阻燃成炭剂笼状1-氧基磷杂-4-三甲基硅氧甲基-2,6,7-三氧杂双环[2.2.2]辛烷酯的合成与应用

Synthesis of Antiflaming Charring Agent Caged 1-Oxyphospha-4-trimethylsiloxy-2,6,7-trioxabicyclo[2.2.2]octane Ester

1-氧基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)与三甲基氯硅烷反应合成阻燃成炭剂笼状1-氧基磷杂-4-三甲基硅氧甲基-2,6,7-三氧杂双环[2.2.2]辛烷酯(PTSPA)。探讨了不同溶剂、反应温度和反应物配比对产物产率的影响,最佳反应条件是以二氧六环为溶剂,三乙胺为缚酸剂,PEPA与三甲基氯硅烷的物质的量比为1∶1.15,95℃反应8h,产率为91.6%。通过FT IR、1 H NMR、元素分析、极限氧指数及差热分析等技术表征了产物的结构及性能。实验表明,目标产物有较好的阻燃成炭性和热稳定性。

Antiflaming charring agent caged 1-oxyphospha-4-trimethylsiloxy-2,6,7-thioxabicyclo [2.2.2]- octane ester （PTSPA） was synthesized from 1-oxy phospha-4-（hydroxymethyl）-2, 6, 7-trioxabicyclo [-2.2.2] octane （PEPA） and trimethylchlorosilane. The effects of different solvent, reaction temperature and ratio of raw materials on product yield were studied. The optimal conditions were obtained as follows： The mole ratio of PEPA and trimethylchlorosilane 1 ： 1.15, dioxane as solvent,triethylamine as the bind- ing acid agent,reaction time of 8 h and reaction temperature at 95℃. The yield was 91.6% . The structure and properties of the flame retardant products were characterized by using FT IR, 1H NMR, elemental a- nalysis, limiting oxygen index and TG-DTA analysis techniques. The product showed good charring property and thermal stability.