中国塑料 ›› 2009, Vol. 23 ›› Issue (09): 71-75 .DOI: 10.19491/j.issn.1001-9278.2009.09.016

• 助剂 • 上一篇    下一篇

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

胡小平 杨俊 李晓燕 李少先 李鸿波 周元林   

  1. 西南科技大学
  • 收稿日期:2009-03-25 修回日期:2009-05-12 出版日期:2009-09-26 发布日期:2009-09-26

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

HU Xiao-ping;YANG Jun;LI Xiao-yan;LI Shao-xian;LI Hong-bo;ZHOU Yuan-lin   

  • Received:2009-03-25 Revised:2009-05-12 Online:2009-09-26 Published:2009-09-26
  • Contact: HU Xiao-Ping

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),通过测试特性黏度确定了最佳合成条件为: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(APP)复配,应用于低密度聚乙烯(PE-LD)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 %,UL94达到V-0级。

关键词: 双螺环, 己二胺, 制备, 熔融聚合, 膨胀型阻燃剂

Abstract: A novel phosphorouse-nitrogen structure containing intumescent flame retardant poly(3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro-[5.5] undecane-3,9-dioxide) hexamethylene diamine (SPHD) was prepared by 3,9-dichloro-2,4,8,10-tetraoxa-3,9-diphosphaspiro-[5.5] undecane-3,9-dioxide ( SPDPC ) and hexamethylene diamine (HD) through melting ploymerization in N2. The effects of ratio of material and reaction temperature on relative molecular weight were studied by intrinsic viscosity test. The results showed that the highest yield was 84 %, and the optimal reaction conditions were as follows: polymerization time, the molar ratio of SPDPC to hexamethylene diamine, reaction temperature were about 4 hours, 1/1.1, 165 ℃, respectively. The molecular structure and thermal stability of SPHD were characterized by FT-IR,1H-NMR and TG, separately. Results showed that the products could be obtained successfully by melt polymerization, which had good thermal stability. The flame retardancy of SPHD was studied when used in PE-LD with addition of ammonium polyphosphate (APP), when the content of SPHD was 15 %, the limiting oxygen index(LOI) value was 27.2 %and V-0 rating of UL94 could be achieved.

Key words: 3, 9-dichloro-2, 4, 8, 10-tetraoxa-3, 9-diphosphaspiro-[5.5] undecane-3, 9-dioxide, hexamethylene diamine, preparation, melt polymerization, intumescent flame retardant