Synthesis of a caged bicyclic phosphates derived anhydride and its performance as a flame-retardant curing agent for epoxy resins
Synthesis of a caged bicyclic phosphates derived anhydride and its performance as a flame-retardant curing agent for epoxy resins
复制标题
笼状双环磷酸酯衍生酸酐的合成及其作为环氧树脂阻燃固化剂的性能
DOI：
10.1002/pat.4565
复制
发表时间：
2019-05-01
影响因子：
3.4
通讯作者：
Guo, Chuigen
中科院分区：
文献类型：
--
作者：
Ma, Tongtong;Li, Liping;Guo, Chuigen
合成了一种新型固化阻燃剂PEPA-TMAC。用傅里叶变换红外光谱（FTIR）和核磁共振（NMR）表征了其化学结构。研究了PEPA-TMAC作为部分固化剂与另一种酸酐组合用于商业环氧树脂（EP）的用途。差示扫描量热法（DSC）结果表明，PEPA-TMAC是一种有效的EP固化剂。动态力学分析（DMA）结果表明，随着PEPA-TMAC的加入，EP复合材料的玻璃化转变温度（T-g）和交联密度（V-e）呈上升趋势。锥形量热仪测试结果表明，随着PEPA-TMAC含量的增加，EP复合材料的峰值热释放速率（PHRR）、总热释放速率（THR）、发烟速率（SPR）和总发烟量（TSP）均显著降低。热重分析表明，PEPA-TMAC的加入大大增加了燃烧过程中的残炭量。用SEM观察了残炭的形貌，结果表明PEPA-TMAC的加入大大提高了EP复合材料的稳定性。热重分析（TGA）、X射线能谱（EDS）和红外光谱（FTIR）分析结果表明，PEPA-TMAC能促进EP复合材料燃烧过程中凝聚相中的磷-碳复合物形成炭化层，从而起到阻燃作用。
A novel curing and flame-retardant agent (PEPA-TMAC) was successfully synthesized. The chemical structure was characterized by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR). Use of PEPA-TMAC as part of the curing agent in combination with another anhydride for a commercial epoxy resin (EP) was studied. Results of differential scanning calorimetry (DSC) indicated that PEPA-TMAC was an effective curing agent for EP. The dynamic mechanical analysis (DMA) results showed that the glass transition temperature (T-g) and cross-linking density (V-e) of EP composites exhibited an increase trend with the addition of PEPA-TMAC. The limiting oxygen index (LOI) value of EP composites reached 26.9%, and the cone calorimeter results indicated that peak heat release rate (PHRR), total heat release (THR), smoke produce rate (SPR), and total smoke produce (TSP) remarkably decreased with increasing PEPA-TMAC content. TGA data showed that the addition of PEPA-TMAC greatly increased the amount of residual char during combustion. The morphology of the residual char was studied by SEM and showed that the addition of PEPA-TMAC greatly increased the stability of EP composites. The thermogravimetric analysis (TGA), energy-dispersive X-ray spectroscopy (EDS), and FTIR results revealed the flame-retardant mechanism that PEPA-TMAC can promote the formation of charred layers with the phospho-carbonaceous complexes in the condensed phase during burning of EP composites.