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首页> 外文期刊>Journal of Applied Polymer Science >Synthesis, characterization, and curing behavior of carborane-containing benzoxazine resins with excellent thermal and thermo-oxidative stability
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Synthesis, characterization, and curing behavior of carborane-containing benzoxazine resins with excellent thermal and thermo-oxidative stability

机译：具有优异的热和热氧化稳定性的含碳硼烷的苯并恶嗪树脂的合成，表征和固化行为

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摘要

Two benzoxazine precursors bearing carborane moiety (1 and 2) were designed and synthesized successfully by the Mannich reaction of corresponding carborane bisphenol (3 and 4) with aniline and formaldehyde in 1,4-dioxane. The obtained precursors were characterized by using multiple spectroscopic techniques including GPC, FTIR, H-1 NMR, C-13 NMR, and B-11 NMR. Nonisothermal DSC studies showed that precursor 1 owned lower apparent activation energies (E-a) than 2. The optimum curing processes of benzoxazine precursors were also obtained on the basis of DSC data. TGA analyses manifested that the incorporation of carborane moiety endowed the obtained benzoxazine resins (cured 1 and 2) with excellent thermal stability and unique thermo-oxidative stability. The T-d data showed that the initial degradation of both cured 1 and 2 under nitrogen and air was postponed to some extent owing to the shielding effect of carborane moiety on adjacent organic fragments. At higher temperature three-dimensional polymer networks with B-O-B and B-C linkages were formed as chars by the reaction of carborane cage with atmospheric moisture, degradation products such as phenolic hydroxyl, and oxygen (under air). Under nitrogen this network hindered the motion of radicals formed at elevated temperature and thus inhibited further polymer degradation processes. While under air, the formed boron-rich networks could hardly be further oxidized into carbon dioxide so that the carborane-containing benzoxazine resins also showed very high char yields. (c) 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016, 133, 43488.
机译：通过相应的碳硼烷双酚（3和4）与苯胺和甲醛在1,4-二恶烷中的曼尼希反应，成功设计和合成了两个带有碳硼烷部分（1和2）的苯并恶嗪前体。通过使用包括GPC，FTIR，H-1 NMR，C-13 NMR和B-11 NMR在内的多种光谱技术对获得的前体进行表征。非等温DSC研究表明，前驱体1的表观活化能（E-a）比2低。根据DSC数据，还获得了苯并恶嗪前驱体的最佳固化过程。 TGA分析表明，碳硼烷部分的引入赋予了获得的苯并恶嗪树脂（固化的1和2）优异的热稳定性和独特的热氧化稳定性。 T-d数据表明，由于碳硼烷部分对相邻有机片段的屏蔽作用，在氮气和空气下固化的1和2的初始降解在一定程度上被推迟。在较高的温度下，通过碳硼烷笼与大气中的水分，降解产物（如酚羟基）和氧气（在空气中）反应，形成了具有B-O-B和B-C键的三维聚合物网络为炭。在氮气下，该网络阻碍了在高温下形成的自由基的运动，因此抑制了进一步的聚合物降解过程。当在空气中时，形成的富硼网络很难进一步氧化成二氧化碳，因此含碳硼烷的苯并恶嗪树脂也显示出很高的炭收率。 （c）2016 Wiley Periodicals，Inc. J. Appl。 Polym。科学2016，133，43488。

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