JP2006225473A - Rubber composition for tire and pneumatic tire using the same - Google Patents
Rubber composition for tire and pneumatic tire using the same Download PDFInfo
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本発明はタイヤ用ゴム組成物に関し、更に詳しくは空気入りタイヤのインナーライナーとして有用なブチルゴム又はブチルゴムとジエン系ゴムとのブレンドを含む、耐空気透過性に優れたゴム組成物及びそれを用いた空気入りタイヤに関する。 The present invention relates to a rubber composition for tires, and more specifically, a rubber composition excellent in air permeation resistance, including butyl rubber or a blend of butyl rubber and diene rubber, which is useful as an inner liner of a pneumatic tire, and the same. Related to pneumatic tires.
空気入りタイヤのインナーライナーには、耐空気透過性を良くするため空気保持性に優れたブチルゴムもしくはハロゲン化ブチルゴム又はそれを含むブレンドゴムが用いられ、さらに強度を付与するためにカーボンブラックが共に用いられるが、ここで粒径の小さいカーボンブラックを用いたり、カーボンブラックの配合量を多量に配合すると耐屈曲疲労性が低下するおそれがあり、ＦＥＦグレードなどの粒径の大きなカーボンブラックが適当量配合されている。そこで耐空気透過性を更に改良すべくクレー、マイカ、ベントナイトなどを配合したインナーライナーに関する発明が提案されている（特許文献１及び２参照）。しかしながら、これらの無機充填剤を配合すると、ゴム組成物の比重が増大して、タイヤ重量の増大を惹き起こし、省燃費性に反することとなるという問題がある。 For the inner liner of pneumatic tires, butyl rubber or halogenated butyl rubber with excellent air retention to improve air permeation resistance or blended rubber containing it is used, and carbon black is used together to add strength. However, if carbon black with a small particle size is used here or a large amount of carbon black is blended, there is a risk that the bending fatigue resistance may be lowered. Carbon black with a large particle size such as FEF grade is blended in an appropriate amount. Has been. In view of this, there has been proposed an invention relating to an inner liner blended with clay, mica, bentonite or the like in order to further improve the air permeation resistance (see Patent Documents 1 and 2). However, when these inorganic fillers are blended, there is a problem that the specific gravity of the rubber composition increases, causing an increase in tire weight, which is contrary to fuel saving.
従って、本発明の目的は、比重を増大させることなく、耐空気透過性を改良するゴム組成物及びそれをインナーライナーに用いた空気入りタイヤを提供することにある。 Accordingly, an object of the present invention is to provide a rubber composition that improves air permeation resistance without increasing the specific gravity, and a pneumatic tire using the rubber composition as an inner liner.
本発明に従えば、ブチル系ゴム又はブチル系ゴムとジエン系ゴムとのブレンドを含むゴム成分１００重量部及び混合時に熱膨張する熱膨張性黒鉛１〜１０重量部を含んでなるゴム組成物並びにそれをインナーライナーに用いた空気入りタイヤが提供される。 According to the present invention, a rubber composition comprising 100 parts by weight of a rubber component including a butyl rubber or a blend of a butyl rubber and a diene rubber, and 1 to 10 parts by weight of thermally expandable graphite that thermally expands upon mixing; A pneumatic tire using the inner liner is provided.
本発明によれば、ブチル系ゴム又はブチル系ゴムとジエン系ゴムとのブレンド１００重量部に対し、混合時（例えば１５０℃〜１９０℃）に熱膨張する熱膨張性黒鉛１〜１０重量部を配合することにより、比重を増大させることなく、耐空気透過性を増大させることができる。 According to the present invention, with respect to 100 parts by weight of butyl rubber or a blend of butyl rubber and diene rubber, 1 to 10 parts by weight of thermally expandable graphite that thermally expands when mixed (for example, 150 ° C. to 190 ° C.). By blending, the air permeation resistance can be increased without increasing the specific gravity.
本発明者は、前記問題を解決すべく、鋭意研究をすすめた結果、混合時の温度で熱膨張する熱膨張性黒鉛を配合することで、少量の配合量で熱膨張性黒鉛が膨張してゴム中に層状に存在するため、比重の増大を惹き起こすことなく、耐空気透過性を大きく向上させることができることを見出した。 As a result of intensive studies to solve the above problems, the present inventor, by adding thermally expandable graphite that thermally expands at the temperature at the time of mixing, expands the thermally expandable graphite with a small amount. It has been found that air permeation resistance can be greatly improved without causing an increase in specific gravity because it exists in a layered manner in rubber.
本発明において使用するゴム成分はブチル系ゴム単独もしくはブチル系ゴムとジエン系ゴムとのブレンドを用いることができる。ブチル系ゴムとしてはインナーライナー用として使用されている任意のブチル系ゴム、例えばブチルゴムや臭化ブチルゴムなどのハロゲン化ブチルゴムを用いることができ、具体的にはエクソンモービル社より市販のブロモブチル２２５５などを用いることができる。 The rubber component used in the present invention can be a butyl rubber alone or a blend of a butyl rubber and a diene rubber. As the butyl rubber, any butyl rubber used for the inner liner, for example, halogenated butyl rubber such as butyl rubber and butyl bromide rubber can be used. Specifically, for example, bromobutyl 2255 commercially available from ExxonMobil Corp. Can be used.
ブチル系ゴムと併用することができるジエン系ゴムとしては、例えば各種天然ゴム（ＮＲ）、各種ポリイソプレンゴム（ＩＲ）、各種ポリブタジエンゴム（ＢＲ）、各種スチレン−ブタジエン共重合体ゴム（ＳＢＲ）、エチレン−プロピレン−ジエンゴム（ＥＰＤＭ）などをあげることができる。ブチル系ゴムとジエンゴムとのブレンド比には特に限定はないが、ブレンドゴム中の６０重量％以上がブチル系ゴムであるのが好ましい。 Examples of diene rubbers that can be used in combination with butyl rubber include, for example, various natural rubbers (NR), various polyisoprene rubbers (IR), various polybutadiene rubbers (BR), various styrene-butadiene copolymer rubbers (SBR), Examples thereof include ethylene-propylene-diene rubber (EPDM). The blend ratio of butyl rubber and diene rubber is not particularly limited, but 60% by weight or more in the blend rubber is preferably butyl rubber.
本発明によれば、熱膨張性黒鉛を配合することで、インナーライナー用ゴム組成物の混合時に膨張し、混練により層状に配置されることで、クレー、マイカ等の配合と同様に耐空気透過性の改善を図ることができると共に、クレー、マイカや予じめ膨張化処理された黒鉛（膨張化処理黒鉛）等の使用の場合のような比重の増大がない。また膨張により体積が増えるため、膨張化処理黒鉛の配合に比し、配合量が大幅に少なくてすむ。熱膨張性黒鉛の配合量が少ないと耐空気透過性の改善が見られないので好ましくなく、逆に配合量が多いと、耐空気透過性は向上するものの、比重が増大するので好ましくない。 According to the present invention, by adding thermally expandable graphite, it expands when the rubber composition for the inner liner is mixed, and is arranged in layers by kneading, so that air permeation resistance is the same as that of clay, mica, etc. In addition, the specific gravity can be improved, and there is no increase in specific gravity as in the case of using clay, mica or pre-expanded graphite (expanded graphite). Further, since the volume increases due to expansion, the amount of the compound can be greatly reduced as compared with the compounding of the expanded graphite. If the blending amount of the heat-expandable graphite is small, it is not preferable because the improvement of the air permeation resistance is not seen. Conversely, if the blending amount is large, the air permeation resistance is improved, but the specific gravity increases.
本発明において使用する熱膨張性黒鉛は、ブチル系ゴム又はブチル系ゴムとジエン系ゴムとのブレンドゴム１００重量部に対し、１〜１０重量部、好ましくは３〜１０重量部配合する。この配合量が少な過ぎると所望の効果が得られないので好ましくなく、逆に多過ぎると比重が増大するので好ましくない。
本発明において使用する膨張黒鉛（Ｅｘｐａｎｄａｂｌｅ）は黒鉛粒子の層間に熱により気化する物質を内包する粒子サイズ３０〜６００μｍ、好ましくは１００〜３５０μｍの粉体物質であり、混合時の熱によって膨張して黒鉛膨張体（Ｅｘｐａｎｄｅｄ Ｇｒａｐｈｉｔｅ）となる。膨張黒鉛は炭素原子から形成されたシートが層状に重なった構造をしており、硫酸や硝酸などとともに酸処理（インターカレーション処理）することによって得られる。この膨張黒鉛は例えば加熱によりその層間物質の気化によって高膨張させて黒鉛膨張体（又は発泡黒鉛）とすることができる。
The thermally expandable graphite used in the present invention is blended in an amount of 1 to 10 parts by weight, preferably 3 to 10 parts by weight, based on 100 parts by weight of butyl rubber or blend rubber of butyl rubber and diene rubber. If the blending amount is too small, the desired effect cannot be obtained.
Expandable graphite (Expandable) used in the present invention is a powder substance having a particle size of 30 to 600 μm, preferably 100 to 350 μm, which encloses a substance that is vaporized by heat between graphite particles, and expands by heat during mixing. It becomes a graphite expanded body (Expanded Graphite). Expanded graphite has a structure in which sheets formed from carbon atoms are stacked in layers, and is obtained by acid treatment (intercalation treatment) together with sulfuric acid, nitric acid and the like. The expanded graphite can be made into a graphite expanded body (or expanded graphite) by, for example, being highly expanded by heating and vaporizing the interlayer material.
膨張黒鉛は既に公知の材料であり、公知の製法によって製造される。一般的には強酸物質と酸化剤との混合液に黒鉛粒子を浸漬し、インターカレーション処理により黒鉛粒子の層間に酸を挿入させて製造する。例えば強酸物質としては濃硫酸、酸化剤として硝酸が使われ、これにより粒子の層間に硫酸が挿入された膨張黒鉛が得られる。膨張黒鉛は熱処理によって層間化合物が揮発することによって層間が開き、膨張する。層間物質に硫酸が用いられる膨張黒鉛は通常３００℃以上での熱処理によって膨張するが、層間物質の改質や他の低沸点酸化合物（例えば硝酸）の使用又は併用によって、膨張開始温度を３００℃以下に下げた膨張黒鉛が製造、市販されている。本発明では混合時に膨張させることから、本発明では膨張開始温度が１５０〜１９０℃の膨張黒鉛を用いるのが好ましい。このような膨張開始温度の膨張黒鉛としては、例えば巴工業（株）よりグラフガード１６０−５０などとして市販されているものを使用することができる。なお、膨張黒鉛は用語的には酸処理を行った直後の未膨張品（Ｅｘｐａｎｄａｂｌｅ）を示すが、熱処理後の既膨張品（Ｅｘｐａｎｄｅｄ）のことを呼ぶ場合もある。本発明にてゴム組成物として配合される膨張黒鉛は熱処理前の未膨張品である。本発明においては、膨張黒鉛を熱膨張性黒鉛と称し、これは前述のようにゴム組成物の混合工程にて膨張させることから、膨張開始温度がより好ましくは１５０〜１８０℃、更に好ましくは１５０〜１７０℃のものが用いられる。膨張開始温度が低過ぎると、熱膨張性黒鉛が混合時に、早期に膨張するため、混合により層状となった黒鉛が細片化するおそれがある。また、膨張開始温度が高過ぎる場合には混合工程時に膨張しないので好ましくない。 Expanded graphite is a known material and is produced by a known production method. In general, the graphite particles are immersed in a mixed solution of a strong acid substance and an oxidizing agent, and an acid is inserted between the layers of the graphite particles by an intercalation treatment. For example, concentrated sulfuric acid is used as a strong acid substance, and nitric acid is used as an oxidizing agent, thereby obtaining expanded graphite in which sulfuric acid is inserted between the particles. Expanded graphite expands when the interlayer opens when the interlayer compound volatilizes by heat treatment. Expanded graphite in which sulfuric acid is used as an interlayer material usually expands by heat treatment at 300 ° C. or higher. However, the expansion start temperature is set to 300 ° C. by modifying the interlayer material or using other low-boiling acid compounds (for example, nitric acid). Expanded graphite lowered to the following is manufactured and marketed. In the present invention, the expanded graphite is expanded at the time of mixing. Therefore, in the present invention, it is preferable to use expanded graphite having an expansion start temperature of 150 to 190 ° C. As the expanded graphite having such an expansion start temperature, for example, a commercially available graph guard 160-50 from Sakai Kogyo Co., Ltd. can be used. In addition, the expanded graphite is a terminology indicating an unexpanded product (Expandable) immediately after the acid treatment, but it may be called an expanded product after the heat treatment. The expanded graphite blended as a rubber composition in the present invention is an unexpanded product before heat treatment. In the present invention, the expanded graphite is referred to as thermally expandable graphite, and since it is expanded in the mixing step of the rubber composition as described above, the expansion start temperature is more preferably 150 to 180 ° C., further preferably 150. The one of ˜170 ° C. is used. If the expansion start temperature is too low, the heat-expandable graphite expands early at the time of mixing, and there is a possibility that the graphite layered by mixing may be fragmented. In addition, when the expansion start temperature is too high, the expansion does not occur during the mixing step, which is not preferable.
本発明に係るゴム組成物には、好ましくはＦＥＦ級、ＧＰＦ級もしくはＳＲＦ級などのカーボンブラックを配合することができ、その配合量は従前通りであり、例えばゴム分１００重量部に対し、３０〜７０重量部配合する。 In the rubber composition according to the present invention, carbon black such as FEF grade, GPF grade or SRF grade can be preferably blended, and the blending amount is as usual, for example, 30 parts by weight with respect to 100 parts by weight of rubber. -70 weight part is mix | blended.
本発明に係るゴム組成物には、前記した成分に加えて、シリカなどのその他の補強剤（フィラー）、加硫又は架橋剤、加硫又は架橋促進剤、各種オイル、老化防止剤、可塑剤などのタイヤ用、その他一般ゴム用に一般的に配合されている各種添加剤を配合することができ、かかる添加剤は一般的な方法で混合して組成物とし、加硫又は架橋するのに使用することができる。これらの添加剤の配合量は本発明の目的に反しない限り、従来の一般的な配合量とすることができる。 In addition to the components described above, the rubber composition according to the present invention includes other reinforcing agents (fillers) such as silica, vulcanization or crosslinking agents, vulcanization or crosslinking accelerators, various oils, antiaging agents, and plasticizers. Various additives that are generally blended for tires and other general rubbers can be blended, and such additives are mixed by a general method to form a composition for vulcanization or crosslinking. Can be used. The blending amounts of these additives may be conventional conventional blending amounts as long as the object of the present invention is not adversely affected.
以下、実施例によって本発明を更に説明するが、本発明の範囲をこれらの実施例に限定するものでないことはいうまでもない。 EXAMPLES Hereinafter, although an Example demonstrates this invention further, it cannot be overemphasized that the scope of the present invention is not limited to these Examples.
実施例１〜３及び比較例１〜４
サンプルの調製
表Ｉに示す配合において、加硫促進剤と硫黄を除く成分を２リットルの密閉型ミキサーで５分間混練し、１６５±５℃に達したときに放出してマスターバッチを得た。このマスターバッチに加硫促進剤と硫黄をオープンロールで混練し、ゴム組成物を得た。
Examples 1-3 and Comparative Examples 1-4
Sample preparation In the formulation shown in Table I, the components other than the vulcanization accelerator and sulfur were kneaded for 5 minutes with a 2 liter closed mixer and released when the temperature reached 165 ± 5 ° C to obtain a master batch. A vulcanization accelerator and sulfur were kneaded with this master batch with an open roll to obtain a rubber composition.
次に得られたゴム組成物を１５×１５×０．２cmの金型中で１７５℃で１０分間加硫して加硫ゴムシートを調製し、以下に示す試験法で加硫ゴムの比重及び耐空気透過性を測定した。結果は表Ｉに示す。なお、結果は比較例１の値を１００として指数表示した。比重は数が小さい方が燃費性に優れ、耐空気透過性は値が大きい方が良好なことを示す。 Next, the rubber composition thus obtained was vulcanized in a 15 × 15 × 0.2 cm mold at 175 ° C. for 10 minutes to prepare a vulcanized rubber sheet. The air permeation resistance was measured. The results are shown in Table I. The results are shown as an index with the value of Comparative Example 1 being 100. A smaller specific gravity indicates better fuel efficiency, and a higher value for air permeation resistance indicates better.
ゴム物性評価試験法
比重：ＪＩＳ Ｋ６２６８に準拠して測定した。
耐空気透過性：ＪＩＳ Ｋ７１２６に準拠して測定した（試験気体：空気（Ｎ2：Ｏ2＝８：２）、試験温度：３０℃）。
Rubber physical property evaluation test method Specific gravity: Measured according to JIS K6268.
Air permeation resistance: Measured according to JIS K7126 (test gas: air (N 2 : O 2 = 8: 2), test temperature: 30 ° C.).
表Ｉ脚注
＊１：エクソンモービル社製ブロモブチル２２５５
＊２：東海カーボン（株）製シーストＶ
＊３：Ｈｕｂｅｒ社製Ｐｏｌｙｆｉｌｅ ＤＬ
＊４：中越黒鉛工業所（株）製ＢＳＰ−６００（熱膨張完了品）
＊５：巴工業（株）製グラフガード１００−１５０（膨張温度１６０℃）
＊６：日本油脂（株）製ビーズステアリン酸
＊７：正同化学工業（株）製酸化亜鉛３種
＊８：昭和シェル石油（株）製デソレックス３号
＊９：鶴見化学工業（株）製油処理イオウ
＊１０：大内新興化学工業（株）製加硫促進剤ノクセラーＣＺ−Ｇ
Table I footnote * 1: Bromobutyl 2255 manufactured by ExxonMobil
* 2: Toast Carbon Co., Ltd. Seest V
* 3: Huber Polyfile DL
* 4: BSP-600 (completion of thermal expansion) manufactured by Chuetsu Graphite Industry Co., Ltd.
* 5: Graph guard 100-150 manufactured by Sakai Kogyo Co., Ltd. (expansion temperature 160 ° C.)
* 6: Beads stearic acid manufactured by Nippon Oil & Fats Co., Ltd. * 7: Three types of zinc oxide manufactured by Shodo Chemical Industry Co., Ltd. * 8: Desolex No. 3 manufactured by Showa Shell Sekiyu K.K. * 9: Oil manufactured by Tsurumi Chemical Industry Co., Ltd. Treated sulfur * 10: Ouchi Shinsei Chemical Co., Ltd. vulcanization accelerator Noxeller CZ-G
以上の通り、本発明によれば、ブチルゴムを含むゴム組成物に混合時に熱膨張する熱膨張性黒鉛を所定量配合することにより、比重の増大を伴なうことなく、耐空気透過性を大きく向上させることができるので空気入りタイヤのインナーライナーとして使用するのに好適である。 As described above, according to the present invention, a predetermined amount of thermally expandable graphite that thermally expands when mixed with a rubber composition containing butyl rubber increases the air permeation resistance without increasing the specific gravity. Since it can improve, it is suitable for using as an inner liner of a pneumatic tire.
Claims (4)
A pneumatic tire using the rubber composition according to claim 1 as an inner liner.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1967543A1 (en) * | 2007-03-06 | 2008-09-10 | Sumitomo Rubber Industries, Ltd. | Rubber composition for inner liner |
| JP2008280366A (en) * | 2007-05-08 | 2008-11-20 | Mitsubishi Cable Ind Ltd | Manufacturing method for rubber molded article, and sealing member manufactured by the method |
| US7659350B2 (en) | 2005-10-14 | 2010-02-09 | The Trustees Of Princeton University | Polymerization method for formation of thermally exfoliated graphite oxide containing polymer |
| US7745528B2 (en) | 2006-10-06 | 2010-06-29 | The Trustees Of Princeton University | Functional graphene-rubber nanocomposites |
| US8110026B2 (en) | 2006-10-06 | 2012-02-07 | The Trustees Of Princeton University | Functional graphene-polymer nanocomposites for gas barrier applications |
| WO2019221918A1 (en) * | 2018-05-14 | 2019-11-21 | Exxonmobil Chemical Patents Inc. | Expandable thermoplastic microsphere doped tire innerliner |
| JP2020193324A (en) * | 2019-05-28 | 2020-12-03 | 株式会社レグルス | Resin composition, thermo-expansive product, and method for producing resin composition |
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2005
- 2005-02-16 JP JP2005039311A patent/JP2006225473A/en active Pending
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| JP2008280366A (en) * | 2007-05-08 | 2008-11-20 | Mitsubishi Cable Ind Ltd | Manufacturing method for rubber molded article, and sealing member manufactured by the method |
| WO2019221918A1 (en) * | 2018-05-14 | 2019-11-21 | Exxonmobil Chemical Patents Inc. | Expandable thermoplastic microsphere doped tire innerliner |
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