新型磷–氮–卤三系阻燃剂的合成及其在PP中的应用

Synthesis of Phosphorus-Nitrogen-Halogen Ternary Systems Flame Retardant and Its Application in PP

五硫化二磷、对卤苯酚和二乙胺经过两步反应,合成了两种新型磷–氮–卤三系阻燃剂:O,O’–二(4–卤代苯基)二硫代磷酸–N,N–二乙铵(4–XC_6H_4O)_2PS_2NH_2Et_2[X=Br(1),Cl(2)],用元素分析、傅里叶变换红外光谱、核磁共振氢谱、紫外–可见吸收光谱和热重分析测定了两种阻燃剂的结构和热稳定性,并测定了它们在聚丙烯(PP)材料中的阻燃性能。热分析结果表明:两种阻燃剂的热稳定高,热分解温度分别为234.8℃和200.7℃;阻燃剂在PP中的质量分数为30%时,两种阻燃剂的极限氧指数(LOI)分别为28.5%和27.1%,垂直燃烧等级达到UL94 V–0级,表明所合成的两种阻燃剂具有良好的阻燃性能和潜在应用前景。

Two new phosphorus-nitrogen-halogen-containing flame retardants,(4–XC6H4O)2PS2NH2Et2 [X=Br(1),Cl(2)] were synthesized via the reaction of phosphorus pentasulfide,4-halophenol and diethylamine in two steps,and their chemical structures were characterized by elemental analysis,fourier transform infrared spectoscopy ,1H NMR spectra and ultraviolet visible spectroscopy. The thermal stabilities of two flame retardants were tested by thermal gravity analysis(TGA),and their flame retardant properties for polypropylene (PP)material were measured by limited oxygen index (LOI) and vertical burning (UL94). The results of TGA show that the initial decomposition temperatures of two flame retardants are 234.8℃and 200.7℃respectively,which indicates the two prepared compounds possess excellent thermal stability. The two flame retardant modified PP materials reach to UL94 V–0 rating and the LOI values reach to 28.5%and 27.1%with 30%two flame retardants respectively. The results indicate that the two prepared phosphorus-nitrogen-halogen-containing flame retardants have good flame retardant effect for PP materials and potential application prospects.