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Aminobenzothiazole-substituted cyclotriphosphazene derivative as reactive flame retardant for epoxy resin
Reactive & Functional Polymers ( IF 4.5 ) Pub Date : 2019-11-09 , DOI: 10.1016/j.reactfunctpolym.2019.104412
Jianwen Cheng , Jun Wang , Shuang Yang , Qianqian Zhang , Yefa Hu , Guoping Ding , Siqi Huo

Aminobenzothiazole-substituted cyclotriphosphazene derivative (ABCP) was successfully synthesized and used as reactive flame retardant to improve the fire safety of epoxy resin (EP). The chemical structure of ABCP was confirmed by Fourier transform infrared spectroscopy (FTIR), 1H and 31P nuclear magnetic resonance (NMR), high-resolution mass spectroscopy (HR-MS) and elemental analysis (EA). The curing behavior, thermal stability, thermo-mechanical property and flame retardancy of the prepared EP systems were studied. The differential scanning calorimeter (DSC) results indicated that ABCP induced the anionic polymerization of EP and facilitated the addition reaction between EP and 4,4′-diamino-diphenyl sulfone (DDS). The thermogravimetric analysis (TGA) results indicated that ABCP accelerated the thermal degradation of EP matrix and contributed to the formation of more residual chars with better thermo-oxidative stability. The dynamic mechanical analysis (DMA) results indicated that EP/DDS/ABCP thermosets exhibited higher storage modulus at 50 °C and their glass transition temperature (Tg) values were slightly reduced by 6–10 °C, in comparison with EP/DDS thermoset. The combustion test results revealed the fire hazards of EP/DDS/ABCP thermosets were effectively reduced. Compared with EP/DDS thermoset, the limiting oxygen index (LOI) value of EP/DDS/ABCP-1.2 thermoset was increased to 31.2% and the sample passed UL94 V-0 rating; the average of heat release rate (av-HRR), peak of heat release rate (pk-HRR) and total heat release (THR) values of EP/DDS/ABCP-1.2 thermoset were reduced by 36.5%, 53.7% and 34.5%, respectively; particularly, the fire growth rate (FIGRA) of EP/DDS/ABCP-0.6 thermoset was reduced by half. The research on flame retardant mechanism disclosed that ABCP played dominated flame retardant effect in condensed phase.



中文翻译:

氨基苯并噻唑取代的环三磷腈衍生物作为环氧树脂的反应性阻燃剂

成功合成了氨基苯并噻唑取代的环三磷腈衍生物(ABCP),并用作反应性阻燃剂,以提高环氧树脂(EP)的防火安全性。ABCP的化学结构已通过傅立叶变换红外光谱(FTIR),1 H和31确认P核磁共振(NMR),高分辨率质谱(HR-MS)和元素分析(EA)。研究了所制备的EP体系的固化行为,热稳定性,热机械性能和阻燃性。差示扫描量热仪(DSC)的结果表明,ABCP诱导了EP的阴离子聚合,并促进了EP与4,4'-二氨基-二苯砜(DDS)之间的加成反应。热重分析(TGA)结果表明,ABCP促进了EP基体的热降解,并有助于形成更多的残炭,并具有更好的热氧化稳定性。动态力学分析(DMA)结果表明,EP / DDS / ABCP热固性材料在50°C时具有较高的储能模量,并且其玻璃化转变温度(T g)的值与EP / DDS热固性塑料相比,降低了6–10°C。燃烧测试结果表明,有效降低了EP / DDS / ABCP热固性材料的着火危险。与EP / DDS热固性材料相比,EP / DDS / ABCP-1.2热固性材料的极限氧指数(LOI)值提高到31.2%,样品通过UL94 V -0等级;EP / DDS / ABCP-1.2热固性树脂的平均放热率(av-HRR),最高放热率(pk-HRR)和总放热(THR)值分别降低了36.5%,53.7%和34.5% , 分别; 特别是,EP / DDS / ABCP-0.6热固性材料的着火率(FIGRA)降低了一半。阻燃机理的研究表明,ABCP在凝结相中起着主导的阻燃作用。

更新日期:2019-11-09
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