JP2007231104A - Rubber composition - Google Patents
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- JP2007231104A JP2007231104A JP2006053521A JP2006053521A JP2007231104A JP 2007231104 A JP2007231104 A JP 2007231104A JP 2006053521 A JP2006053521 A JP 2006053521A JP 2006053521 A JP2006053521 A JP 2006053521A JP 2007231104 A JP2007231104 A JP 2007231104A
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Abstract
Description
本発明はゴム組成物に関し、更に詳しくはゴム物性に実質的な影響を及ぼすことなく、酸化亜鉛の配合量を減らしたゴム組成物に関する。 The present invention relates to a rubber composition, and more particularly to a rubber composition in which the compounding amount of zinc oxide is reduced without substantially affecting rubber physical properties.
ゴム組成物中の酸化亜鉛の使用量を削減することが試みられている。例えば天然ゴム、ジエン系ゴムもしくはクロロプレンゴム、ニトリルゴム、エチレンプロピレンゴムから選ばれた1種以上のゴム成分100重量部に対し、粒径200nm以下の酸化亜鉛微粒子をカーボンブラック粒子中に均質に分散させた酸化亜鉛複合カーボンブラック20〜200重量部を配合してなるゴム組成物が知られており(特許文献1参照)、この方法によれば、少ない酸化亜鉛の使用量でも強度及び耐摩耗性に優れたゴム組成物が得られる旨記載されている。 Attempts have been made to reduce the amount of zinc oxide used in rubber compositions. For example, zinc oxide fine particles having a particle size of 200 nm or less are uniformly dispersed in carbon black particles with respect to 100 parts by weight of one or more rubber components selected from natural rubber, diene rubber or chloroprene rubber, nitrile rubber, and ethylene propylene rubber. A rubber composition comprising 20 to 200 parts by weight of zinc oxide composite carbon black is known (see Patent Document 1). According to this method, strength and wear resistance can be achieved even with a small amount of zinc oxide used. It is described that an excellent rubber composition can be obtained.
従って、本発明の目的はゴム組成物の物性、特に機械的強度、粘弾性特性を実質的に低下させることなく、ゴム組成物中の酸化亜鉛の配合量を著しく少なくすることにある。 Accordingly, an object of the present invention is to significantly reduce the amount of zinc oxide in the rubber composition without substantially reducing the physical properties, particularly mechanical strength and viscoelastic properties of the rubber composition.
本発明に従えば、ジエン系ゴム、カーボンブラック及び/又はシリカ、イオウを含み並びに加硫促進助剤として平均粒子径80nm未満の酸化亜鉛を含んでなるゴム組成物が提供される。 According to the present invention, there is provided a rubber composition comprising diene rubber, carbon black and / or silica, sulfur and zinc oxide having an average particle size of less than 80 nm as a vulcanization acceleration aid.
本発明によれば、ゴム組成物中に、平均粒子径が80nm以下の酸化亜鉛を用いることによりゴム組成物の物性、特に機械的物性、粘弾性特性を低下させることなく、ゴム組成物中の亜鉛の使用量を最大1/10まで減らすことができる。 According to the present invention, by using zinc oxide having an average particle size of 80 nm or less in the rubber composition, the physical properties of the rubber composition, particularly mechanical properties and viscoelastic properties are not deteriorated. The amount of zinc used can be reduced to a maximum of 1/10.
本発明者らは前記課題を解決すべく研究を進めた結果、今回、通気法で測定した平均粒子径が80nm未満、好ましくは50〜20nmで、窒素吸着法(BET法)(JIS−K6217−2(カーボンブラック用)準拠)で測定した比表面積が10m2/g以上(更に好ましくは100〜200m2/g)の酸化亜鉛(従来の汎用酸化亜鉛の平均粒子径は0.25〜0.6μm、比表面積は4〜7m2/g)を使用することにより、亜鉛の使用量を従来の1/10に減らしてもほぼ同じ物性を発現できることを見出した。 As a result of researches to solve the above problems, the present inventors have determined that the average particle diameter measured by the aeration method is less than 80 nm, preferably 50 to 20 nm, and the nitrogen adsorption method (BET method) (JIS-K6217-). 2 (for carbon black)) zinc oxide having a specific surface area of 10 m 2 / g or more (more preferably 100 to 200 m 2 / g) (average particle size of conventional general-purpose zinc oxide is 0.25 to 0. 0). By using 6 μm and a specific surface area of 4 to 7 m 2 / g), it was found that substantially the same physical properties can be expressed even if the amount of zinc used is reduced to 1/10 of the conventional amount.
本発明の好ましい態様では、ジエン系ゴム100重量部に対して、カーボンブラック及び/又はシリカ20〜150重量部、イオウ1〜5重量部並びに加硫促進助剤として平均粒子径80nm未満の酸化亜鉛0.01〜5重量部を配合する。 In a preferred embodiment of the present invention, zinc oxide having an average particle size of less than 80 nm as a vulcanization accelerating aid and carbon black and / or silica 20 to 150 parts by weight, sulfur 1 to 5 parts by weight and 100 parts by weight of diene rubber. 0.01-5 weight part is mix | blended.
本発明のゴム組成物に配合するジエン系ゴムは各種ゴム組成物に一般的に配合することができる任意のジエン系ゴム、例えば天然ゴム(NR)、ポリイソプレンゴム(IR)、各種スチレン−ブタジエン共重合体ゴム(SBR)、各種ポリブタジエンゴム(BR)、アクリロニトリル−ブタジエン共重合体ゴム(NBR)、ブチルゴム(IIR)などを単独又は任意のブレンドとして使用することができる。 The diene rubber compounded in the rubber composition of the present invention may be any diene rubber that can be generally compounded in various rubber compositions such as natural rubber (NR), polyisoprene rubber (IR), various styrene-butadienes. Copolymer rubber (SBR), various polybutadiene rubbers (BR), acrylonitrile-butadiene copolymer rubber (NBR), butyl rubber (IIR) and the like can be used alone or as any blend.
本発明において使用するカーボンブラック及び/又はシリカは、ジエン系ゴム100重量部に対し、好ましくは20〜150重量部、更に好ましくは50〜150重量部配合する。この配合量が少ないと補強効果が低すぎて、機械的物性を満足しないおそれがあり、また多過ぎると不良分散、硬度の上昇、伸びの低下をひきおこすおそれがある。使用することができるカーボンブラック及びシリカには特に限定はなく、またカーボンブラックとシリカの使用比率には特に限定はない。 The carbon black and / or silica used in the present invention is preferably blended in an amount of 20 to 150 parts by weight, more preferably 50 to 150 parts by weight, based on 100 parts by weight of the diene rubber. If the blending amount is too small, the reinforcing effect is too low and the mechanical properties may not be satisfied. If the blending amount is too large, poor dispersion, increased hardness, and reduced elongation may occur. Carbon black and silica that can be used are not particularly limited, and the ratio of carbon black and silica is not particularly limited.
本発明において使用するイオウは、ゴム組成物中に配合するのに使用される任意のイオウを用いることができ、その配合量には特に限定はないが、ジエン系ゴム100重量部に対し、好ましくは1〜5重量部、更に好ましくは1〜3重量部とする。この配合量が少ないと架橋密度が低すぎて機械的物性が低すぎるおそれがあり、また多いと架橋密度が高すぎて伸びの低下、硬度上昇のおそれがある。 As the sulfur used in the present invention, any sulfur used for blending in the rubber composition can be used, and the blending amount thereof is not particularly limited, but is preferably based on 100 parts by weight of the diene rubber. Is 1 to 5 parts by weight, more preferably 1 to 3 parts by weight. If the blending amount is small, the crosslinking density is too low and the mechanical properties may be too low. If the blending amount is too large, the crosslinking density is too high and the elongation may decrease and the hardness may increase.
本発明において加硫促進剤助剤として使用する酸化亜鉛は前述の如く平均粒子径が80nm未満のもの、好ましくは平均粒子径が50〜20nmで、比表面積が10m2/g以上(更に好ましくは100〜200m2/g)のものを使用する。使用する酸化亜鉛の平均粒子径が大きいと表面の反応サイトが減少するので好ましくない。また粒子の比表面積が小さいと同様の理由で好ましくない。 As described above, the zinc oxide used as a vulcanization accelerator auxiliary in the present invention has an average particle size of less than 80 nm, preferably an average particle size of 50 to 20 nm, and a specific surface area of 10 m 2 / g or more (more preferably 100-200 m 2 / g) is used. If the average particle size of the zinc oxide used is large, the number of reaction sites on the surface decreases, which is not preferable. Moreover, it is not preferable for the same reason that the specific surface area of the particles is small.
本発明において使用する平均粒子径が80nm未満の酸化亜鉛は例えば気相法と呼ばれる方法で製造することができる。気相法(PVS法)とは、米国ナノフェーズテクノロジー社が開発した超微粒子製造技術で、原料(金属亜鉛)が熱エネルギーによって、金属原子の蒸気となり、反応ガス(酸素)との接触により、金属酸化物の分子(即ち酸化亜鉛)並びにクラスターが形成され、その後、瞬時に冷却することにより、粒径の増大が抑えられ、80nm未満の酸化亜鉛を得ることができる。 Zinc oxide having an average particle size of less than 80 nm used in the present invention can be produced, for example, by a method called a gas phase method. The vapor phase method (PVS method) is an ultrafine particle manufacturing technology developed by the US Nanophase Technology Company. The raw material (metal zinc) becomes vapor of metal atoms by thermal energy, and comes into contact with the reaction gas (oxygen). Metal oxide molecules (that is, zinc oxide) and clusters are formed, and then cooled instantaneously, thereby suppressing an increase in particle size and obtaining zinc oxide of less than 80 nm.
本発明に係るゴム組成物には、前記した成分に加えて、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、その他のゴム組成物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練して組成物とし、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 is used for tires such as vulcanization or crosslinking agents, vulcanization or crosslinking accelerators, various oils, anti-aging agents, plasticizers, and other rubber compositions. Various additives that are generally blended in the above can be blended, and such additives can be kneaded by a general method to form a composition, which can be used for vulcanization or crosslinking. As long as the amount of these additives is not contrary to the object of the present invention, a conventional general amount can be used.
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1〜2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1.6リットルの密閉型ミキサーで5分間混練し、150℃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。このゴム組成物を用いて以下に示す試験法で未加硫物性を評価した。結果は表Iに示す。
Examples 1-2 and Comparative Examples 1-4
Sample preparation In the formulation shown in Table I, the components excluding the vulcanization accelerator and sulfur were kneaded for 5 minutes in a 1.6 liter closed mixer and released when the temperature reached 150 ° C to obtain a master batch. A vulcanization accelerator and sulfur were kneaded with this masterbatch with an open roll to obtain a rubber composition. Using this rubber composition, unvulcanized physical properties were evaluated by the following test methods. The results are shown in Table I.
次に得られたゴム組成物を15×15×0.2cmの金型中で160℃で15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物性を測定した。結果は表Iに示す。 Next, the obtained rubber composition was vulcanized in a 15 × 15 × 0.2 cm mold at 160 ° C. for 15 minutes to prepare a vulcanized rubber sheet, and the physical properties of the vulcanized rubber were measured by the following test methods. It was measured. The results are shown in Table I.
ゴム物性評価試験法
JIS−A硬度:JIS K6253に準拠して測定。
300%モジュラス(M300)及び100%モジュラス(M100):JIS K6251に準拠して測定。
破断強度(TB)及び破断伸び(EB):JIS K6251に準拠して測定。
Rubber physical property evaluation test method JIS-A hardness: Measured according to JIS K6253.
300% modulus (M300) and 100% modulus (M100): Measured according to JIS K6251.
Breaking strength (TB) and breaking elongation (EB): Measured according to JIS K6251.
tanδ(0℃及び60℃):伸長型粘弾性測定機(東洋精機(株)製)を使用して初期伸長10%、歪率±2%、周波数20Hz条件で温度0℃及び60℃で測定。 tan δ (0 ° C. and 60 ° C.): Measured at a temperature of 0 ° C. and 60 ° C. using an extension-type viscoelasticity measuring device (manufactured by Toyo Seiki Co., Ltd.) with an initial elongation of 10%, a distortion rate of ± 2%, and a frequency of 20 Hz. .
表I脚注
*1:日本ゼオン(株)製SBR(Nipol 1502)
*2:東海カーボン(株)製カーボンブラック(シーストKH)
*3:正同化学工業(株)製酸化亜鉛(酸化亜鉛3種、平均粒子径0.5μm、比表面積5m2/g)
*4:シーアイ化成(株)製ナノ亜鉛華(平均粒子径34nm、比表面積30m2/g)
*5:日本油脂(株)製ステアリン酸(ビーズステアリン酸 YR)
*6:FLEXSYS製老化防止剤6C(SANTOFLEX6PPD)
*7:鶴見化学工業(株)製油処理硫黄(金華印微粉硫黄 151メッシュ)
*8:大内新興化学工業(株)製加硫促進剤 CZ(ノクセラーCZ−G)
Table I footnote * 1: SBR (Nipol 1502) manufactured by Nippon Zeon Co., Ltd.
* 2: Carbon black (Seast KH) manufactured by Tokai Carbon Co., Ltd.
* 3: Zinc oxide manufactured by Shodo Chemical Co., Ltd. (3 types of zinc oxide, average particle size 0.5 μm, specific surface area 5 m 2 / g)
* 4: Nano zinc white (average particle size: 34 nm, specific surface area: 30 m 2 / g) manufactured by CI Kasei Co., Ltd.
* 5: Stearic acid (bead stearic acid YR) manufactured by Nippon Oil & Fats Co., Ltd.
* 6: Anti-aging agent 6C (SANTOFLEX 6PPD) manufactured by FLEXSYS
* 7: Tsurumi Chemical Industry Co., Ltd. oil-treated sulfur (Jinhua stamp fine powder sulfur 151 mesh)
* 8: Vulcanization accelerator CZ (Noxeller CZ-G) manufactured by Ouchi Shinsei Chemical Industry Co., Ltd.
比較例1はZnOを配合していない例で架橋密度(M100)が上がらず、比較例2は通常の使用量を1/3に減らしたもの、比較例3は通常の使用例を示す。
実施例1は破断強度が比較例2及び3より高く、その他物性は比較例2とほぼ同等である。
実施例2はモジュラスが比較例3より高く、tan−δ(60℃)が比較例3より低く、低燃費性に優れている。
Comparative Example 1 is an example in which ZnO is not blended, and the crosslink density (M100) does not increase. Comparative Example 2 is a case where the normal use amount is reduced to 1/3, and Comparative Example 3 is a normal use example.
Example 1 has a higher breaking strength than Comparative Examples 2 and 3, and other physical properties are almost the same as Comparative Example 2.
In Example 2, the modulus is higher than that of Comparative Example 3, tan-δ (60 ° C.) is lower than that of Comparative Example 3, and the fuel efficiency is excellent.
本発明によれば、ゴム組成物の物性に実質的な悪影響を及ぼすことなく、ゴム組成物中の酸化亜鉛の配合量を著しく少なくすることができる。 According to the present invention, the blending amount of zinc oxide in the rubber composition can be remarkably reduced without substantially adversely affecting the physical properties of the rubber composition.
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CN103665610A (en) * | 2013-11-29 | 2014-03-26 | 山东永泰化工有限公司 | Black sidewall rubber of radial tire of passenger car |
JP2017088789A (en) * | 2015-11-13 | 2017-05-25 | 株式会社ブリヂストン | Rubber composition and method for producing the same, and vulcanized rubber and method for producing the same |
CN105400016A (en) * | 2015-12-08 | 2016-03-16 | 黄涌芮 | High-strength rubber and preparation method thereof |
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