新型无卤阻燃剂二乙基次膦酸铝的合成及阻燃应用

Synthesis and Application of Novel Halogen-Free Flame Retardant Aluminum Diethylphosphinate

使用双引发剂合成新型无卤阻燃剂二乙基次膦酸铝(Al Pi).当反应温度为80℃、反应时间为2 h、硫酸铝溶液浓度为0.1 mol/L、pH位于2.0~2.5时,产率为94.4%.产品结构通过FT-IR、ICP、~1H NMR、^(31)P NMR等分析手段表征,热重分析(TG)结果(T_(1%)=391.88℃,T_(5%)=429.38℃)表明产物热稳定性良好.当Al Pi在尼龙66(PA66)中添加量为15%时,垂直燃烧测试(UL-94)达V-0级,极限氧指数(LOI)达33.2%,阻燃性能明显提高,且冲击强度、弯曲强度等力学性能指数仍保持在材料可使用范围内.

Aluminum diethylphosphinate （A1Pi）was synthesized by di-initiator. The optimal reaction conditions were explored, and the yield of A1Pi is up to 94.4% under the conditions that the reaction temperature, time, concentration of aluminum sulfate solution and pH are 80 ℃, 2 h, 0.1 mol/L and 2.0-2.5, respectively. The molecular structure of the sample was characterized by FT-IR, ICP, ^1H NMR and 3,p NMR. The result of thermal stability of the products stated that T1% and T5% are up to 391.88 ℃ and 429.38 ℃ respectively, which could meet decomposition temperature of the excellent flame retardant. The application of A1Pi to Nylon 66（PA66）was investigated. When the content is 15%, the LOI to 33.2% and UL94 to V-0, the flame retardant of PA66 has been significantly enhanced. And the bending strength and impact strength still have been remained at reasonable range.