McReynolds Brandon T, Mojtabai Kavon D, Penners Nicole, Kim Gaeun, Lindholm Samantha, Lee Youngmin, McCoy John D, Chowdhury Sanchari
Department of Materials and Metallurgical Engineering, New Mexico Institute of Mining and Technology, Socorro, NM 87801, USA.
Department of Chemical Engineering, New Mexico Institute of Mining and Technology, Socorro, NM 87801, USA.
Polymers (Basel). 2023 Feb 23;15(5):1106. doi: 10.3390/polym15051106.
We studied the effect of side reactions on the reversibility of epoxy with thermoreversible Diels-Alder (DA) cycloadducts based on furan and maleimide chemistry. The most common side reaction is the maleimide homopolymerization which introduces irreversible crosslinking in the network adversely affecting the recyclability. The main challenge is that the temperatures at which maleimide homopolymerization can occur are approximately the same as the temperatures at which retro-DA (rDA) reactions depolymerize the networks. Here we conducted detailed studies on three different strategies to minimize the effect of the side reaction. First, we controlled the ratio of maleimide to furan to reduce the concentration of maleimide groups which diminishes the effects of the side reaction. Second, we applied a radical-reaction inhibitor. Inclusion of hydroquinone, a known free radical scavenger, is found to retard the onset of the side reaction both in the temperature sweep and isothermal measurements. Finally, we employed a new trismaleimide precursor that has a lower maleimide concentration and reduces the rate of the side reaction. Our results provide insights into how to minimize formation of irreversible crosslinking by side reactions in reversible DA materials using maleimides, which is important for their application as novel self-healing, recyclable, and 3D-printable materials.
我们研究了基于呋喃和马来酰亚胺化学的热可逆狄尔斯-阿尔德(DA)环加成物的副反应对环氧树脂可逆性的影响。最常见的副反应是马来酰亚胺均聚反应,该反应会在网络中引入不可逆交联,对可回收性产生不利影响。主要挑战在于,马来酰亚胺均聚反应可能发生的温度与逆DA(rDA)反应使网络解聚的温度大致相同。在此,我们对三种不同策略进行了详细研究,以尽量减少副反应的影响。首先,我们控制马来酰亚胺与呋喃的比例,以降低马来酰亚胺基团的浓度,从而减少副反应的影响。其次,我们应用了一种自由基反应抑制剂。研究发现,加入对苯二酚(一种已知的自由基清除剂)可在升温扫描和等温测量中延缓副反应的发生。最后,我们采用了一种新的三马来酰亚胺前体,其马来酰亚胺浓度较低,可降低副反应速率。我们的研究结果为如何在使用马来酰亚胺的可逆DA材料中通过副反应最小化不可逆交联的形成提供了见解,这对于它们作为新型自修复、可回收和3D可打印材料的应用非常重要。