硅氮磷协同阻燃剂的合成及其阻燃性能

Synthesis and Flame Retardance of a Silicon,Nitrogen,Phosphorus Synergistic Flame Retardant

以三羟乙基异氰尿酸酯(赛克)、二甲基二氯硅烷(DMDCS)和1-氧代-1-磷杂-4-羟甲基-2,6,7-三氧杂双环[2.2.2]辛烷(PEPA)为原料,合成多元素协同阻燃剂异氰尿酸三{2-[二甲基(1-氧代-1-磷杂-2,6,7-三氧杂双环[2.2.2]辛烷基-4-甲氧基)硅氧基]乙基}酯(TPOSC),探讨反应温度对HCl气体放完所需时间的影响和反应物配比等对产物收率的影响。实验结果表明,以二氧六环为溶剂,在n(赛克)︰n(DMDCS)︰n(PEPA)=1.0︰3.0︰3.3、第一步在70℃反应7 h、第二步在90℃反应8 h的最优工艺条件下,收率可达92.1%。FTIR、1H NMR、热重分析等表征结果显示,合成的产物结构与目标产物一致,产物有较好的热稳定性,对聚丙烯阻燃成炭的效果好,且与三聚氰胺氰尿酸盐复配使用时具有很好的阻燃协同增效性。

A multi-element synergistic flame retardant, 1, 3, 5-tris{2- [dimethyl（1-oxo-1- phospha-2, 6, 7-trioxabicyclo [ 2.2.2 ] octalkyl-4-methyloxy）siloxy ] ethyl } isocyanurate（TPO SC）, was synthesized from 1, 3, 5-tris（2-hydroxyethyl） isocyanurate, dimethyldichlorosilane and 1-oxo- 1-phospha-4-hydroxymethyl-2, 6, 7-trioxabicyclo [2.2.2 ] octane（PEPA）, and was characterized by means of FTIR, ^1H NMR, and TG/DTA. The effect of reaction temperature on the reaction time when HCl was completely released and the influence of raw material ratio on the product yield were investigated. It was showed that, under the optimal conditions of dioxane as solvent, n（1, 3, 5-tris（2- hydroxyethyl）cyanurate） ： n（dimethyldichlorosilane） ： n（PEPA） 1.0 ： 3.0 ： 3.3, 70 ℃ and 7 h for the first step reaction, and 90 ℃ and 8 h for the second step reaction, the product yield could reach 92.1%. The characterization results verified the structure of the product. The product has excellent thermal stability and high flame-retardance efficiency for polypropylene（PP）. Besides, when it was mixed with melamine cyanurate and was applied to PP, high synergistic flame-retardance efficiency was found.