Synthesis of solid reactive organophosphorus-nitrogen flame retardant and its application in epoxy resin,Journal of Applied Polymer Science

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Synthesis of solid reactive organophosphorus-nitrogen flame retardant and its application in epoxy resin
Journal of Applied Polymer Science ( IF 2.7 ) Pub Date : 2023-06-15 , DOI: 10.1002/app.54282
Chaojiu Chen ₁ , Xinlong Wang ₁ , Tao Luo ₁ , Honggang Zhen ₁ , Xiuying Yang ₁ , Lin Yang ₁ , Zhengjuan Yan ₁

Affiliation

A solid reactive organophosphorus-nitrogen flame retardant 4N-BDP was devised and synthesized in order to address the flaws of the widely used organophosphorus flame retardants BDP as well as the issue of flame retardant modification of epoxy resin (EP). A series of flame-retardant EP composites were prepared by adding 4N-BDP and BDP to EP in a specific proportion. The flame-retardant properties of the two were compared, and the flame-retardant mechanism of 4N-BDP was deeply analyzed. The results of the UL-94 test revealed that sample 4N-BDP-6 obtained the greatest V-0 level, while BDP-6 had no level, when the addition ratio of flame retardant was 8.03%. In the cone calorimeter test, the peak smoke production rate (pSPR) and total smoke production (TSP) of BDP-6 were not significantly different from those of pure EP. In contrast, TSP and pSPR of 4N-BDP-6 decreased by 39.50% and 50.00% respectively compared with EP. Compared with BDP, 4N-BDP shows better flame retardancy and smoke suppression performance, which can significantly improve the fire resistance of EP. The flame-retardant mechanism of 4N-BDP was resolved by scanning electron microscopy, XPS, and thermogravimetric analysis/infrared spectrometry. 4N-BDP can increase the residual carbon rate of the composites, improve the residual carbon strength, play an excellent condensed phase flame retardant effect, and avoid further decomposition of the materials. In the gas phase, the decomposition of 4N-BDP produces PO·, PO₂· and NH₃, which play a good quenching effect and dilution effect. The escape of NH₃ will leave bubbles in the residual carbon, making the residual carbon more fluffy, further improving the ability of heat insulation and oxygen insulation, and enhancing the flame retardant effect of the condensed phase. In general, the flame-retardant mechanism of 4N-BDP is a synergistic combination of condensed phase and gas phase flame retardant mechanism. This work provides a new approach to improve the defects of organophosphorus flame retardant BDP commonly used in the market and enhance the fire resistance of EP.

中文翻译：

固体反应型有机磷氮阻燃剂的合成及其在环氧树脂中的应用

针对目前广泛使用的有机磷系阻燃剂BDP的缺陷以及环氧树脂（EP）的阻燃改性问题，设计合成了固体反应型有机磷氮系阻燃剂4N-BDP。通过在EP中按一定比例添加4N-BDP和BDP制备了一系列阻燃EP复合材料。比较了两者的阻燃性能，深入分析了4N-BDP的阻燃机理。UL-94测试结果显示，当阻燃剂添加比例为8.03%时，样品4N-BDP-6获得了最大的V-0水平，而BDP-6则没有水平。在锥形量热仪测试中，BDP-6的峰值发烟量（pSPR）和总发烟量（TSP）与纯EP没有显着差异。相比之下，4N-BDP-6的TSP和pSPR与EP相比分别降低了39.50%和50.00%。与BDP相比，4N-BDP表现出更好的阻燃、抑烟性能，可显着提高EP的耐火性能。通过扫描电子显微镜、XPS、热重分析/红外光谱分析解析了4N-BDP的阻燃机理。4N-BDP可以提高复合材料的残碳率，提高残碳强度，发挥优异的凝聚相阻燃效果，避免材料进一步分解。在气相中，4N-BDP分解生成PO·，PO 可显着提高EP的耐火性能。通过扫描电子显微镜、XPS、热重分析/红外光谱分析解析了4N-BDP的阻燃机理。4N-BDP可以提高复合材料的残碳率，提高残碳强度，发挥优异的凝聚相阻燃效果，避免材料进一步分解。在气相中，4N-BDP分解生成PO·，PO 可显着提高EP的耐火性能。通过扫描电子显微镜、XPS、热重分析/红外光谱分析解析了4N-BDP的阻燃机理。4N-BDP可以提高复合材料的残碳率，提高残碳强度，发挥优异的凝聚相阻燃效果，避免材料进一步分解。在气相中，4N-BDP分解生成PO·，PO₂ ·和NH ₃，起到良好的淬火作用和稀释作用。_{NH 3}的逸出会在残炭中留下气泡，使残炭更加蓬松，进一步提高隔热、隔氧能力，增强凝聚相的阻燃效果。总的来说，4N-BDP的阻燃机理是凝聚相阻燃机理和气相阻燃机理的协同组合。该工作为改善市场常用的有机磷阻燃剂BDP的缺陷、增强EP的耐火性能提供了新的途径。

更新日期：2023-06-15

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