Rubber composition containing modified conjugated diene-based polymer bonded to fullerene
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Example 1 and Comparative Examples 1 to 4
[0018] In each formulation shown in Table I (parts by weight), the components other than the vulcanization accelerator and sulfur were mixed by a 0.25 liter internal mixer for 3 to 5 minutes to obtain a master batch, which was then mixed with the vulcanization accelerator and sulfur by an 8-inch open roll to obtain a rubber composition. This composition was press vulcanized in a 15×15×0.2 cm mold at 160° C. for 20 minutes to obtain a rubber sheet.
[0019] Each vulcanized rubber sheet obtained above was evaluated by the following method.
[0020] 300% modulus (MPa): Measured according to JIS K6301
[0021] tan δ (60° C.): Value measured using viscoelasticity spectrometer (Toyo Seiki) at a temperature of 60° C. under conditions of an initial strain of 10%, a dynamic strain of ±2%, and a frequency of 20 Hz. Note that when considering tread rubber for a tire, the lower this value, the smaller the rolling resistance and therefore the smaller the heat ...
Example
Example 2 and Comparative Examples 5 to 7
[0037] In each formulation shown in Table II (parts by weight), the components other than the vulcanization accelerator and sulfur were mixed in a 0.25 liter internal mixer for 3 to 5 minutes to obtain a master batch, which was then mixed with the vulcanization accelerator and sulfur by an 8-inch open roll to obtain a rubber composition. This composition was press vulcanized in a 15×15×0.2 cm mold at 160° C. for 20 minutes to obtain a rubber sheet.
[0038] Each vulcanized rubber sheet obtained above was evaluated by the following method.
[0039] Viscoelasticity: tan δ (60° C.) and tan δ (0° C.) values measured using a viscoelasticity spectrometer (Toyo Seiki) at temperatures of 60° C. and 0° C. under conditions of an initial strain of 10%, a dynamic strain of ±2% and a frequency of 20 Hz and the ratio of the same.
[0040] Note that the lower the value of the tan δ (60° C.), the smaller the rolling resistance, therefore the smaller the heat buil...
Example
[0042] Synthesis Example
[0043] Note that the reagents used in the following Synthesis Examples were as follows:
[0044] Cyclohexane, Styrene: Made by Kanto Chemical, dehydrated by Molecular Sieve 4A, and bubbled with nitrogen.
[0045] Butadiene: Made by Japan Petrochemical, purity 99.3%, dehydrated by Molecular Sieve 4A.
[0046] n-Butyl lithium: Made by Kanto Chemical, n-hexane solution 1.58 mol / liter.
[0047] N,N,N′,N′-Tetramethylethyl diamine (TMEDA): Dehydrated by Molecular Sieve 4A and bubbled with nitrogen.
[0048] Toluene: Made by Kanto Chemical, refluxed in the presence of metal sodium for about 1 week, checked for deep blue color of benzophenoneketyl (i.e., indicator of dehydration), then distilled.
[0049] Fullerene: Tokyo Kasei C60>99.9% fullerene dehydrated and dried.
[0050] Synthesis of Unmodified SBR (SBR-NF)
[0051] A nitrogen-substituted 10-liter autoclave reactor was charged with 3138 g of cyclohexane, 115.6 g (1.110 mol) of styrene, 438.9 g of butadiene (8.172 mol) and 1....
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