磷化酚醛树脂的合成及其阻燃性能研究

以苯酚,三氯氧磷(POCl3),热塑性酚醛树脂(FR)为原料,三乙胺(Et3N)为缚酸剂合成了一种新型的含磷阻燃剂-磷化酚醛树脂(FR-P),采用红外光谱(FT IR),核磁共振磷谱(31PNMR),电感耦合等离子体发射光谱(ICP)及热重分析(TG)对聚合物的结构及热性能进行了表征,探讨了合成中的各因素对反应的影响,得出了最佳的合成工艺条件,并将合成的化合物用于PC的阻燃,采用热分析法、极限氧指数法(LOI)对阻燃体系的热性能和阻燃性能进行了表征,并与PC/FR阻燃体系进行了比较。研究结果表明,FR-P在高温下的热稳定性和成炭性与FR相比有较大的提高,它能促进PC热降解时成炭,使PC的热分解速率降低,当FR-P添加量为15%时,阻燃体系的LOI达31%,且通过UL94V-1级测试,其阻燃效果远远好于FR。

Study on the Synthesis of Phosphorous Phenolic Resin and Its Flame Retardance

A novel phosohorus-containing flame retardant-phosphorous phenolic resin(FR-P) was synthesized from phenol,phosphoryl trichloride(POCl_3) and phenol formaldehyde resin(FR),while triethylamine(Et_3N) was used as a deacid reagent.The structure and thermal properties of the resin were tested with FT IR,()~(31)P NMR spectroscopy,inductance coupling plasma emission spectroscopy(ICP) and thermogravimetric analysis(TG).The effect of various factors on the synthesis was also studied to find the appropriate synthetic conditions.The resin was used as flame retardant for preparing flame retardant PC resins.The thermal properties and flame retardance of this system was investigated by TGA and limiting oxygen index(LOI) values and the flame retardance of this system was compared with PC/FR.The results showed that the thermal property and charred property in high temperture of FR-P were better than FR.FR-P could make more char in the degradation of PC and the decomposition rate of PC was decreased.When the content of FR-P was 15%,the LOI value of the flame retardant PC was 31% and through UL94V-1 grade test which was better than FR.