阻燃成炭剂二甲基硅氧基双笼环磷酸酯的合成

1-氧基磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)与二甲基二氯硅烷反应合成阻燃成炭剂——二甲基硅氧基双笼环磷酸酯,即二甲基硅酸二{1-氧基磷杂-2,6,7-三氧杂双环[2.2.2]辛烷-(4)-甲}酯(DSDE)。考察了不同溶剂、反应温度和反应物配比对产物产率的影响,得到了最佳的反应条件是PEPA与二甲基二氯硅烷的摩尔比为2.16∶1,产率达92.6%。通过FTIR、1HNMR、元素分析、差热分析及极限氧指数表征了产物的结构及性能。研究表明,目标产物有较好的阻燃成炭性和热稳定性。

Synthesis of Flame Charring Agent Dimethicone Double Cage Phosphate

Flame charring agent caged dimethicone double cage phosphate were synthesized from 1-oxy phospha-4- (hydroxymethyl)-2, 6, 7- trioxabicyclo [2. 2. 2] octane (PEPA) and dimethyldichlorosilane, it was dimethyl silicate di{1-oxy phospha- 2, 6, 7-trioxabicyclo[2. 2. 2]octane -(4)- methyl} ester (DSDE). The effects of different solvent, eaction temperature and amount ratio of substance on product yield was discussed, the optimal conditions were selected as follows PEPA and dimethyldichlorosilane in molar ratios 2.16:1, the yield was 92.6%. The structure and properties of flame retardant products was characterized by using FTIR, 1H-NMR, elemental analysis, TG-DTA analysis and limiting oxygen index techniques. Experiments showed the product had a good char and thermal stability.