Ionita Daniela, Cristea Mariana, Gaina Constantin, Silion Mihaela, Simionescu Bogdan C
"Petru Poni" Institute of Macromolecular Chemistry, Aleea Grigore Ghica 41A, 700487 Iasi, Romania.
Polymers (Basel). 2023 Oct 9;15(19):4028. doi: 10.3390/polym15194028.
The present work is focused on polyester resins obtained from the diglycidyl ether of bisphenol A and anthracene modified 5-maleimidoisophthalic acid. Because the maleimide-anthracene Diels-Alder (DA) adduct is stable at high temperatures, it is considered a good option for high performance polymers. However, the information related to the retroDA reaction for this type of adduct is sometimes incoherent. A detailed thermal study (conventional TGA, HiRes TGA, MTGA, DSC, MDSC) was performed in order to establish whether the rDA reaction can be revealed for this type of anthracene modified polyester resins. The TGA method confirmed the cleavage of the anthracene-maleimide DA adduct, while the DSC demonstrated the presence of anthracene in the system. At high temperatures, unprotected maleimide homopolymerizes and/or reacts with allyl groups according to the -ene reaction. Therefore, the thermal DA reaction is not displayed anymore upon the subsequent cooling, and the glass transition region is registered at a higher temperature range during the second heating. The use of sample-controlled thermal analysis (HiRes TGA) and MTGA improved the TGA result; however, it was not possible to separate the very complex degradation processes that are interconnected.
本工作聚焦于由双酚A的二缩水甘油醚与蒽改性的5-马来酰亚胺间苯二甲酸制得的聚酯树脂。由于马来酰亚胺-蒽狄尔斯-阿尔德(DA)加合物在高温下稳定,它被认为是高性能聚合物的一个良好选择。然而,有关这类加合物的逆DA反应的信息有时并不一致。为了确定对于这类蒽改性聚酯树脂是否能揭示逆DA反应,进行了详细的热研究(常规热重分析、高分辨热重分析、调制式热重分析、差示扫描量热法、调制式差示扫描量热法)。热重分析方法证实了蒽-马来酰亚胺DA加合物的裂解,而差示扫描量热法表明体系中存在蒽。在高温下,未受保护的马来酰亚胺会根据烯反应进行均聚和/或与烯丙基反应。因此,在随后的冷却过程中热DA反应不再显现,并且在第二次加热期间玻璃化转变区域出现在更高的温度范围。使用样品控制热分析(高分辨热重分析)和调制式热重分析改善了热重分析结果;然而,不可能分离相互关联的非常复杂的降解过程。