Huo Siqi, Yang Shuang, Wang Jun, Cheng Jianwen, Zhang Qianqian, Hu Yefa, Ding Guoping, Zhang Qiaoxin, Song Pingan
School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan 430070, People's Republic of China; Center for Future Materials, University of Southern Queensland, Toowoomba 4350, Australia.
School of Mechanical and Electronic Engineering, Wuhan University of Technology, Wuhan 430070, People's Republic of China; Institute of Advanced Material Manufacturing Equipment and Technology, Wuhan University of Technology, Wuhan 430070, People's Republic of China.
J Hazard Mater. 2020 Mar 15;386:121984. doi: 10.1016/j.jhazmat.2019.121984. Epub 2019 Dec 26.
The development of phosphorus-containing flame retardants combining good compatibility with matrix, low curing temperature, and mechanically reinforcing effect has remained a major challenge. Herein, we reported the synthesis of a liquid flame-retardant curing agent (DA) via the nucleophilic substitution between diphenylphosphinic chloride and 1-(3-aminopropyl)-imidazole (AI). DA exhibited good blending and latency towards epoxy resin (EP) at room temperature. According to DSC studies, DA could rapidly cure EP at moderate temperature. Compared with EP/AI sample, EP/DA samples displayed comparable or higher glass transition temperature (T) and enhanced mechanical properties due to the introduction of rigid diphenylphosphinyl group and improved cross-linking density. Moreover, DA improved the flame-retardant performances of EP thermoset. For instance, the LOI and UL94 rating of EP/DA-16 sample achieved 37.2 % and V-0, respectively. In addition, the peak of heat release rate (PHRR), average of heat release rate (AHRR), fire growth rate (FIGRA), and total heat release (THR) for EP/DA-16 sample reduced by 32 %, 42 %, 28 % and 27 % in comparison to EP/AI sample, respectively. DA was characterized by its good compatibility with EP, moderate curing temperature, fast curing rate, suitable thermal latency, mechanical reinforcing and flame-retardant effects, and thus it had a broad application prospect in various industrial fields.
开发出与基体具有良好相容性、低固化温度且具有机械增强效果的含磷阻燃剂仍然是一项重大挑战。在此,我们报道了通过二苯基次膦酰氯与1-(3-氨丙基)-咪唑(AI)之间的亲核取代反应合成一种液体阻燃固化剂(DA)。DA在室温下对环氧树脂(EP)表现出良好的共混性和潜伏性。根据DSC研究,DA能在中等温度下快速固化EP。与EP/AI样品相比,EP/DA样品由于引入了刚性二苯基膦酰基并提高了交联密度,显示出相当或更高的玻璃化转变温度(T)以及增强的机械性能。此外,DA提高了EP热固性材料的阻燃性能。例如,EP/DA-16样品的极限氧指数(LOI)和UL94等级分别达到37.2%和V-0。此外,与EP/AI样品相比,EP/DA-16样品的热释放速率峰值(PHRR)、平均热释放速率(AHRR)、火灾增长速率(FIGRA)和总热释放(THR)分别降低了32%、42%、28%和27%。DA的特点是与EP具有良好的相容性、中等固化温度、快速固化速率、合适的热潜伏性、机械增强和阻燃效果,因此在各个工业领域具有广阔的应用前景。