第117号(A4、E)4C/3 湯浅ほか

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1 Improved Silica Dispersibility with Functionalized S-SBR for Lower Rolling Resistance Takeshi Yuasa Takuo Sone Tetsuo Tominaga Munetaka Iwano Generally, rolling resistance of tire is closely related to hysteresis loss properties which are considered to depend on the dispersibility of filler in tire tread compounds. It is known that strong interaction between rubber materials and filler can improve the filler dispersibility. For the purpose of achieving the good interaction with silica filler, some modified styrene butadiene rubbers with functional groups at polymer chain ends have been developed by solution polymerization system S-SBRs. They showed significant reduction in the hysteresis loss of silica reinforced compounds. In particular, the modified S-SBR with both primary amino group and alkoxysilyl group exhibited excellently lower hysteresis loss properties. In order to investigate the dispersion of silica in compounds with this modified S-SBR directly, the measurements of transmission electron microscopy TEM and ultra small angle X-ray scattering USAXS were carried out. As a result, the excellent dispersion state of silica in the compounds with this modified S-SBR was observed, and we found that smaller size of silica aggregates could reduce the hysteresis loss to much lower level. This result coincided with that obtained by dynamic viscoelastic measurement. 16 JSR TECHNICAL REVIEW No.117/2010

2 n N N p JSR TECHNICAL REVIEW No.117/

3 q G δ G ω δ G δ G δ δ δ Δ δ Δ G δ G G G G G Δ G G G G δ δ G δ G δ 18 JSR TECHNICAL REVIEW No.117/2010

4 促されたと推測している Δ G はS-SBR-C S-SBR-B S- 集体が観測された 一方 Sample iii すなわち 末 SBR-Aの順に小さく ペイン効果の優劣からも 末端に一 端変性S-SBR-Cを用いた試料では Sample i に比べて 級アミノ基とアルコキシシリル基を有するS-SBR-Cがシリカの 極めて均一な数十nmスケールの凝集体が試料中に分散 分散に有効である傾向が確認された していた 表4に3D-TEM像の解析により得られたシリカ凝 3 2 TEMによる観察 集体の平均体積 および そのばらつきを示す Sample コンパウンド中におけるシリカの分散性を実空間で観察 iii 中のシリカの平均体積はSample i 中のそれよりも小さ するため TEMによる観 察を試 みた 図3に結 果を示 く またばらつきも少なかった この結果も動的粘弾性測 す Sample i においては シリカは比較的大きい凝集体 定の傾向と一致しており S-SBR-Cがシリカ分散に優れて として試料中に不均一に観測された その一方で一級アミ いることがわかった ノ基とアルコキシシリル基を有するSample iii はSample TEMによる観察は実空間での直接観察であり シリカ i ii と比較して明らかにシリカが細かく均一に分散して 分散性の評価に非常に有効である しかしその一方で限 おり 5 0 0nm以上におよぶ大きな凝集塊はほとんど観測さ られた範囲での観察となるため 次に示すUSAXS測定を れなかった この傾向は動的粘弾性測定により推測される 実施し シリカの構造を相補的に考察した シリカの分散性と一致していた 3 4 USAXS測定による構造解析 3 33D-TEMによる観察 コンパウンド中におけるシリカ粒子の構造を USAXS測 図4に3D-TEMによる観察結果を示す 図中では個々の 定により解析することを試みた 図5に 各試料から得られ シリカの凝集体を区別して示している 3D-TEMによる観 たUSAXSプロファイルを示 す 未 変 性S-SBRと変 性S- 察結果は 通常のTEM 2D-TEM の結果と同様 Sam- SBRを用いた試料では 形状の異なるプロファイルが得ら ple i すなわち 未変性のS-SBR-Aを用いた試料にお れ シリカの分散状態の大きな変化が示唆された 未変 いては 数十nmから数百nmにわたる 様々な大きさの凝 性S-SBRを用いたSample i はべき乗則にしたがった散乱 Figure3 TEM images of sample i a, sample ii b, and sample iii c. Figure4 3D-TEM images of sample i a and sample iii b. JSR TECHNICAL REVIEW No.117/

5 q q Rubber Chem. Technol 63 Rubber Chem. Technol JSR TECHNICAL REVIEW No.117/2010

6 J. Appl. Crystallogr 36 J. Polym. Sci., Part B: polym. Phys 41 Compos. Interfaces 10 Polymer 45 Curr. Opin. Solid State Mater. Sci 8 Langmuir 21 JSR TECHNICAL REVIEW No.117/

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