含磷苯并咪唑基铜配合物合成及阻燃环氧树脂的性能

为了改性环氧树脂阻燃性能,通过取代反应和缩合反应制备一种新型含磷/氮二元杂化物—磷酸4-(1H-苯并咪唑-2-基)-苯基酯二苯酯(PBIm),并作为有机官能团与乙酸铜-水合物反应合成含磷苯并咪唑基铜配合物阻燃剂PBIm-Cu,将其添加到环氧树脂(EP)中,制备阻燃环氧树脂复合材料(PBIm-Cu/EP).通过红外光谱、X-射线光电子能谱、核磁氢谱和核磁磷谱对阻燃剂PBIm和PBIm-Cu进行结构表征.采用热重分析仪(TGA)、极限氧指数测定仪(LOI)和锥形量热仪(CCA)测试复合材料的热稳定性和阻燃性能.PBIm-Cu质量分数为7%的PBIm-Cu/EP体系在垂直燃烧测试中通过了 V-1级,LOI增加到31.6%,并且,峰值放热速率(PHRR)、总热释放量(THR)和总排烟量(TSP)较纯EP分别降低64%,41%和43%,残重率达到了26.7%.SEM 结果显示:PBIm-Cu/EP材料燃烧后碳层表面光滑连续且致密.

Synthesis of phosphorus-containing benzimidazole-based copper complex and properties of flame-retardant epoxy resin

In order to modify the flame retardant property of epoxy resin, a new type of phosphorous/nitrogen dihydric compound, phosphoric acid 4-(1H-benzoimidazol-2-yl)-phenyl ester diphenyl ester (PBIm), was prepared by substitution reaction and condensation reaction, and used as an organic functional group to react with copper acetate-hydrate to synthesize phosphorus-containing benzimidazole-based copper complex flame retardant PBIm-Cu. It was added to epoxy resin (EP) to prepare flame retardant epoxy resin composite (PBIm-Cu /EP). The structure of the flame retardants PBIm and PBIm-Cu was characterized by infrared spectroscopy, X-ray photoelectron spectroscopy, hydrogen nuclear magnetic spectrum and phosphorus nuclear magnetic spectrum. Thermogravimetric analyzer (TGA), limiting oxygen index (LOI) and cone calorimeter (CCA) were used to test the thermal stability and flame retardancy of composite materials. The PBIm-Cu/EP system with a PBIm-Cu mass fraction of 7% passed the V-1 level in the vertical combustion test, and the LOI was increased to 31.6%. Moreover, compared with pure EP, the peak heat release rate (PHRR), total heat release rate (THR) and total smoke exhaust rate (TSP) were decreased by 64%, 41% and 43%, respectively, and the residual weight rate reached 26.7%. SEM results show that the surface of the carbon layer after the combustion of PBIm-Cu/EP material is smooth, continuous and dense.