JP2007186567A - Rubber composition for tread of tire - Google Patents
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Abstract
Description
本発明は、タイヤトレッド用ゴム組成物に関し、更に詳細には、低燃費性を損なうことなく、ドライおよびウェット操縦安定性、低温性能、並びに加工性を向上させたタイヤトレッド用ゴム組成物に関する。 The present invention relates to a rubber composition for a tire tread, and more particularly, to a rubber composition for a tire tread having improved dry and wet handling stability, low temperature performance, and processability without impairing low fuel consumption.
今日、シリカ多量配合系ゴムのキャップコンパウンドについては、低燃費性と降雨時の安全性(ウェット性能)を両立する技術として位置付けられ、タイヤメーカー各社において様々な研究がなされているが、シリカ配合時の基本的な問題点として、ドライ性能の低下とシリカの再凝集性による加工性の低下を挙げることができる。また、最近では、環境保全上の観点から、従来、タイヤゴムの可塑剤として一般に用いられてきた石油系アロマオイルのタイヤ摩耗に伴う大気中への飛散の問題も指摘されている。 Today, silica compound rubber compound is positioned as a technology that achieves both low fuel consumption and rain safety (wet performance), and various researches have been conducted by tire manufacturers. As basic problems, there are a decrease in dry performance and a decrease in workability due to re-aggregation of silica. In addition, recently, from the viewpoint of environmental protection, the problem of scattering of petroleum-based aroma oil, which has been conventionally used as a plasticizer for tire rubber, into the atmosphere accompanying tire wear has been pointed out.
従来、耐摩耗性を高レベルに維持しながら、氷結路面および積雪路面でのグリップ性を高めたスタッドレスタイヤ用のゴム組成物において、ジエン系ゴムに対して樹脂パウダー、ポリノルボルネンエラストマーおよびテルペン樹脂を配合する技術が、以下の特許文献1に開示され、また、雪上や氷上、濡れた路面に対するグリップ性を高めたタイヤトレッド用ゴム組成物において、ジエン系ゴムに対して軟化剤含有ノルボルネン系重合体および粘着付与剤としてのテルペン樹脂又はロジンエステルを配合する技術が、以下の特許文献2に開示され、更に、ブチル系ゴムの強度を高めることによってウェットグリップ性能と耐摩耗性を両立させたタイヤトレッド用ゴム組成物において、SBR等のジエン系ゴムに対して、テルペン樹脂やロジン樹脂等の樹脂を配合する技術が、以下の特許文献3に開示されている。 Conventionally, a rubber composition for studless tires with improved wear resistance on ice and snowy road surfaces while maintaining wear resistance at a high level, resin powder, polynorbornene elastomer and terpene resin are added to diene rubber. A compounding technique is disclosed in the following Patent Document 1, and a rubber composition for a tire tread having improved grip properties on snow, on ice, or a wet road surface, and a softening agent-containing norbornene polymer in a diene rubber And a technique for blending a terpene resin or rosin ester as a tackifier is disclosed in the following Patent Document 2, and further, the tire tread that achieves both wet grip performance and wear resistance by increasing the strength of the butyl rubber. Terpene resin and rosin for diene rubber such as SBR Art of compounding resin butter, and the like is disclosed in Patent Document 3 below.
また、前述した上記第一の問題点に関連して、加工性とグリップ性能の双方に優れるタイヤトレッドゴム組成物を得るために、軟化点80〜160℃のテルペン系樹脂を10〜150重量部の量でジエン系ゴムに配合する先行技術は、以下の特許文献4に開示され、また、上記第一および第二の問題点に関連して、加工性と低転がり抵抗とに優れるタイヤトレッドゴム組成物を得るために、非石油系で高ガラス転位温度(Tg)のグリセロール脂肪酸トリエステルをベースに、必要に応じて少量の植物油を更に含む可塑剤を、多量シリカ配合系ジエン系ゴム組成物に所定量配合する先行技術は、以下の特許文献5に開示されている。 Further, in order to obtain a tire tread rubber composition excellent in both workability and grip performance in relation to the first problem described above, 10 to 150 parts by weight of a terpene resin having a softening point of 80 to 160 ° C. The prior art blended into the diene rubber in an amount of 5 is disclosed in Patent Document 4 below, and in relation to the first and second problems, the tire tread rubber is excellent in workability and low rolling resistance. In order to obtain a composition, a non-petroleum high glass transition temperature (Tg) glycerol fatty acid triester is used as a base, and a plasticizer further containing a small amount of vegetable oil, if necessary, a large amount silica compounded diene rubber composition The prior art which mix | blends a predetermined quantity with is disclosed by the following patent documents 5. FIG.
本発明では、上記諸問題の解決に鑑みてなされたもので、シリカ配合系ゴム組成物に対し、高Tgと低Tgの樹脂成分を配合することにより、シリカ配合系ゴム組成物の低燃費性を損なうことなく、ドライおよびウェット操縦安定性、低温性能、並びに加工性を向上させたタイヤトレッド用ゴム組成物を提供することを目的とする。 The present invention has been made in view of the solution of the above-mentioned problems. By blending a high Tg and low Tg resin component into a silica compounded rubber composition, the fuel efficiency of the silica compounded rubber composition is improved. An object of the present invention is to provide a rubber composition for a tire tread having improved dry and wet handling stability, low temperature performance, and processability without impairing the performance.
本発明によれば、ジエン系ゴム100重量部に対し、BET比表面積100〜300m2/gのシリカを10重量部以上含む補強性充填剤30〜150重量部、シランカップリング剤をシリカ配合量に対して0.1〜15重量%配合してなるタイヤトレッド用ゴム組成物において、
(1)Tg:50〜120℃のテルペン樹脂、および
(2)(a)Tg:−50〜10℃で、水酸基価:120mg/KOH以下のテルペン系液状樹脂および(b)Tg:−50〜10℃のロジンとエステルを反応させて得られるロジンのエステル化合物の少なくとも一種
を配合比(1):(2)=20:80〜80:20の範囲で、その合計配合量として1〜20重量部配合したタイヤトレッド用ゴム組成物が提供される。
According to the present invention, 30 to 150 parts by weight of a reinforcing filler containing 10 parts by weight or more of silica having a BET specific surface area of 100 to 300 m 2 / g with respect to 100 parts by weight of diene rubber, and the amount of silane coupling agent added to silica In the rubber composition for a tire tread formed by blending 0.1 to 15% by weight with respect to
(1) Tg: terpene resin having a temperature of 50 to 120 ° C. At least one kind of rosin ester compound obtained by reacting rosin and ester at 10 ° C. is in the range of blending ratio (1) :( 2) = 20: 80-80: 20, and the total blending amount is 1-20 wt. A partially blended rubber composition for tire treads is provided.
本発明では、シリカ配合系ゴム組成物における加工性とドライ性能の低下の問題が、高Tgのテルペン樹脂と、低Tgのテルペン系液状樹脂および/または低Tgのロジンのエステルとを所定配合比で、所定量シリカ配合系ゴム組成物に配合することによって、一挙に解決できることを見出したものである。 In the present invention, the problem of deterioration in processability and dry performance in the silica compounded rubber composition is that a high Tg terpene resin and a low Tg terpene liquid resin and / or a low Tg rosin ester have a predetermined compounding ratio. Thus, it has been found that a predetermined amount can be solved at once by blending with a silica-blended rubber composition.
本発明のタイヤトレッド用ゴム組成物に配合される上記高Tgのテルペン樹脂としては、Tg:50〜120℃、より好ましくは60〜100℃のテルペン樹脂が用いられる。かかるテルペン樹脂としては、テルペン樹脂、水添テルペン樹脂、テルペンフェノール樹脂、芳香族変性テルペン樹脂などから、当該所定のTgを有するものが選定使用される。 As said high Tg terpene resin mix | blended with the rubber composition for tire treads of this invention, Tg: 50-120 degreeC, More preferably, the terpene resin of 60-100 degreeC is used. As such a terpene resin, a terpene resin, a hydrogenated terpene resin, a terpene phenol resin, an aromatic modified terpene resin, or the like is selected and used.
また、本発明のタイヤトレッド用ゴム組成物に配合される上記低Tgの(a)テルペン系液状樹脂としては、Tg:−50〜10℃、より好ましくは−40〜0℃で、水酸基価:120mg/KOH以下、好ましくは100mg/KOH以下のテルペン系液状樹脂が用いられる。かかるテルペン系液状樹脂としては、例えば、テルペン樹脂、水添テルペン樹脂、テルペンフェノール樹脂、芳香族変性樹脂などから、当該所定のTgを有するものが選定使用される。 The low Tg (a) terpene-based liquid resin blended in the tire tread rubber composition of the present invention has a Tg of −50 to 10 ° C., more preferably −40 to 0 ° C., and a hydroxyl value: A terpene-based liquid resin of 120 mg / KOH or less, preferably 100 mg / KOH or less is used. As such terpene-based liquid resin, for example, a terpene resin, a hydrogenated terpene resin, a terpene phenol resin, an aromatic modified resin, or the like is selected and used.
また、本発明のタイヤトレッド用ゴム組成物に配合される上記低Tgの(b)ロジンのエステル化合物としては、Tg:−50〜10℃、より好ましくは−40〜0℃の、ロジンのエステル化合物が用いられる。かかるロジンのエステル化合物としては、例えば、(a)トール油、トール油レジン、トール油脂肪酸等のロジン類と、(b)1価あるいは多価の各種アルコール類(このうち、好適なものは、エチレングリコール、ジエチレングリコール、トリエチレングリコール、プロピレングリコール等)とのエステル化合物が使用される。 In addition, the low Tg (b) rosin ester compound blended in the tire tread rubber composition of the present invention has a Tg of -50 to 10 ° C, more preferably -40 to 0 ° C. A compound is used. Examples of such rosin ester compounds include (a) rosins such as tall oil, tall oil resin and tall oil fatty acid, and (b) various monovalent or polyhydric alcohols (among these, preferred ones are: Ester compounds with ethylene glycol, diethylene glycol, triethylene glycol, propylene glycol, etc.) are used.
本発明のタイヤトレッド用ゴム組成物には、前記高Tgのテルペン樹脂と、低Tgの(a)テルペン系液状樹脂および(b)ロジンのエステル化合物の少なくとも一種との配合比を、20:80〜80:20、より好ましくは、30:70〜70:30の範囲で、ジエン系ゴム組成物100重量部に対し、合計配合量1〜20重量部、より好ましくは1.5〜15重量部の量で配合使用される。当該高Tgのテルペン樹脂の配合比が20未満である場合および80を超える場合は、ドライ性能とウェット性能のバランスが悪化するほか、加工性の改善効果が小さいので、好ましくない。またその合計量が1重量部未満では所期の効果を発揮できず、逆に20重量部を超えると、発熱(低燃費性)と耐摩耗性が悪化するので、好ましくない。 In the tire tread rubber composition of the present invention, the blend ratio of the high Tg terpene resin and at least one of the low Tg (a) terpene liquid resin and (b) rosin ester compound is 20:80. -80: 20, more preferably in the range of 30: 70-70: 30, with respect to 100 parts by weight of the diene rubber composition, the total blending amount is 1-20 parts by weight, more preferably 1.5-15 parts by weight. Is used in an amount of. When the blending ratio of the high Tg terpene resin is less than 20 or more than 80, the balance between the dry performance and the wet performance is deteriorated, and the workability improvement effect is small, which is not preferable. If the total amount is less than 1 part by weight, the desired effect cannot be exhibited. Conversely, if it exceeds 20 parts by weight, heat generation (low fuel consumption) and wear resistance are deteriorated, which is not preferable.
本発明のタイヤトレッド用ゴム組成物に用いられるジエン系ゴム成分としては、例えば、天然ゴム(NR)、あるいは、ポリイソプレンゴム(IR)、各種ブタジエンゴム(BR)、各種スチレン−ブタジエン共重合体ゴム(SBR)、アクリロニトリル−ブタジエン共重合体ゴム(NBR)、クロロプレンゴム、エチレン−プロピレン−ジエン共重合体ゴム、スチレン−イソプレン共重合体ゴム、スチレン−イソプレン−ブタジエン共重合体ゴム、イソプレン−ブタジエン共重合体ゴム等の合成ゴムが挙げられ、当該ゴム成分は、単独で、あるいは二種以上混合して使用されてよい。 Examples of the diene rubber component used in the tire tread rubber composition of the present invention include natural rubber (NR), polyisoprene rubber (IR), various butadiene rubbers (BR), and various styrene-butadiene copolymers. Rubber (SBR), acrylonitrile-butadiene copolymer rubber (NBR), chloroprene rubber, ethylene-propylene-diene copolymer rubber, styrene-isoprene copolymer rubber, styrene-isoprene-butadiene copolymer rubber, isoprene-butadiene Synthetic rubbers such as copolymer rubbers may be mentioned, and the rubber components may be used alone or in admixture of two or more.
本発明のタイヤトレッド用ゴム組成物に配合される補強性充填剤としては、BET比表面積100〜300m2/gのシリカを10重量部以上、好ましくは20〜100重量部含む補強性充填剤30〜150重量部、好ましくは40〜120重量部が使用される。当該シリカの配合量が10重量部未満では低発熱性のゴム組成物を得ることができず、逆にシリカを含む補強性充填剤の配合量が150重量部を超えると、加工性および耐摩耗性等が低下するので、好ましくない。上記シリカ以外の補強性充填剤としては、通常、カーボンブラック等が好ましく用いられるが、これに限定されるものではない。 As the reinforcing filler blended in the rubber composition for tire treads of the present invention, the reinforcing filler 30 containing 10 parts by weight or more, preferably 20 to 100 parts by weight of silica having a BET specific surface area of 100 to 300 m 2 / g. Up to 150 parts by weight, preferably 40 to 120 parts by weight are used. If the compounding amount of the silica is less than 10 parts by weight, a low heat-generating rubber composition cannot be obtained. Conversely, if the compounding amount of the reinforcing filler containing silica exceeds 150 parts by weight, the workability and wear resistance are reduced. This is not preferable because the properties and the like are lowered. As the reinforcing filler other than silica, usually, carbon black or the like is preferably used, but is not limited thereto.
本発明のタイヤトレッド用ゴム組成物には、通常シリカと共に配合されるシランカップリング剤をシリカ配合量の0.1〜15重量%、好ましくは4〜10重量%の量で配合使用される。かかるシランカップリング剤としては、当該タイヤ用ゴム組成物に一般に用いられるシランカップリング剤のいずれもが単独で、あるいは併用して使用されてよい。 In the rubber composition for a tire tread of the present invention, a silane coupling agent that is usually blended with silica is blended and used in an amount of 0.1 to 15% by weight, preferably 4 to 10% by weight of the blended amount of silica. As such a silane coupling agent, any of the silane coupling agents generally used in the tire rubber composition may be used alone or in combination.
本発明のタイヤトレッド用ゴム組成物には、更に、通常の加硫または架橋剤、加硫または架橋促進剤、老化防止剤、充填材、可塑剤、その他タイヤゴム用に配合されている各種配合剤を配合することができ、かかる配合剤は、一般的な方法で混練してゴム組成物とし、加硫または架橋することができる。これら配合剤の配合量も、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。 The rubber composition for a tire tread of the present invention is further added with a usual vulcanization or crosslinking agent, a vulcanization or crosslinking accelerator, an anti-aging agent, a filler, a plasticizer, and other various compounding agents blended for tire rubber. The compounding agent can be kneaded by a general method to obtain a rubber composition, which can be vulcanized or crosslinked. The compounding amounts of these compounding agents can be set to conventional general compounding amounts as long as the object of the present invention is not violated.
本発明の実施例及び比較例で用いたロジンのエステル化合物(トール油のジエチレングリコールエステル)は、以下の調製法によって得た。
トール油のジエチレングリコールエステルの調製
攪拌機、窒素導入管、温度計、ディーン・スターク分水器を備えた四つ口フラスコに、トール油(脂肪酸45%、ロジン38%、酸価157、商品名:ハートールSR−30、ハリマ化成製)1500g、ジエチレングリコール265g(OH/COOH=1.2)、酸化マグネシウム1.8gを加えた。攪拌して均一化した後、200℃まで昇温し、同温度にて10時間エステル化を行った。その後、減圧下で未反応アルコール等を除去し、トール油のジエチレングリコールエステルを得た。
The ester compound of rosin (diethylene glycol ester of tall oil) used in Examples and Comparative Examples of the present invention was obtained by the following preparation method.
Preparation of tall oil diethylene glycol ester A four-necked flask equipped with a stirrer, nitrogen inlet tube, thermometer, Dean-Stark water separator, tall oil (45% fatty acid, 38% rosin, acid value 157, trade name: Hartle) SR-30, Harima Chemicals) 1500 g, diethylene glycol 265 g (OH / COOH = 1.2), and magnesium oxide 1.8 g were added. After stirring and homogenizing, the temperature was raised to 200 ° C., and esterification was performed at the same temperature for 10 hours. Thereafter, unreacted alcohol and the like were removed under reduced pressure to obtain diethylene glycol ester of tall oil.
試験サンプルの作製
以下の表1に示す配合における加硫促進剤と硫黄を除く成分を、1.7Lの密閉式バンバリーミキサーで5分間混練し、160℃に達したときに当該ミキサー外に放出して室温まで冷却させた後、このマスターバッチを同ミキサー内に投入し、加硫促進剤と硫黄を配合、混練してゴム組成物を得た。このゴム組成物の一部を押出加工性試験に供した。残余のゴム組成物を15×15×0.2cmの金型中で、160℃、20分間プレス加硫して試験片(ゴムシート)を得、これを転がり抵抗試験および低温性能試験に供した。
Preparation of test sample The components other than the vulcanization accelerator and sulfur in the composition shown in Table 1 below were kneaded for 5 minutes in a 1.7 L closed Banbury mixer, and released to the outside of the mixer when the temperature reached 160 ° C. After cooling to room temperature, this master batch was put into the mixer, and a vulcanization accelerator and sulfur were blended and kneaded to obtain a rubber composition. A part of this rubber composition was subjected to an extrudability test. The remaining rubber composition was press vulcanized at 160 ° C. for 20 minutes in a 15 × 15 × 0.2 cm mold to obtain a test piece (rubber sheet), which was subjected to a rolling resistance test and a low temperature performance test. .
試験タイヤの作製
上記と同様の方法により表1に示す各例の配合組成からなるゴム組成部を得、これをキャップトレッドとして押出し、195/65R15サイズの試験タイヤを作製して、ドライおよびウェット操縦安定性試験に供した。
Preparation of test tire A rubber composition part comprising the compounding composition of each example shown in Table 1 was obtained in the same manner as described above, and this was extruded as a cap tread to prepare a test tire of 195 / 65R15 size. It was subjected to a stability test.
試験方法
1)押出加工性:上記キャップトレッドの押出時に、押出物の幅・ゲージが所定寸法に安定した後の押出機のスクリュー回転数を、比較例1を100とする指数で表示した。指数が大きい程、押出加工性が良好であることを示す。
2)転がり抵抗:粘弾性スペクトロメーター(東洋精機製作所製)を用いて、温度60℃で、初期歪:10%、動的歪:±2%、周波数20Hzの条件下でtanδ(60℃)を測定し、比較例1を100として指数で表示した。数値が大きい程、転がり抵抗が優れていることを示す。
Test Method 1) Extrudability: When the cap tread was extruded, the screw rotation speed of the extruder after the extrudate width / gauge was stabilized to a predetermined dimension was indicated by an index with Comparative Example 1 as 100. A larger index indicates better extrudability.
2) Rolling resistance: Using a viscoelastic spectrometer (manufactured by Toyo Seiki Seisakusho Co., Ltd.), at a temperature of 60 ° C., initial strain: 10%, dynamic strain: ± 2%, frequency 20 Hz, tan δ (60 ° C.) Measured and displayed as an index with Comparative Example 1 as 100. It shows that rolling resistance is excellent, so that a numerical value is large.
3)ドライ操縦安定性:排気量2Lの試験車両に4輪とも同じ仕様のテストタイヤを装着し、乾燥した舗装路面上におけるグリップレベルと操舵性をフィーリング評価し、比較例1を100とする指数で表示した。数値が大きい程、ドライ操縦安定性が良好であることを示す。
4)ウェット操縦安定性:排気量2Lの試験車両に4輪とも同じ仕様のテストタイヤを装着し、水深2mmの湿潤路におけるグリップレベルと操舵性をフィーリング評価し、比較例1を100とする指数で表示した。数値が大きい程、ウェット操縦安定性が良好であることを示す。
5)低温性能:ブリティッシュ・ポータブル・スキッドテスターを用いて、氷上温度(温度:−3℃)の条件下で測定し、比較例1を100として指数で表示した。数値が大きい程、低温性能が優れていることを示す。
3) Dry handling stability: Test tires with the same specifications are mounted on a test vehicle with a displacement of 2L, and the grip level and steering performance on a dry paved road surface are evaluated. Comparative Example 1 is set to 100. Expressed as an index. It shows that dry steering stability is so favorable that a numerical value is large.
4) Wet handling stability: Test tires with the same specifications are mounted on a test vehicle with a displacement of 2 liters, and the grip level and steering performance on a wet road with a water depth of 2 mm are evaluated for feeling. Expressed as an index. It shows that wet steering stability is so favorable that a numerical value is large.
5) Low temperature performance: Measured under conditions of on-ice temperature (temperature: -3 ° C) using a British portable skid tester. It shows that low temperature performance is excellent, so that a numerical value is large.
実施例1〜5および比較例1〜4
結果を以下の表1に示す。
The results are shown in Table 1 below.
表1の結果によれば、高Tgテルペン樹脂と、低Tgテルペン系液状樹脂および/またはロジンのエステル化合物の少なくとも一種を併用配合した本発明のゴム組成物では、低転がり抵抗を維持した上、ドライおよびウェット操縦安定性、低温性能、並びに加工性が向上していることが分る。 According to the results of Table 1, in the rubber composition of the present invention in which a high Tg terpene resin and at least one of a low Tg terpene-based liquid resin and / or an ester compound of rosin are combined, a low rolling resistance is maintained. It can be seen that dry and wet handling stability, low temperature performance, and processability are improved.
よって、本発明のゴム組成物は、タイヤトレッド用ゴム組成物として極めて有用である。 Therefore, the rubber composition of the present invention is extremely useful as a rubber composition for tire treads.
Claims (1)
(1)Tg:50〜120℃のテルペン樹脂、および
(2)(a)Tg:−50〜10℃で、水酸基価:120mg/KOH以下のテルペン系液状樹脂および(b)Tg:−50〜10℃のロジンとエステルを反応させて得られるロジンのエステル化合物の少なくとも一種
を配合比(1):(2)=20:80〜80:20の範囲で、その合計配合量として1〜20重量部配合したことを特徴とするタイヤトレッド用ゴム組成物。 30 to 150 parts by weight of a reinforcing filler containing 10 parts by weight or more of silica having a BET specific surface area of 100 to 300 m 2 / g with respect to 100 parts by weight of the diene rubber, and 0.1% of the silane coupling agent relative to the amount of silica. In the rubber composition for a tire tread formed by blending ~ 15% by weight,
(1) Tg: terpene resin having a temperature of 50 to 120 ° C. At least one kind of rosin ester compound obtained by reacting rosin and ester at 10 ° C. is in the range of blending ratio (1) :( 2) = 20: 80-80: 20, and the total blending amount is 1-20 wt. A rubber composition for a tire tread, characterized in that it is partially blended.
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