Wang Hao, Wang Yinjie, Su Yan, Yu Chuang, Han Jia, Liu Jiping
School of Materials Science and Engineering, Beijing Institute of Technology, 5 Zhongguancun South Street, Haidian District, Beijing 100081, China.
Polymers (Basel). 2024 Apr 27;16(9):1224. doi: 10.3390/polym16091224.
The flammability of epoxy resins and knowing how to achieve curing are particularly important factors during use. A novel approach for enhancing the fire resistance and reducing the smoke emission of epoxy resin during the curing process is suggested, which involves the utilization of a three-source integrated polymerization intumescent flame-retardant. In this study, the synthesis of poly 4,4-diaminodiphenylsulfone spirocyclic pentaerythritol bisphosphonate (PCS) is achieved through using solution polymerization, utilizing 4,4'-diaminodiphenylsulfone (DDS) and spirocyclic pentaerythritol bisphosphorate disphosphoryl chloride (SPDPC) as initial components. Following that, the EP underwent the inclusion of PCS to examine its resistance to heat, its ability to prevent flames, its effectiveness in reducing smoke and its curing effect. Compared to the unmodified epoxy resin, the addition of PCS can not only cure the epoxy resin, but also decompose before the epoxy resin and has a good carbonization effect. With the addition of 7 wt.% PCS, the LOI value can achieve 31.2% and successfully pass the UL-94 test with a V-0 rating. Moreover, the cone calorimeter experiment demonstrated a noteworthy decline of 59.7% in the maximum heat release rate (pHRR), 63.7% in overall heat release (THR), and 42.3% in total smoke generation (TSP). Based on the examination of TG-FTIR and SEM findings, there is ample evidence to suggest that PCS, functioning as a phosphorus-nitrogen intumescent flame-retardant that combines three origins, has the potential to exhibit a favorable flame-retardant impact in both its gas and condensed phases.
环氧树脂的可燃性以及如何实现固化是使用过程中特别重要的因素。本文提出了一种在固化过程中提高环氧树脂耐火性并减少烟雾排放的新方法，该方法涉及使用三源一体化聚合膨胀型阻燃剂。在本研究中，通过溶液聚合，以4,4'-二氨基二苯砜（DDS）和螺环季戊四醇双磷酸酯二磷酰氯（SPDPC）为起始原料，合成了聚4,4-二氨基二苯砜螺环季戊四醇双磷酸酯（PCS）。随后，将PCS加入到环氧树脂中，以研究其耐热性、阻燃能力、减少烟雾的效果以及固化效果。与未改性的环氧树脂相比，添加PCS不仅可以使环氧树脂固化，还能在环氧树脂之前分解并具有良好的碳化效果。添加7 wt.%的PCS时，极限氧指数（LOI）值可达到31.2%，并成功通过UL-94测试，达到V-0等级。此外，锥形量热仪实验表明，最大热释放速率（pHRR）显著下降了59.7%，总热释放（THR）下降了63.7%，总烟雾生成量（TSP）下降了42.3%。基于热重-傅里叶变换红外光谱（TG-FTIR）和扫描电子显微镜（SEM）结果的研究，有充分证据表明，作为一种具有三种来源的磷-氮膨胀型阻燃剂，PCS在气相和凝聚相都有可能表现出良好的阻燃效果。
