熔融聚合法制备一种具有双螺环结构的膨胀型阻燃剂及其性能研究  

Properties of A Intumescent Flame Retardant Containing SPDPC Prepared by Melting Polymerization

作　　者：胡小平[1] 杨俊[1] 李晓燕[1] 李少先[1] 李鸿波[1] 周元林[1] 

机构地区：[1]西南科技大学材料科学与工程学院,四川绵阳621010

出　　处：《中国塑料》2009年第9期71-75,共5页China Plastics

基　　金：四川省教育厅青年基金(2006B049)

摘　　要：采用3,9二氯2,4,8,10四氧杂3,9二磷杂螺环[5,5]3,9二氧十一烷(SPDPC)与己二胺,在氮气保护下采用熔融聚合法合成了一种新型膨胀型阻燃剂螺环磷酸酯己二胺共聚物(SPHD),测试了产物的特性黏度。结果表明,SPHD的最佳合成条件为:反应温度165℃,n(SPDPC)/n(己二胺)=1/1.1,反应时间约4 h,产率达84%;采用红外光谱、核磁共振氢谱对共聚物SPHD进行了结构表征,证实了目标产物的成功制备;热重分析显示其具有良好的热稳定性;通过与聚磷酸铵复配,应用于低密度聚乙烯中,初步测试了其阻燃性能,当SPHD含量为15%时,复合材料的氧指数值为27.2%,UL 94达到V-0级。A novel phosphorouse/nitrogen containing intumescent flame retardant poly（3,9-dichlo- ro-2,4, 8, 10-tetraoxa-3, 9-diphosphaspiro-[-5, 5] undecane 3, 9 dioxide） hexamethylene diamine （SPHD） was prepared via melting ploymerization of 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro-[5,5] undecane-3,9-dioxide （ SPDPC ） and hexamethylene diamine （HD）. The effects of the molar ratio of materials and reaction temperature on the molecular weight of the product were studied. A high yield of 84% was obtained, and the optimal reaction conditions were as follows： polymerization time： 4 hours, the molar ratio of SPDPC to HD： 1/1. 1, reaction temperature： 165 ℃. The molecular structure was confirmed by FT-IR and 1H-NMR. TG showed the products possessed a good thermal stability. The obtained SPHD employed as a flame retardant together with ammonium polyphosphate in PELD. When the content of SPHD was 15 wt%, a limiting oxygen index of 27. 2% and UL 94 rate of V-0 were achieved.

关 键 词：双螺环 己二胺 制备 熔融聚合 膨胀型阻燃剂 

分 类 号：TQ314.248[化学工程—高聚物工业] TQ326.9