.

[FIGURES 8-9 OMITTED]

For the tires with the lowest rolling resistance, a savings of about $8,600 per 18-wheel rig has
been calculated, excluding any differences in the raw material cost of the tires. The laboratory
measurement of tangent [delta] in compression is highly correlated with rolling resistance of the
field tires, as shown in figure 10. If it is possible to approach the tangent [delta] obtained in the
more favorable laboratory tests, we may extrapolate that savings in excess of $10,000 per rig
might be achieved.

[FIGURE 10 OMITTED]

Summary

Royalac 150 when used with an activator can enhance the performance of the silica/silane
system in NR to significantly improve loss factor without major sacrifice in abrasion resistance or
other performance properties. Laboratory results were confirmed by rolling resistance and tread
wear results from a fleet test of truck tires. The potential economic impact is felt to be sufficient
to justify additional technical work to find a practical activator formulation.

Table 1--passenger and truck tread compounds and test data

Tire tread type Passenger Truck


Compound A B C D

Solution SBR (Solflex 1216) 75.0 75.0 -- --


Polybutadiene (Budene 1207) 25.0 25.0 -- --
Natural rubber (SIR 20) -- -- 100.0 100.0
N-234 carbon black 72.0 5.0 -- --
N-220 carbon black -- -- 60.0 5.0
Silica (Zeosil 1165) -- 80.0 -- 60.0
Aromatic oil (Sundex 790) 32.5 40.0 7.0 7.0
TESPT silane (Silquest A-1289) -- 3.6 -- 4.8

Second pass
Zinc oxide (Kadox 911) 2.5 2.5 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0 2.0 2.0
Industrene R stearic acid 1.0 1.0 2.0 2.0
Sunproof improved wax 1.5 1.5 1.5 1.5

Final pass
TBBS (Delac NS) 1.5 1.5 1.0 1.0
DPG -- 2.0 -- 1.0
Sulfur 2.0 2.0 2.0 2.0

Mooney at 100[degrees]C
Viscosity, ML 1+4 78.0 91.0 59.0 59.0

Mooney at 135[degrees]C
Scorch, MS t3, minutes 22.1 11.3 13.7 15.2

Rheometer at 160[degrees]C
ML, lb.-in. 7.9 9.8 7.2 6.7
MH, lb.-in. 34.2 36.4 41.7 36.0
Ts2, minutes 5.8 2.6 4.8 4.6

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T90, minutes 11.2 14.0 6.5 8.2

Cured at 160[degrees]C
Tensile strength, MPa 17.0 20.6 28.4 27.4
Elongation at break, % 420 420 513.8 587.6
M 100, MPa 2.4 2.3 3.0 1.9
M 300, MPa 11.5 12.3 15.2 9.1
Hardness, A 63.0 59.0 64.0 62.0
M300/M100 4.8 5.3 5.1 4.9

MTS at 10 Hz and 60[degrees]C


Tangent delta
Peak-to-peak strain,
2 0.184 0.110 0.178 0.140
4 0.198 0.120 0.180 0.145
6 0.201 0.123 0.175 0.139
8 0.204 0.125 0.166 0.142
10 0.205 0.128 0.160 0.138

E', MPa
Peak-to-peak strain,
2 8.1 6.7 7.1 4.4
4 7.1 6.2 6.1 4.1
6 6.5 6.0 5.6 3.9
8 6.2 5.8 5.4 3.9
10 5.9 5.7 5.3 3.9

Table 2--silica as partial replacement for carbon black

Compound E F G H

Natural rubber 100.0 100.0 100.0 100.0


N-220 carbon black 59.0 41.0 23.0 5.0
Precipitated silica - 20.0 40.0 60.0
Aromatic oil 7.0 7.0 7.0 7.0
TESPT silane polysulfide - 1.4 2.8 3.6
Activator - 1.5 2.0 2.5

2nd pass
Zinc oxide 3.0 3.0 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0 2.0 2.0
Industrene R stearic acid 2.0 2.0 2.0 2.0
Sunproof improved wax 1.5 1.5 1.5 1.5

Final pass
TBBS Delac NS 1.00 1.00 1.00 1.00
TATD Royalac 150 - 0.40 0.40 0.40
CTP retarder (Santogard PVI) 0.20 0.20 0.20 0.20
Sulfur 2.00 2.25 2.25 2.25

Mooney at 100[degrees]C
Viscosity, ML 1+4 63 59 61 57

Mooney at 135[degrees]C
Scorch, MS t3, minutes 16.6 11.9 12.8 20.4

Rheometer at 160[degrees]C
ML, lb-in. 7.1 6.7 6.1 5.6
MH, lb-in. 40.4 41.0 38.0 35.6

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Ts2, minutes 3.3 2.8 3.2 3.9


T90, minutes 6.8 5.0 5.9 7.1
Cured at 160[degrees]C, minutes 9 7 8 9
Tensile strength, MPa 28.3 28.9 27.9 28.2
Elongation at break, % 541 537 574 618
M 100, MPa 2.8 2.9 2.6 2.3
M 300, MPa 14.7 14.9 12.4 10.9
Hardness, A 66 64 63 61
Die C tear, kN/m 109 97 117 119
M300/M100 5.2 5.1 4.9 4.6

Aged 2 weeks at 70[degrees]C


Tensile strength, MPa 27.9 27.0 27.3 28.0
Elongation at break, % 448 447 482 520
M100, MPa 4.4 4.8 4.1 3.8
M300, MPa 19.5 19.3 18.0 16.3
Hardness, A 72 71 67 67
Die C tear, kN/m 89 80 73 63

DIN abrasion index


Average of 3 samples 99.5 101.0 96.3 96.7
RPA test at 1OHz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1.5 0.114 0.074 0.058 0.068
2 0.137 0.085 0.069 0.070
4 0.188 0.113 0.089 0.082
10 0.211 0.136 0.107 0.104
G', MPa
Peak-to-peak strain, %
1.5 5.1 3.4 2.7 2.6
2 4.6 3.2 2.6 2.5
4 3.6 2.7 2.3 2.3
10 2.4 2.1 1.9 1.9
MTS at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1 0.151 0.080 0.069 0.054
2 0.182 0.101 0.086 0.083
4 0.185 0.113 0.099 0.088
6 0.176 0.113 0.101 0.092
8 0.171 0.112 0.100 0.089
10 0.163 0.110 0.097 0.088
E', MPa
Peak-to-peak strain, %
1 8.5 6.9 5.7 5.3
2 7.4 6.4 5.5 5.1
4 6.4 6.0 5.3 4.9
6 6.0 5.8 5.3 4.9
8 5.8 5.7 5.2 4.9
10 5.7 5.7 5.3 4.9

Table 3--effect of silane level

Compound I J K

Natural rubber 100.0 100.0 100.0


N-220 carbon black 59.0 5.0 5.0
Precipitated silica - 60.0 60.0

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Aromatic oil 7.0 7.0 7.0


TESPT silane - 6.0 4.8
Activator - 2.5 2.5

2nd pass
Zinc oxide 3.0 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0 2.0
Industrene R stearic acid 2.0 2.0 2.0
Sunproof improved wax 1.5 1.5 1.5

Final pass
Delac NS 1.00 1.00 1.00
Royalac 150 - 0.40 0.40
CTP retarder 0.20 0.20 0.20
Sulfur 2.00 2.00 2.00

Mooney at 100[degrees]C
Viscosity, ML 1+4 56 58 62

Mooney at 135[degrees]C
Scorch, MS t3, minutes 17.1 11.8 14.2
18 pt. rise time, minutes 21.1 19.7 22.1

Rheometer at 160[degrees]C
ML, lb.-in. 6.2 6.0 6.5
MH, lb.-in. 38.6 38.1 37.4
Ts2, minutes 3.5 3.3 3.5
T90, minutes 7.2 6.3 6.7
Cured at 160[degrees]C, minutes 9 8 9
Tensile strength, MPa 28.8 29.0 28.5
Elongation at break, % 566 588 586
M 100, MPa 2.7 2.7 2.2
M 300, MPa 13.8 12.7 11.8
Hardness, A 64 63 61
M300/M100 5.2 4.7 5.3
Die C tear, kN/m 108 125 124
Aged 2 weeks at 70[degrees]C
Tensile strength, MPa 28.6 27.7 27.9
Elongation at break, % 462 448 482
M100, MPa 4.3 4.6 4.3
M300, MPa 19.2 19.1 18.2
Hardness, A 69 70 70
Die C tear, kN/m 98 94 89

DIN abrasion index


Average of 3 samples 95.5 101.0 95.8
RPA test at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1.5 0.116 0.054 0.059
2 0.129 0.062 0.067
4 0.172 0.068 0.073
10 0.190 0.080 0.093
G', MPa
Peak-to-peak strain, %
1.5 4.3 2.6 2.7
2 3.9 2.5 2.6
4 3.0 2.2 2.4
10 2.2 2.0 2.0

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MTS at 10 Hz and 60[degrees]C


Tangent delta
Peak-to-peak strain, %
1 0.144 0.099 0.079
2 0.169 0.101 0.085
4 0.180 0.103 0.093
6 0.174 0.108 0.091
8 0.158 0.105 0.093
10 0.154 0.101 0.092
E', MPa
Peak-to-peak strain, %
1 7.2 4.8 5.6
2 6.3 4.7 5.3
4 5.5 4.5 5.1
6 5.1 4.5 5.1
10 4.9 4.6 5.1

Compound L M

Natural rubber 100.0 100.0


N-220 carbon black 5.0 5.0
Precipitated silica 60.0 60.0
Aromatic oil 7.0 7.0
TESPT silane 3.6 2.4
Activator 2.5 2.5

2nd pass
Zinc oxide 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0
Industrene R stearic acid 2.0 2.0
Sunproof improved wax 1.5 1.5

Final pass
Delac NS 1.00 1.00
Royalac 150 0.40 0.40
CTP retarder 0.20 0.20
Sulfur 2.25 2.40

Mooney at 100[degrees]C
Viscosity, ML 1+4 61 65

Mooney at 135[degrees]C
Scorch, MS t3, minutes 17.6 22.4
18 pt. rise time, minutes 25.3 27.5

Rheometer at 160[degrees]C
ML, lb.-in. 6.5 7.7
MH, lb.-in. 36.8 38.9
Ts2, minutes 3.8 3.7
T90, minutes 7.0 7.3
Cured at 160[degrees]C, minutes 9 9
Tensile strength, MPa 28.9 28.2
Elongation at break, % 623 647
M 100, MPa 2.2 2.1
M 300, MPa 10.9 9.8
Hardness, A 62 59
M300/M100 4.9 4.7
Die C tear, kN/m 109 115
Aged 2 weeks at 70[degrees]C

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Tensile strength, MPa 28.2 27.1


Elongation at break, % 469 488
M100, MPa 4.1 3.9
M300, MPa 17.7 16.7
Hardness, A 68 71
Die C tear, kN/m 85 69

DIN abrasion index


Average of 3 samples 93.7 88.0
RPA test at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1.5 0.058 0.067
2 0.069 0.076
4 0.076 0.095
10 0.095 0.108
G', MPa
Peak-to-peak strain, %
1.5 2.7 3.3
2 2.5 3.2
4 2.3 2.8
10 2.0 2.3
MTS at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1 0.068 0.095
2 0.085 0.101
4 0.093 0.113
6 0.094 0.112
8 0.091 0.114
10 0.086 0.113
E', MPa
Peak-to-peak strain, %
1 5.1 4.0
2 4.9 4.1
4 4.8 4.0
6 4.7 3.9
10 4.8 3.9

Table 4--effect of secondary accelerator type and level

Compound N O P

Natural rubber 100.0 100.0 100.0


N-220 carbon black 59.0 5.0 5.0
Precipitated silica - 60.0 60.0
Aromatic oil 7.0 7.0 7.0
TESPT silane - 4.8 4.8
Activator - - -

2nd pass
Zinc oxide 3.0 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0 2.0
Industrene R stearic acid 2.0 2.0 2.0
Sunproof improved wax 1.5 1.5 1.5

Final pass
Delac NS 1.00 1.00 1.00
Royalac 150 - - -

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CTP retarder 0.20 - 0.20


DPG - 0.50 1.00
Sulfur 2.00 2.12 2.00

Mooney at 100[degrees]C
Viscosity, ML 1+4 57 65 54

Mooney at 135[degrees]C
Scorch, MS t3, minutes 14.4 14.4 13.6
18 pt. rise time, minutes 17.5 19.6 19.4

Rheometer at 160[degrees]C
ML, lb.-in. 6.8 7.5 6.7
MH, lb.-in. 40.7 32.1 36.1
Ts2, minutes 3.3 3.3 3.1
T90, minutes 6.7 10.1 6.9
Cured at 160[degrees]C, minutes 9 12 9
Tensile strength, MPa 28.4 22.6 27.4
Elongation at break, % 537 592 617
M 100, MPa 2.9 1.5 2.0
M 300, MPa 14.8 7.7 10.0
Hardness, A 64 61 62
M300/M100 5.1 5.1 5.3
Die C tear, kN/m 125.0 114.0 124.0
Aged 2 weeks at 70[degrees]C
Tensile strength, MPa 27.9 27.3 27.9
Elongation at break, % 446 544 537
M100, MPa 4.6 2.9 3.3
M300, MPa 19.7 13.9 15.0
Hardness, A 72 70 68
Die C tear, kN/m 98 - 103

DIN abrasion index


Average of 3 samples 94.2 71.2 76.3
RPA test at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1.5 0.110 0.084 0.066
2 0.129 0.095 0.071
4 0.181 0.127 0.090
10 0.202 0.156 0.110

G', MPa
Peak-to-peak strain, %
1.5 5.0 4.4 3.4
2 4.5 4.2 3.2
4 3.4 3.5 2.8
10 2.4 2.6 2.3
MTS at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1 0.147 0.136 0.110
2 0.175 0.148 0.134
4 0.180 0.156 0.138
6 0.175 0.156 0.134
8 0.163 0.154 0.135
10 0.158 0.151 0.132
E', MPa
Peak-to-peak strain, %

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1 7.9 4.9 4.8


2 6.8 4.6 4.5
4 5.9 4.3 4.2
6 5.5 4.2 4.1
8 5.3 4.2 4.0
10 5.2 4.2 4.0

Compound Q R

Natural rubber 100.0 100.0


N-220 carbon black 5.0 5.0
Precipitated silica 60.0 60.0
Aromatic oil 7.0 7.0
TESPT silane 3.6 3.6
Activator 2.5 2.5

2nd pass
Zinc oxide 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0
Industrene R stearic acid 2.0 2.0
Sunproof improved wax 1.5 1.5

Final pass
Delac NS 1.00 1.00
Royalac 150 0.25 0.40
CTP retarder 0.20 0.20
DPG - -
Sulfur 2.30 2.25

Mooney at 100[degrees]C
Viscosity, ML 1+4 63 62

Mooney at 135[degrees]C
Scorch, MS t3, minutes 16.3 15.4
18 pt. rise time, minutes 19.2 21.1

Rheometer at 160[degrees]C
ML, lb.-in. 7.0 7.3
MH, lb.-in. 39.4 39.9
Ts2, minutes 3.5 3.5
T90, minutes 6.8 6.5
Cured at 160[degrees]C, minutes 9 9
Tensile strength, MPa 27.6 29.0
Elongation at break, % 625 606
M 100, MPa 2.1 2.3
M 300, MPa 10.3 11.6
Hardness, A 65 62
M300/M100 5.0 5.1
Die C tear, kN/m 116.0 128.0
Aged 2 weeks at 70[degrees]C
Tensile strength, MPa 28.7 27.9
Elongation at break, % 509 489
M100, MPa 4.2 4.4
M300, MPa 17.6 18.0
Hardness, A 73 73
Die C tear, kN/m 69 89

DIN abrasion index


Average of 3 samples 86.2 99.9

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RPA test at 10 Hz and 60[degrees]C


Tangent delta
Peak-to-peak strain, %
1.5 0.063 0.057
2 0.077 0.064
4 0.103 0.082
10 0.133 0.101

G', MPa
Peak-to-peak strain, %
1.5 5.3 3.6
2 5.0 3.4
4 4.2 3.0
10 3.1 2.4
MTS at 10 Hz and 60[degrees]C
Tangent delta
Peak-to-peak strain, %
1 0.082 0.091
2 0.103 0.111
4 0.116 0.112
6 0.115 0.112
8 0.112 0.111
10 0.107 0.109
E', MPa
Peak-to-peak strain, %
1 6.4 5.6
2 6.2 5.5
4 5.8 5.1
6 5.5 5.0
8 5.4 5.0
10 5.4 5.0

Table 5--effect of activator components

Compound S T U V

Natural rubber 100.0 100.0 100.0 100.0


N-220 carbon black 5.0 5.0 5.0 5.0
Precipitated silica 60.0 60.0 60.0 60.0
Aromatic oil 7.0 7.0 7.0 7.0
TESPT Silane 3.6 3.6 3.6 3.6

2nd pass
Activator 1 2.50 0.00 0.00 0.00
Component A 0.00 0.55 0.15 0.15
Component B 0.00 0.68 0.20 0.20
Component C 0.00 0.17 0.17 1.60
Zinc oxide 3.0 3.0 3.0 3.0
Flexzone 7P 2.0 2.0 2.0 2.0
Industrene R 2.0 2.0 2.0 2.0
Sunproof improved 1.5 1.5 1.5 1.5

Final pass for all. 1.00 Delac NS; 0.40 Royalac 150; 0.20 CTP retarder;
2.25 sulfur

Mooney at 135[degrees]C
Scorch, MS t3, min. 17 15 15 16
Rheometer at 160[degrees]C
ML, lb.-in. 6.2 5.8 5.9 5.8

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MH, lb.-in. 39.9 35.2 39.7 39.4


Ts2, minutes 4.3 5.0 4.2 4.0
T50, minutes 6.6 7.5 7.3 6.7
T90, minutes 7.7 8.8 8.6 7.7
Cured at 160[degrees]C, minutes 13.0 14.0 15.0 13.0
Tensile strength, Mpa 26.6 25.4 25.2 26.4
Elongation at break, % 532.0 549.0 541.0 544.0
M 100, MPa 2.4 2.1 2.2 2.2
M 300, MPa 12.4 10.9 11.0 12.0
Hardness, A 64.0 63.0 61.0 62.0
DIN abrasion index
Average of 3 samples 104.9 89.8 101.4 105.4
RPA test at 10 Hz and 60[degrees]C
Tangent S PtP Strain, %
1.5 0.051 0.057 0.055 0.056
2 0.065 0.069 0.067 0.055
4 0.079 0.083 0.081 0.080
10 0.101 0.104 0.104 0.097
G', MPa PtP Strain, %
1.5 3.1 2.5 3.1 3.0
2 3.0 2.4 2.9 2.9
4 2.7 2.2 2.6 2.6
10 2.3 1.9 2.2 2.2

Compound W X Y Z

Natural rubber 100.0 100.0 100.0 100.0


N-220 carbon black 5.0 5.0 5.0 5.0
Precipitated silica 60.0 60.0 60.0 60.0
Aromatic oil 7.0 7.0 7.0 7.0
TESPT Silane 3.6 3.6 3.6 3.6

2nd pass
Activator 1 0.00 0.00 0.00 0.00
Component A 0.55 0.55 0.35 0.55
Component B 0.68 0.20 0.44 0.20
Component C 1.60 1.60 0.89 0.17
Zinc oxide 3.0 3.0 3.0 3.0
Flexzone 7P 2.0 2.0 2.0 2.0
Industrene R 2.0 2.0 2.0 2.0
Sunproof improved 1.5 1.5 1.5 1.5

Final pass for all. 1.00 Delac NS; 0.40 Royalac 150; 0.20 CTP retarder;
2.25 sulfur

Mooney at 135[degrees]C
Scorch, MS t3, min. 14 22 23 24
Rheometer at 160[degrees]C
ML, lb.-in. 5.5 5.4 5.6 5.5
MH, lb.-in. 41.0 36.1 34.2 32.8
Ts2, minutes 3.8 4.9 5.1 5.3
T50, minutes 6.4 7.9 7.6 7.8
T90, minutes 7.4 9.2 8.8 9.2
Cured at 160[degrees]C, minutes 13.0 14.0 14.0 14.0
Tensile strength, Mpa 26.1 25.2 24.0 25.0
Elongation at break, % 502.0 532.0 554.0 552.0
M 100, MPa 2.5 2.1 1.9 2.0
M 300, MPa 13.1 11.3 10.2 10.4
Hardness, A 62.0 62.0 62.0 62.0

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DIN abrasion index


Average of 3 samples 106.9 95.0 96.8 75.0
RPA test at 10 Hz and 60[degrees]C
Tangent S PtP Strain, %
1.5 0.045 0.056 0.055 0.057
2 0.052 0.063 0.070 0.070
4 0.064 0.083 0.083 0.091
10 0.084 0.102 0.107 0.114
G', MPa PtP Strain, %
1.5 2.7 2.6 2.4 2.6
2 2.7 2.5 2.3 2.5
4 2.4 2.3 2.1 2.2
10 2.1 1.9 1.8 1.9

Compound AA AB

Natural rubber 100.0 100.0


N-220 carbon black 5.0 5.0
Precipitated silica 60.0 60.0
Aromatic oil 7.0 7.0
TESPT Silane 3.6 3.6

2nd pass
Activator 1 0.00 0.00
Component A 0.15 0.15
Component B 0.68 0.68
Component C 0.17 1.60
Zinc oxide 3.0 3.0
Flexzone 7P 2.0 2.0
Industrene R 2.0 2.0
Sunproof improved 1.5 1.5

Final pass for all. 1.00 Delac NS; 0.40 Royalac 150; 0.20 CTP retarder;
2.25 sulfur

Mooney at 135[degrees]C
Scorch, MS t3, min. 16 13
Rheometer at 160[degrees]C
ML, lb.-in. 6.1 5.6
MH, lb.-in. 37.7 40.5
Ts2, minutes 4.0 3.4
T50, minutes 6.2 5.8
T90, minutes 7.2 6.7
Cured at 160[degrees]C, minutes 12.0 12.0
Tensile strength, Mpa 25.1 22.8
Elongation at break, % 513.0 570.0
M 100, MPa 2.1 1.7
M 300, MPa 11.8 9.1
Hardness, A 62.0 62.0
DIN abrasion index
Average of 3 samples 99.0 116.8
RPA test at 10 Hz and 60[degrees]C
Tangent S PtP Strain, %
1.5 0.055 0.046
2 0.058 0.057
4 0.074 0.075
10 0.097 0.093
G', MPa PtP Strain, %
1.5 2.9 3.0

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2 2.8 2.9
4 2.5 2.6
10 2.2 2.3

Table 6--regression analysis for activator component effects

Component

Constant A B

t3 at 135[degrees]C 25.6 1.0 * -14.6 (b)


P value 0.77 0.00
t90 at 160[degrees]C 9.18 1.27 (b) -2.75 (a)
P value 0.01 0.00
RPA tan [delta] - 4% 0.100 -0.020 (a) -0.028 (a)
P value 0.04 0.00
RPA tan [delta] - 10% 0.125 -0.020 (a) -0.028 (a)
P value 0.02 0.00
DIN abr. index 93.4 -34.9 (b) 18.6 (a)
P value 0.01 0.05

Component

C [R.sup.2]

t3 at 135[degrees]C 0.0 * 73.3


P value 0.63
t90 at 160[degrees]C -0.50 (a) 78.9
P value 0.07
RPA tan [delta] - 4% -0.005 62.9
P value 0.36
RPA tan [delta] - 10% -0.007 (a) 71.7
P value 0.09
DIN abr. index 10.3 (a) 89.0
P value 0.01

Color code for above: (a) Green = good, (b) Blue = bad

* Strikethrough = Not significant, P>0.5, due to random


chance more than 50% of time.

** Bold = Highly significant, P<0.01, due to random change


less than 1% of time.

Table 7--testing of compounds for tire tests

Compound AC AD AE

Natural rubber 100.0 100.0 100.0


N-220 carbon black 59.0 5.0 5.0
Precipitated silica - 60.0 60.0
Aromatic oil 7.0 7.0 7.0
TESPT silane polysulfide - 4.8 4.8

2nd pass
Activator 1 - 2.5 -
Activator 2 - - 2.1
Zinc oxide 3.0 3.0 3.0
Flexzone 7P antiozonant 2.0 2.0 2.0

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Industrene R stearic acid 2.0 2.0 2.0


Sunproof improved wax 1.5 1.5 1.5

Final pass
Delac NS 1.0 1.0 1.0
Royalac 150 - 0.6 0.6
CTP retarder 0.2 0.2 0.2
Sulfur 2.0 2.3 2.3

Mooney at 100[degrees]C
Viscosity, ML 1+4 54.0 83.0 87.0

Mooney at 135[degrees]C
Scorch, MS t3, minutes 18.3 5.5 9.1

Rheometer at 160[degrees]C
ML, lb.-in. 7.2 9.5 8.2
MH, lb.-in. 39.3 44.8 45.1
Ts2, minutes 4.2 2.2 2.9
T50, minutes 6.1 3.8 4.8
T90, minutes 7.7 5.9 6.9
Cured at 160[degrees]C, minutes 10.0 8.0 9.0
Tensile strength, MPa 26.2 26.9 26.6
Elongation at break, % 506.0 516.0 510.0
M 100, MPa 2.7 3.1 3.4
M 300, MPa 13.9 14.6 14.7
Hardness, A 65.0 65.0 65.0

Aged 2 weeks at 70[degrees]C


Tensile strength, MPa 27.0 25.2 23.4
Elongation at break, % 405.0 414.0 380.0
M100, MPa 4.6 4.9 5.2
M300, MPa 20.1 19.2 19.2
Hardness, A 72.0 72.0 74.0
DIN abrasion index 105.6 105.1 99.3

COPYRIGHT 2006 Lippincott & Peto, Inc.


No portion of this article can be reproduced without the express written permission from the copyright holder.
Copyright 2006, Gale Group. All rights reserved. Gale Group is a Thomson Corporation Company.

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