Synthesis of Imidazolium Salt-Terminated Poly(amidoamine)-Typed POSS-Core Dendrimers and Their Solution and Bulk Properties
Synthesis of Imidazolium Salt-Terminated Poly(amidoamine)-Typed POSS-Core Dendrimers and Their Solution and Bulk Properties
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咪唑鎓盐封端聚酰胺胺型 POSS 核心树枝状聚合物的合成及其溶液和本体性能
DOI：
10.1038/pj.2013.60
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发表时间：
2014
期刊：
影响因子：
--
通讯作者：
S.
中科院分区：
文献类型：
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作者：
Naka;K.; Shinke;R.; Yamada;M.; Belkada;F.; Aijo;Y.; Irie;Y. Shankar;S. R.; Smaran;K. S.; Matsumi;N.; Tomita;S.; Sakurai;S.
以1-溴丙烷为原料，合成了以溴化咪唑为端基的第一代和第二代聚酰胺-胺（PAMAM）型多面体低聚倍半硅氧烷（POSS）为核的树枝状大分子POSS-PIm 16 Br和POSS-PIm 32 Br。POSS-PIm 16 Br和POSS-PIm 32 Br的结构通过多核核磁共振数据、MALDI-TOF-MS光谱和元素分析进行了鉴定。通过POSS-PIm 16 Br和POSS-PIm 32 Br的阴离子交换反应制备的咪唑鎓六氟磷酸盐（PF 6）封端的第一代和第二代POSS-核树枝状聚合物（分别表示为POSS-PIm 16 PF 6和POSS-PIm 32 PF 6）的流延膜的广角X射线散射（WAXS）数据表征为两个无定形晕的出现，在q= 15 nm− 1处具有强峰，在q= 10 nm− 1附近具有另一个弱峰。我们目前的POSS-PIm 16 PF 6和POSS-PIm 32 PF 6的流延膜的X射线衍射数据反映了与1-丁基-3-甲基咪唑六氟磷酸盐相同的特征。通过POSS-PIm 16 Br和POSS-PIm 32 Br的阴离子交换反应制备了以咪唑双（三氟甲磺酰基）酰亚胺（TFSI）为端基的POSS-核树枝状大分子，并加入LiTFSI后，用交流阻抗法测定了其离子电导率.在51 C下，对于低代和较少锂盐添加的POSS-核心树枝状聚合物观察到4.03× 10− 5 S cm− 1的最大离子电导率。
Imidazolium bromide-terminated first and second generation poly (amidoamine)(PAMAM)-typed polyhedral oligomeric silsesquioxane (POSS)-core dendrimers, denoted as POSS-PIm16Br and POSS-PIm32Br, respectively, were prepared by the reaction of the corresponding imidazole-terminated PAMAM-typed POSS-core dendrimers with 1-bromopropane. The structures of POSS-PIm16Br and POSS-PIm32Br were identified using multinuclear nuclear magnetic resonance data, MALDI-TOF-MS spectra, and elemental analysis. Wide-angle X-ray scattering (WAXS) data for cast films of the imidazolium hexafluorophosphate (PF 6)-terminated first and second generation POSS-core dendrimers, denoted as POSS-PIm16PF 6 and POSS-PIm32PF 6, respectively, which were prepared by anion exchange reactions of POSS-PIm16Br and POSS-PIm32Br, were characterized by the occurrence of two amorphous halos, with a strong peak at q= 15 nm− 1 and another weak peak around q= 10 nm− 1. Our present X-ray diffraction data for the cast films of POSS-PIm16PF 6 and POSS-PIm32PF 6 reflect the same features that were described for 1-butyl-3-methylimidazolium hexafluorophosphate. Ionic conductivities for the imidazolium bis (trifluoromethanesulfonyl) imide (TFSI)-terminated POSS-core dendrimers, which were prepared by anion exchange reactions of POSS-PIm16Br and POSS-PIm32Br, were estimated by the ac impedance method after the addition of LiTFSI. Maximum ionic conductivity of 4.03× 10− 5 S cm− 1 at 51 C was observed for the POSS-core dendrimer of lower generation and less lithium salt addition.