Synthesis of a Novel P/N/S-Containing Flame Retardant and Its Application in Epoxy Resin: Thermal Property, Flame Retardance, and Pyrolysis Behavior
Synthesis of a Novel P/N/S-Containing Flame Retardant and Its Application in Epoxy Resin: Thermal Property, Flame Retardance, and Pyrolysis Behavior
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新型 P/N/S 阻燃剂的合成及其在环氧树脂中的应用：热性能、阻燃性和热解行为
DOI：
10.1021/acs.iecr.6b03416
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发表时间：
2016-11-09
影响因子：
4.2
通讯作者：
Weng, Jiabao
中科院分区：
文献类型：
--
作者：
Jian, Rongkun;Wang, Pan;Weng, Jiabao
设计了DOPO与2-氨基苯并噻唑（ABZ）的复配体系，制备了含磷、氮、硫的DOPO-ABZ阻燃剂，并用高分辨质谱（HRMS）、红外光谱（FTIR）、核磁共振氢谱（1H NMR）和31磷谱（31 P NMR）对其结构进行了表征。通过DSC和TGA发现，与EP相比，EP/DOPO-ABZ制剂的热稳定性降低。分别通过LOI、UL-94和锥形量热仪测试评价了材料的燃烧性能。结果表明，DOPO-ABZ对EP具有阻燃作用，EP/7. 5 wt % DOPO-ABZ阻燃体系达到V-0级，氧指数达到33.5%; DOPO-ABZ用量增加到10wt%时，可进一步抑制弯曲环氧树脂的热释放和烟释放。最后，通过TG-FTIR和py-GC/MS研究了DOPO-ABZ的阻燃机理，发现DOPO-ABZ通过生成含磷自由基和含氮/硫挥发物发挥气相阻燃作用。
The combination of DOPO and 2-aminobenzothiazole (ABZ) was designed to develop P/N/S-containing flame retardant DOPO-ABZ, and its chemical structure was confirmed by HRMS, FTIR, and 1H and 31P NMR. The reduced thermal stability of EP/DOPO-ABZ formulations was found through DSC and TGA, as compared to that of EP. Fire properties were evaluated by LOI, UL-94, and cone calorimeter tests, respectively. The results indicated that DOPO-ABZ imparted flame retardance to EP, and that EP/7.5 wt % DOPO-ABZ passed the V-0 rating, and acquired a LOI value of 33.5%; moreover, when the loading of DOPO-ABZ increased to 10 wt %, it could further suppress the heat release and smoke release of the curved epoxy resin. Finally, the flame-retardant mechanism was studied by TG-FTIR and py-GC/MS, disclosing that DOPO-ABZ exerted predominant gaseous-phase activity of fire inhibition via generating phosphorus-containing free radicals and nitrogen/sulfur-containing volatiles.