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Poly(p-phenylene)s tethered with oligo(ethylene oxide): synthesis by Yamamoto polymerization and properties as solid polymer electrolytes
Polymer Chemistry ( IF 4.1 ) Pub Date : 2020/03/02 , DOI: 10.1039/d0py00115e Hannes Nederstedt 1, 2, 3, 4, 5 , Patric Jannasch 1, 2, 3, 4, 5
Polymer Chemistry ( IF 4.1 ) Pub Date : 2020/03/02 , DOI: 10.1039/d0py00115e Hannes Nederstedt 1, 2, 3, 4, 5 , Patric Jannasch 1, 2, 3, 4, 5
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Salt-containing supramolecular assemblies of rigid-rod polymers tethered with flexible ion-solvating side chains represent a synthetic pathway towards thin ion-conducting solid electrolyte membranes with high dimensional stability. In the present work we have synthesized poly(p-phenylene)s (PpPs) carrying di-, tri- and tetra(ethylene oxide) side chains, respectively. p-Dichlorophenyl oligo(ethylene oxide) monomers were polymerized by Ni-mediated Yamamoto polymerization via in situ reduction of Ni(II). This gave PpPs with an average degree of polymerization reaching 60, where each phenylene ring carried one oligo(ethylene oxide) side chain. Results from calorimetry and X-ray scattering measurements clearly showed the formation of molecular composites, i.e., bicontinuous morphologies with mechanically reinforcing layers of the stiff PpP backbones separated by the flexible oligo(ethylene oxide) side chains. This morphology was retained after adding lithium bis(trifluoromethane)sulfonimide (LiTFSI) to form salt-in-polymer electrolytes, but with an increased distance between adjacent backbones. Furthermore, upon addition of salt the order-to-disorder transition (ODT) region increased from ∼50–170 °C to ∼75–200 °C at [EO]/[Li] = 20. Increasing salt concentrations also revealed a maximum in the ODT enthalpy at [EO]/[Li] = 40. At 80 and 160 °C, the ionic conductivity reached 1.1 × 10−4 and 1.0 × 10−3 S cm−1, respectively. Finally, we demonstrate that ionic conductivity of the polymer electrolytes can be significantly increased by additions of triglyme.
中文翻译：
聚（对亚苯基）与低聚（环氧乙烷）的连接：山本聚合法合成及其作为固体聚合物电解质的性质
刚性杆聚合物的含盐超分子组件与柔性离子溶解侧链相连，代表了通向具有高尺寸稳定性的薄离子导电固体电解质膜的合成途径。另外，在本工作中，我们（合成的多p亚苯基）S（P p分别携带二，三和四（环氧乙烷）侧链PS），。通过Ni介导的Yamamoto聚合反应通过对Ni（II）的原位还原来聚合对-二氯苯基低聚（环氧乙烷）单体。这给了P pPs平均聚合度达到60，其中每个亚苯基环带有一个低聚（环氧乙烷）侧链。量热法和X射线散射测量结果清楚地表明了分子复合物的形成，即具有刚性P p的机械增强层的双连续形态P骨架被柔性的低聚（环氧乙烷）侧链隔开。加入双（三氟甲烷）磺酰亚胺锂（LiTFSI）形成聚合物中的盐电解质后，这种形态得以保留，但相邻骨架之间的距离增加了。此外，在添加盐时，[EO] / [Li] = 20时，有序向无序过渡（ODT）区从约50-170°C增至约75-200°C。在[EO] / [Li] = 40的ODT焓中，离子电导率分别达到1.1×10 -4和1.0×10 -3 S cm -1。最后，我们证明了通过添加三甘醇二甲醚可以显着提高聚合物电解质的离子电导率。
更新日期：2020-03-31
中文翻译：
聚（对亚苯基）与低聚（环氧乙烷）的连接：山本聚合法合成及其作为固体聚合物电解质的性质
刚性杆聚合物的含盐超分子组件与柔性离子溶解侧链相连，代表了通向具有高尺寸稳定性的薄离子导电固体电解质膜的合成途径。另外，在本工作中，我们（合成的多p亚苯基）S（P p分别携带二，三和四（环氧乙烷）侧链PS），。通过Ni介导的Yamamoto聚合反应通过对Ni（II）的原位还原来聚合对-二氯苯基低聚（环氧乙烷）单体。这给了P pPs平均聚合度达到60，其中每个亚苯基环带有一个低聚（环氧乙烷）侧链。量热法和X射线散射测量结果清楚地表明了分子复合物的形成，即具有刚性P p的机械增强层的双连续形态P骨架被柔性的低聚（环氧乙烷）侧链隔开。加入双（三氟甲烷）磺酰亚胺锂（LiTFSI）形成聚合物中的盐电解质后，这种形态得以保留，但相邻骨架之间的距离增加了。此外，在添加盐时，[EO] / [Li] = 20时，有序向无序过渡（ODT）区从约50-170°C增至约75-200°C。在[EO] / [Li] = 40的ODT焓中，离子电导率分别达到1.1×10 -4和1.0×10 -3 S cm -1。最后，我们证明了通过添加三甘醇二甲醚可以显着提高聚合物电解质的离子电导率。
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