Cycloolefin-based rubber and process for producing same, rubber composition, crosslinked rubber object, and tire
A technology of cyclic olefin and manufacturing method, which is applied in the field of rubber cross-linked products, tires, rubber for tire materials, and cyclic olefin-based rubber, can solve the problem of inability to cope with low fuel consumption, inability to match, and deterioration of tire physical properties And other issues
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[0125] Hereinafter, the present invention will be further described based on detailed examples, but the present invention is not limited to these examples. In addition, the following "parts" are based on weight unless otherwise specified. In addition, experiments and evaluations are as follows.
[0126]
[0127] Gel permeation chromatography (GPC) system HLC-8220 (manufactured by Tosoh Co.) and H-type column HZ-M (manufactured by Tosoh Co.) were used to measure tetrahydrofuran as a solvent at 40 ° C. The weight of the cyclic olefin rubber Average molecular weight (Mw) and molecular weight distribution (Mw / Mn) were measured as polystyrene conversion values.
[0128]
[0129] by deuterated chloroform solution of cyclic olefin rubber 1 H-NMR spectrum measurement was used to measure the ratio of the peak integral value unique to silyl groups and the peak integral value derived from olefins. Then, the ratio of terminal silyl groups introduced into the polymer chain of the cy...
reference example 1
[0142] (Reference example 1) Preparation of diisobutyl mono(n-hexyloxy)aluminum / toluene solution (2.5% by weight)
[0143] In a nitrogen atmosphere, 88 parts of toluene and 7.8 parts of a 25.4% by weight triisobutylaluminum / n-hexane solution (manufactured by Tosoh Finechem) were added to a glass container with a stirrer. Cool to -45°C, and slowly add 1.02 parts of n-hexanol (equal molar amount to triisobutylaluminum) dropwise while vigorously stirring. Thereafter, it was left to stand at room temperature while stirring to prepare a diisobutylmono(n-hexyloxy)aluminum / toluene solution (2.5% by weight).
manufacture example 1
[0144] (Production Example 1) Production of terminal silane-modified cyclic olefin polymer solution (A-1)
[0145] Under nitrogen atmosphere, 435 parts of 1.0 wt% WCl 6 / toluene solution and 215 parts of 2.5% by weight of diisobutyl mono(n-hexyloxy)aluminum / toluene solution prepared in Reference Example 1 were added in a pressure-resistant reaction vessel with a stirrer, and stirred for 15 minutes, thereby A catalyst solution was obtained. Then, under a nitrogen atmosphere, 1500 parts of cyclopentene as a monocyclic olefin and 5.4 parts of bis(triethoxysilyl)ethylene were added to a pressure-resistant glass reaction vessel with a stirrer, where 650 parts of the catalyst solution prepared above were subjected to a polymerization reaction at 25° C. for 4 hours. After 4 hours of polymerization reaction, excess ethanol was added to the pressure-resistant reaction container to terminate the polymerization, and a terminal silane-modified cyclic olefin polymer solution (A-1) was ob...
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Abstract
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