首页> 外文期刊>Journal of Polymer Science, Part B. Polymer Physics >Epoxy resin/poly(epsilon-caprolactone) blends cured with 2,2-bis[4(4-aminophenoxy)phenyl]propane. II. Studies by Fourier transform infrared and carbon-13 cross-polarization/magic-angle spinning nuclear magnetic resonance spectroscopy
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Epoxy resin/poly(epsilon-caprolactone) blends cured with 2,2-bis[4(4-aminophenoxy)phenyl]propane. II. Studies by Fourier transform infrared and carbon-13 cross-polarization/magic-angle spinning nuclear magnetic resonance spectroscopy

机译:用2,2-双[4(4-氨基苯氧基)苯基]丙烷固化的环氧树脂/聚(ε-己内酯)共混物。二。傅里叶变换红外和碳13交叉极化/魔角旋转核磁共振波谱研究

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Crystalline thermosetting blends composed of 2,2'-bis [4-(4-aminophenoxy)phenyl]propane-crosslinked epoxy resin (ER) and poly(epsilon-caprolactone) (PCL) were investigated by means of Fourier transform infrared (FTIR) spectroscopy and high-resolution solid-state NMR spectroscopy. FTIR investigations indicated that there were specific intermolecular interactions between ER and PCL and that the intermolecular hydrogen-bonding interactions were weaker than the self-association in pure epoxy. The intermolecular hydrogen bonding was considered to be the driving force for the miscibility of the thermosetting blends. For the examination of the miscibility of the thermosetting blends at the molecular level, high-resolution solid-state C-13 crosspolarity/magic-angle spinning (CP-MAS) NMR spectroscopy was employed. The line width of C-13 CP-MAS spectra decreased with increasing PCL contents, and the chemical shift of the carbonyl carbon resonance of PCL shifted to a low field with an increasing epoxy content in the blends. The proton spin-lattice relaxation experiments in the laboratory frame showed that all the blends possessed identical, composition-dependent relaxation times (i.e., the proton spin-lattice relaxation times in the laboratory frame), suggesting that the thermosetting blends were homogeneous on the scale of 20-30 nm in terms of the spin-diffusion mechanism, and this was in a good agreement with the results of differential scanning calorimetry and dynamic mechanical analysis. For the examination of the miscibility of the blends at the molecular level, the behavior of the proton lattice relaxation in the rotating frame was investigated. The homogeneity of the thermosetting blends at the molecular level was quite dependent on the blend composition. The PCL-lean ER/PCL blends (e.g., 70/30) displayed a single homogeneous amorphous phase, and the molecular chains were intimately mixed on the segmental scale. The PCL-rich blends displayed biexponential decay in experiments concerning the proton spin-lattice relaxation times in the rotating frame, which was ascribed to amorphous and crystalline phases. In the amorphous region, the molecular chains of epoxy and PCL were intimately mixed at the molecular level. (C) 2003 Wiley Periodicals, Inc. [References: 54]
机译:借助傅立叶变换红外光谱(FTIR)研究了由2,2'-双[4-(4-(4-氨基苯氧基)苯基]丙烷交联的环氧树脂(ER)和聚(ε-己内酯)(PCL)组成的晶体热固性共混物光谱学和高分辨率固态NMR光谱学。 FTIR研究表明,ER和PCL之间存在特定的分子间相互作用,并且分子间的氢键相互作用弱于纯环氧树脂中的自缔合。分子间氢键被认为是热固性共混物混溶性的驱动力。为了在分子水平上检查热固性混合物的混溶性,使用了高分辨率固态C-13交叉极性/魔角旋转(CP-MAS)NMR光谱。 C-13 CP-MAS光谱的线宽随着PCL含量的增加而降低,并且随着共混物中环氧含量的增加,PCL的羰基碳共振的化学位移移至低电场。实验室框架中的质子自旋晶格弛豫实验表明,所有共混物均具有相同的,依赖于成分的弛豫时间(即实验室框架中的质子自旋晶格弛豫时间),这表明热固性共混物在规模上是均匀的就自旋扩散机理而言,它具有20-30nm的波长,这与差示扫描量热法和动态力学分析的结果非常吻合。为了在分子水平上检查共混物的可混溶性,研究了在旋转框架中质子晶格弛豫的行为。在分子水平上热固性共混物的均匀性完全取决于共混物的组成。贫PCL的ER / PCL共混物(例如70/30)显示出单一的均匀无定形相,并且分子链在分段范围内紧密混合。富含PCL的混合物在有关旋转框架中质子自旋晶格弛豫时间的实验中显示出双指数衰减,归因于非晶相和结晶相。在非晶区域,环氧树脂和PCL的分子链在分子水平上紧密混合。 (C)2003 Wiley Periodicals,Inc. [参考:54]

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