磷-硼杂化聚合物/环氧树脂复合材料的制备及阻燃性能

以二氯磷酸苯酯（PDCP）、硼酸双甘油酯（DGB）为原料，通过逐步聚合得到磷-硼杂化聚合物（PDCP-DGB），PDCP-DGB与环氧树脂共混体系经交联固化制备磷硼元素共杂化环氧树脂基（PDCP-DGB/EP）阻燃复合材料。利用FTIR、核磁共振波谱仪（NMR）、凝胶渗透色谱仪（GPC）、TG、氧指数（LOI）测定仪、微型量热仪、SEM和XPS对PDCP-DGB和PDCP-DGB/EP复合材料进行表征。结果表明，随着PDCP-DGB质量分数的增加，PDCP-DGB/EP复合材料最大分解速率温度升高，残重率提高，LOI上升，烟密度等级和最大烟密度降低，热释放速率峰值（PHRR）降低，总热释放量（THR）减小；PDCP-DGB有利于提高PDCP-DGB/EP复合材料的热稳定性能和阻燃性能，但对其力学性能影响较小；当PDCP-DGB质量分数为15wt%时，PDCP-DGB/EP复合材料LOI达到28.3%，较纯EP提高了47.4%，垂直燃烧（UL-94）等级达到V-0级；THR、PHRR分别降低了28%、23%，残炭率升高了5.11%；SEM图像显示，PDCP-DGB/EP复合材料的残炭表面得到很好的改善，致密、连续且平整。 

Preparation and flame retardant properties of phosphorus-boron hybrid polymer/epoxy resin composites

A containing phosphorus-boron hybrid polymer (PDCP-DGB) was synthesized by step-reaction polymerization using phenyl dichlorophosphate (PDCP) and boric diglyceride (DGB) as the raw materials. A series of PDCP-DGB/epoxy resin (EP) flame retardant composites were prepared by crosslinking and curing between PDCP-DGB and EP blends. The structure of PDCP-DGB was characterized by FTIR and nuclear magnetic resonance. The PDCP-DGB/EP composites were investigated by gel permeation chromatography (GPC), TG, limit oxygen index (LOI), microscale combustion calorimeter, SEM and XPS. The results indicate that with the increase of mass fraction of PDCP-DGB, the temperature of maximum decomposition rate of PDCP-DGB/EP composite, the residual mass rate and the LOI improve, but the smoke density level, maximum smoke density, peak value of heat release rate (PHRR) and total heat release (THR) decrease. PDCP-DGB is conducive to improve the thermal stability and flame retardant properties of PDCP-DGB/EP composite and has little influence on the mechanical properties of PDCP-DGB/EP composites. When the mass fraction of PDCP-DGB reaches 15wt%, the LOI reaches 28.3%, which is 47.4% higher than that of the pure EP, the vertical burning (UL-94) reaches V-0 level, the THR and PHRR decrease by 28% and 23%, respectively, the residual mass rate increases by 5.11%. SEM images show that the carbon residue surface of PDCP-DGB/EP composites is well improved, which is dense, continuous and smooth.