Study on Homogeneity in Sulfur Cross-Linked Network Structures of Isoprene Rubber by TD-NMR and AFM – Zinc Stearate System,Macromolecules

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Study on Homogeneity in Sulfur Cross-Linked Network Structures of Isoprene Rubber by TD-NMR and AFM – Zinc Stearate System
Macromolecules ( IF 5.1 ) Pub Date : 2020-09-15 , DOI: 10.1021/acs.macromol.0c01266
Kosuke Miyaji _{1,

2} , Takuma Sugiyama _{1,

2} , Takumi Ohashi ₂ , Kay Saalwächter ₃ , Yuko Ikeda _{2,

4}

Affiliation

An important role of the zinc stearate (ZnSt₂) activator in the sulfur cross-linking reaction of isoprene rubber is proved by combination of ¹H double-quantum nuclear magnetic resonance spectroscopy and nanomechanical mapping of atomic force microscopy for the first time. The dinuclear-type bridging bidentate zinc/stearate complex (intermediate I) is well dispersed in the rubber matrix to result in the formation of a highly homogeneous network structure by reacting with N-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine and sulfur. Upon increasing the concentration of ZnSt₂, the amount of generated intermediate I increases, and consequently, the molecular weight between the constraints (M_c) decreases proportionally. However, a large amount of ZnSt₂ widens the distribution of 1/M_c and decreases the network uniformity. These results are based on the first qualitative agreement between the relative 1/M_c values, and in particular the width of their inhomogeneous distributions, measured by the two techniques. High potential for controlling a network structure in a vulcanizate is shown, where an amount of the generated intermediate I plays a key role.

中文翻译：

TD-NMR和AFM-硬脂酸锌体系研究异戊二烯橡胶硫交联网络结构的均质性

首次结合¹ H双量子核磁共振波谱和原子力显微镜的纳米力学图谱证明了硬脂酸锌（ZnSt ₂）活化剂在异戊二烯橡胶的硫交联反应中的重要作用。双核型桥接二齿锌/硬脂酸酯络合物（中间体I）很好地分散在橡胶基质中，从而通过与N-（1,3-苯并噻唑-2-基硫烷基）环己胺和硫。随着ZnSt ₂浓度的增加，中间体I的生成量增加，因此，限制条件之间的分子量（M _c）按比例减少。但是，大量的ZnSt ₂会使1 / M _c的分布变宽，并降低网络均匀性。这些结果是基于相对的1 / M _c值之间的第一个定性一致性，尤其是通过两种技术测得的它们的非均匀分布的宽度。显示了在硫化橡胶中控制网络结构的高潜力，其中生成的中间体I的数量起关键作用。

更新日期：2020-10-13

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