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One-Pot Synthesis and Characterization of Novel Shape-Memory Poly(ε-Caprolactone) Based Polyurethane-Epoxy Co-networks with Diels–Alder Couplings

机译:基于Diels-Alder偶联的新型基于形状记忆聚(ε-己内酯)的聚氨酯-环氧共网络的单罐合成和表征

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摘要

The present work aimed at the preparation and investigation of different epoxy-polyurethane (EP-PU) co-networks. The EP-PU co-networks were obtained by applying two different synthetic strategies, in which the coupling element, the Diels–Alder (DA) adduct, was prepared previously or formed “in situ” in the reaction between furan functionalized polyurethane and furfuryl amine-diglycidyl ether bisphenol-A oligomers (FA_DGEBA). For the synthesis of these EP-PU networks, poly(ε-caprolactone)-diol (PCD, Mn = 2 kg/mol) and poly(ε-caprolactone) (PCL) with different molecular weights (Mn = 10, 25 and 50 kg/mol) and 1,6-hexamethylenediisocyanate (HDI) were used. The EP-PU co-networks were characterized by Attenuated Total Reflectance Fourier-Transform Infrared spectroscopy (AT-FT-IR), differential scanning calorimetry (DSC) and dynamical mechanical analysis (DMA). Scanning electron microscopy (SEM) was applied to assess the morphology of the EP-PU samples. It was demonstrated that the stress–strain curves for the EP-PUs could be interpreted based on the Standard Linear Solid (SLS) model. The DMA traces of some EP-PUs (depending on the composition and the synthetic method) revealed a plateau-like region above the melting temperature (Tm) of PCL confirming the presence of cross-linked structure. This feature predicted shape memory (SM) behavior for these EP-PU samples. Indeed, very good shape fixity and moderate shape recovery were obtained. The shape recovery processes of these EP-PU samples were described using double exponential decay functions.
机译:当前的工作旨在准备和研究不同的环氧-聚氨酯(EP-PU)共网络。 EP-PU共网络是通过应用两种不同的合成策略而获得的,其中偶合元素Diels–Alder(DA)加合物是事先制备的或在呋喃官能化的聚氨酯与糠胺之间的反应中“原位”形成的。 -二缩水甘油基醚双酚A低聚物(FA_DGEBA)。为了合成这些EP-PU网络,需要使用不同分子量(Mn = 10、25和50)的聚(ε-己内酯)-二醇(PCD,Mn = 2 kg / mol)和聚(ε-己内酯)(PCL) (kg / mol)和1,6-六亚甲基二异氰酸酯(HDI)。 EP-PU共网络的特征在于衰减全反射傅立叶变换红外光谱(AT-FT-IR),差示扫描量热法(DSC)和动态力学分析(DMA)。扫描电子显微镜(SEM)用于评估EP-PU样品的形态。结果表明,可以根据标准线性实体(SLS)模型解释EP-PU的应力-应变曲线。一些EP-PU的DMA痕迹(取决于组成和合成方法)显示出高于PCL熔化温度(Tm)的平台状区域,证实了交联结构的存在。此功能可以预测这些EP-PU样品的形状记忆(SM)行为。实际上,获得了非常好的形状固定性和适度的形状恢复性。使用双指数衰减函数描述了这些EP-PU样品的形状恢复过程。

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