阻燃剂磷酰密胺的合成与应用

Synthesis and A pplication of Flame Retardant PhosphoryI Melamine

以三聚氰胺钠盐和三氯氧磷为原料,合成了阻燃剂磷酰密胺(磷酰三聚氰胺)。最佳工艺条件为氮气保护下,以氯仿为溶剂,三聚氰胺钠盐溶解后,缓慢滴加三氯氧磷,三聚氰胺钠盐与三氯氧磷的摩尔比为1:1.05,控制温度为60℃,保温反应7 h,加蒸馏水反应至无氯化氢气体产生后抽滤,用冰水纯化处理,得到产物,产率为90.5%。通过红外光谱(FTIR)、核磁共振氢谱(^(1)H-NMR)对产物进行了表征,通过差热分析(TG-DTA)分析了产物的热稳定性能,将产物应用于886不饱和树脂,进行了极限氧指数(LOI)测定、垂直燃烧测试及力学测试。结果表明,产物初始分解温度为275℃,具有较好的热稳定性及较高的残炭率;将产物应用于886不饱和树脂材料后,材料具有较好的成炭性及阻燃效果,同时,还具有增塑性。

A novel flame retardant,phosphoryl melamine was synthesized from sodium melamine and phosphorus oxychloride.The optimal conditions were selected as follows:n(sodium melamine):n(phosphorus oxychloride)=1:1.05 while trichloromethane as the solvent.Phosphorus oxychloride was added dropwise after sodium melamine was dissolved and reacted for 7 h at 60 C under nitrogen atmosphere,distilled water was added to react until no hydrogen chloride gas was produced and then filtered,finally purified with ice water,the yield could reach 90.5%.The product was characterized by FTIR,^(1)H-NMR.The thermal stability of the product was tested by TG-DTA.The limit oxygen index(LOI),vertical flammability and mechanical property was tested when it was applied to 886 unsaturated resin.Results showed that the product began to decompose at 275℃,it had good thermal stability and high carbon residue rate.The product presented certain plasticization and a good effect on antiflaming when it was applied to 886 unsaturated resin.