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Solid-state and time domain NMR to elucidate degradation behavior of thermally aged poly (urea-urethane)
Polymer Degradation and Stability ( IF 5.9 ) Pub Date : 2019-12-11 , DOI: 10.1016/j.polymdegradstab.2019.109052
Kaori Numata , Atsushi Asano , Yasumoto Nakazawa

We have demonstrated that solid-state and time-domain Nuclear Magnetic Resonance spectroscopy (NMR) techniques are effective in monitoring the degradation site of poly (urea-urethane). We prepared two types of commercial poly (urea-urethane), Urethane-A and Urethane-B, and aged them at 100 °C for up to 10000 h. We performed tensile strength tests and solid-state NMR experiments, in which 13C and 15N NMR spectra and T2 were collected. The tensile strength of Urethane-A decreased, increased and decreased again, whereas that of Urethane-B decreased at a lower rate with aging. Solid-state NMR experiments clearly showed that the degradation of Urethane-A was caused by molecular chain scission and cross-linking in its urea bonds, and that of Urethane-B occurred owing to molecular chain scission in its urethane bonds. T2 had three components, short T2 (T2S), intermediate T2 (T2I) and long T2 (T2L), whose fractions were xS, xI and xL, respectively. We have demonstrated that molecular chain scission in urea bonds decreases xS and increases xL, and that in urethane bonds increases T2I and T2L without changing all the T2 fractions.



中文翻译:

固态和时域NMR阐明热老化的聚(脲-尿烷)的降解行为

我们已经证明,固态和时域核磁共振波谱(NMR)技术可有效地监测聚(脲-氨基甲酸酯)的降解位点。我们准备了两种类型的商品化聚脲(Urea-Aurethane),Urethane-A和Urethane-B,并在100°C下老化了10000 h。我们进行了抗张强度测试和固态NMR实验,其中13 C和15 N NMR光谱和T 2被收集。氨基甲酸酯-A的抗张强度随着老化而降低,增加和降低,而氨基甲酸酯-B的抗张强度以较低的速率降低。固态NMR实验清楚地表明,氨基甲酸酯-A的降解是由其脲键的分子链断裂和交联引起的,而氨基甲酸酯-B的降解是由于其氨基甲酸酯键的分子链断裂引起的。T 2具有三个成分,短T 2T 2 S),中间T 2T 2 I)和长T 2T 2 L),其分数为x SXX大号,分别。我们已经证明,脲键的分子链断裂降低x S并增加x L,而氨基甲酸酯键的分子链断裂增加T 2 IT 2 L而不改变所有的T 2分数。

更新日期:2019-12-11
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