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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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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.
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.
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.
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.
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]
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:
Based on the fastest wearing groove from on-tire fleet trials, the projected distance to wear-out
showed:
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.
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.
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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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
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
Compound E F G H
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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Compound I J K
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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
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Compound L M
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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Compound N O P
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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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
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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Compound Q R
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
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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
Compound S T U V
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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Compound W X Y Z
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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Compound AA AB
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
Component
Constant A B
Component
C [R.sup.2]
Color code for above: (a) Green = good, (b) Blue = bad
Compound AC AD AE
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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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
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