新型有机磷-氮协同阻燃剂的合成与应用  

Synthesis and Application of A Novel Organic P-N Synergistic Flame Retardant

作　　者：娄帅 仲柿成 谭榆斌 武文斌 王彦林[1] Lou Shuai;Zhong Shicheng;Tan Yubin;Wu Wenbin;Wang Yanlin(School of Chemistry and Life Sciences,Suzhou University of Science and Technology,Suzhou 215009,China;TianPing College of Suzhou University of Science and Technology,Suzhou 215011,China)

机构地区：[1]苏州科技大学化学与生命科学学院,江苏苏州215009 [2]苏州科技大学天平学院,江苏苏州215011

出　　处：《工程塑料应用》2023年第2期139-144,共6页Engineering Plastics Application

基　　金：2021年苏州科技大学校级通识教育任选课项目(2021TSY-31)。

摘　　要：以三聚氰胺钠盐和苯基磷酰二氯为原料,合成了新型有机磷-氮阻燃剂苯基磷酰二三聚氰胺(PPBM)。最佳合成工艺为:氮气保护下,三聚氰胺钠盐和苯基磷酰二氯的物质的量比为2.1∶1,三聚氰胺钠盐溶解于四氯化碳后,苯基磷酰二氯缓慢滴入,75℃下反应6 h后加蒸馏水反应1 h,抽滤,蒸馏水洗涤,干燥,收率为92.4%。傅里叶变换红外光谱、核磁共振氢谱的表征结果显示合成产物与目标化合物PPBM结构一致,热重-差热分析结果表明,PPBM具有良好的热稳定性和较高的残炭率。将PPBM应用于886A不饱和聚酯树脂中,垂直燃烧测试、极限氧指数测定的结果表明,PPBM具有较好的膨胀成炭性和优良的阻燃效果。通过燃烧后残炭的扫描电子显微镜表征分析了PPBM的阻燃机理,同时也进一步证明了PPBM具有良好的磷-氮协同增效阻燃性能。A novel organic phosphorus-nitrogen flame retardant phenylphosphonic bismelamine(PPBM)was synthesized using phenylphosphonic dichloride and sodium melamine as raw materials.The optimum synthesis process is as follows:under nitrogen protection,the molar ratio of sodium melamine and phenylphosphonic dichloride is 2.1∶1,phenylphosphonic dichloride is slowly dropped after sodium melamine is dissolved in carbon tetrachlorideand and they are reacted at 75℃for 6 h,then reacted with adding distilled water for 1 h,and then the synthesized product is filtered,finally washed with distilled water and dried,the yield is 92.4%.The product was characterized by FTIR and 1H NMR.The characterization results show that the product has the same structure with the target compound PPBM,and the thermal analysis shows that the product has good thermal stability and high carbon residue.The product was applied to 886A unsaturated polyester resin,the results of the vertical flammability,limiting oxygen index test show that phenylphosphonic bismelamine has good expansion charring property and flame retardancy effect.The flame retardant mechanism of the product was analyzed by SEM characterization of the carbon residue after combustion,the results further prove that the product has good phosphorus-nitrogen synergistic flame retardancy effect.

关 键 词：磷-氮协同阻燃剂 三聚氰胺钠盐 苯基磷酰二氯 苯基磷酰二三聚氰胺 膨胀成炭 

分 类 号：TQ314.24[化学工程—高聚物工业]