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氢氧化铝纳米片的制备及其对膨胀型阻燃环氧复合材料的阻燃性和热稳定性的协同作用

Preparation and synergistic effect of aluminum hydroxide nanoplates on the fire resistance and thermal stability of the intumescent flame retardant epoxy composite.

作者信息

Doanh Truong Cong, Thi Nhung Hac, Nguyen Hong Tham, Oanh Ho Thi, Doan Tien Dat, Tuyen Nguyen Duc, Vu Minh-Tan, Hoang Mai Ha

机构信息

Hanoi University of Industry 298 Cau Dien, Bac Tu Liem Hanoi 12000 Vietnam.

Institute of Chemistry, Vietnam Academy of Science and Technology 18 Hoang Quoc Viet, Cau Giay Hanoi 10072 Vietnam

出版信息

RSC Adv. 2025 May 20;15(21):16814-16825. doi: 10.1039/d5ra00231a. eCollection 2025 May 15.

DOI:10.1039/d5ra00231a
PMID:40395801
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC12091328/
Abstract

Aluminum hydroxide nanoplates (nATH), with an average particle size of about 350-450 nm and a thickness of 30 nm, were successfully synthesized through a hydrothermal process using an Al(OH) gel precursor. The ATH nanoplates were then surface-treated with organic compounds and incorporated into an intumescent flame-retardant epoxy system containing polyethyleneimine-modified ammonium polyphosphate (APP@PEI). Among them, the combination of APP@PEI and PEI-treated nATH (nATH) exhibited the highest synergistic effect on the fire resistance and thermal stability of epoxy resin due to the superior dispersion of the nanoplates. Additionally, the optimal mass ratio of two flame retardant additives was examined. As a result, a nanocomposite containing 3 wt% nATH and 7 wt% APP@PEI exhibited the best flame resistance and thermal-oxidative stability. This nanocomposite reached a V-0 rating in the UL-94 vertical burning test with a high limiting oxygen index value of 31.1%, and a substantial char yield of 17.98% at 900 °C. Char residues of samples were analyzed by Fourier transform infrared spectroscopy, X-ray diffraction, and scanning electron microscopy coupled with energy dispersive X-ray analysis to investigate the reasonable flame retardant mechanism. The results demonstrated that the formation of highly thermally stable aluminum phosphates played an important role in the augmentation of the flame retardancy in the condensed phase. Furthermore, tension and Izod impact tests indicated that the presence of nATH notably increased the mechanical properties of composite loading APP@PEI. This combination provides a promising approach for intumescent flame retardant applications in epoxy resin.

摘要

氢氧化铝纳米片(nATH)平均粒径约为350 - 450纳米,厚度为30纳米,通过水热法使用Al(OH)凝胶前驱体成功合成。然后用有机化合物对ATH纳米片进行表面处理,并将其掺入含有聚乙烯亚胺改性聚磷酸铵(APP@PEI)的膨胀型阻燃环氧树脂体系中。其中,APP@PEI与经PEI处理的nATH(nATH)的组合对环氧树脂的耐火性和热稳定性表现出最高的协同效应,这归因于纳米片的优异分散性。此外,还研究了两种阻燃添加剂的最佳质量比。结果,含有3 wt% nATH和7 wt% APP@PEI的纳米复合材料表现出最佳的阻燃性和热氧化稳定性。该纳米复合材料在UL - 94垂直燃烧试验中达到V - 0等级,极限氧指数值高达31.1%,在900℃时残炭率为17.98%。通过傅里叶变换红外光谱、X射线衍射以及扫描电子显微镜结合能量色散X射线分析对样品的残炭进行分析,以研究合理的阻燃机理。结果表明,高热稳定性磷酸铝的形成在凝聚相阻燃性增强中起重要作用。此外,拉伸和悬臂梁冲击试验表明,nATH的存在显著提高了负载APP@PEI的复合材料的力学性能。这种组合为环氧树脂的膨胀型阻燃应用提供了一种有前景的方法。

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