一步法制备苯基次膦酸铝及阻燃应用

A Novel Preparation of Aluminum Phenylphosphinate and Its Flame Retardancy Application

在水相中以苯膦二氯和十八水硫酸铝为原料,采用一步法反应,合成了无卤阻燃剂苯基次膦酸铝(BPAAl)。采用1HNMR、31PNMR、FTIR、ICP对产品结构进行表征,并对其反应条件进行探讨,得到最优条件为:苯膦二氯滴加温度5℃,反应温度90℃、反应时间3 h,硫酸铝浓度3 mol/L,在该条件下产率达89.6%。热重分析结果表明,产品起始失重温度在350℃,热稳定性好,具备优良阻燃剂的特征。并研究了BPA-Al在尼龙6中的应用,结果表明,添加量达到10%时,经过阻燃改性的PA6材料极限氧指数达到30%、UL94垂直燃烧达到V-0级,阻燃性能显著提高;拉伸强度达到84.9 k Pa,力学性能好。

A novel one-step preparation of halogen-free flame retardant aluminum phenylphosphinate（BPA-Al） from the raw materials of dichlorophenylphosphine and aluminium sulfate octadecahydrate in aqueous phase system was studied.The molecular structure of the sample was characterized by means of ^1HNMR,31PNMR,FTIR and ICP.Under the optimal reaction conditions,the adding temperature of dichlorophenylphosphine 5 ℃,reaction temperature 90 ℃,reaction time 3 h,the concentration of aluminium sulfate 3 mol/L,the yield of BPA-Al was up to 89.6%.The thermal stability of the product was investigated in detail by TG-DTA,which reveals that the product＇ s thermal stability is consistent with the initial decomposition temperature of the excellent flame retardant is 350 ℃.The application of BPA-Al to Nylon 6（PA6） was investigated.The results show that the flame retardancy of PA6 was significantly enhanced,with the LOI of the modified PA6 reaching 30% and the UL94 of the vertical burning reaching the level of V-0 when the volume of addition was 10%.Meanwhile,the modified PA6 also exhibited excellent mechanical property,with the tensile strength reaching 84.9 k Pa.