磷元素杂化双联六臂星形聚合物/聚丙烯复合材料的制备及阻燃性能

Preparation and Flame Retardant Properties of Hybrid Containing-Phosphorus Double Linked Six Arm Star Polymer/Polypropylene Composites

以二氯磷酸苯酯(PDCP)、乙二醇(EG)、氯磷酸二苯酯(DPCP)、六氯环三磷腈(HCCP)为原料,三乙胺(TEA)为缚酸剂,合成磷元素杂化双联六臂星形聚合物(DLSASP),利用双辊开放式热炼机和平板硫化成型机制备磷元素杂化双联六臂星形聚合物/聚丙烯(DLSASP/PP)复合材料。红外光谱、凝胶渗透色谱表征DLSASP的结构,氧指数(LOI)测定、热重分析、微型量热研究DLSASP/PP复合材料的阻燃性能、热稳定性能、燃烧性能,扫描电镜、X射线光电子能谱表征炭层形貌及组成,利用Flynn-Wall-Ozawa(FWO)法计算复合材料的热降解活化能(E_a)。结果表明,随着DLSASP添加量的提高,初始分解温度(T_(5%))、最大分解速率温度(T_(max))、最大失重速率(MMLR)、热释放速率峰值(PHRR)和总热释放量(THR)呈降低趋势,LOI和残重率均呈升高趋势;当DLSASP添加量为30%时,平均活化能为117.86 kJ/mol。

A double linked six arm star polymer (DLSASP) was synthesized by phenyl dichlorophosphate(PDCP), ethylene glycol(EG), diphenyl chlorophosphate(DPCP), hydroxyethyl methylacrylate (HCCP), using triethylamine (TEA) as acid binding agent. The DLSASP/PP composites were prepared by the polymer and polypropylene mixing. The structure and average molecular weight of DLSASP were characterized by FT-IR and gel permeation chromatography (GPC). The flame retardancy, thermal stability and combustion properties of DLSASP/PP composites were investigated by limit oxygen index(LOI), TGA and microscale combustion calorimetry (MCC);the morphology and composition of the char layer was investigated by SEM and XPS. The thermal decomposition activation energy (Ea) of composites were calculated by Flynn-Wall-Ozawa(FWO) method. The results show that with the increase of DLSASP addition, the temperature of 5% mass loss (T5%), temperature of maximum decomposition rate (Tmax), maximum mass loss rate(MMLR), peak heat release rate (PHRR) and total heat release (THR) decrease, but LOI and the residual mass show an increasing trend. When the amount of DLSASP is 30%, the average activation energy is 117.86 kJ/mol.