新型磷-硅阻燃剂的合成及对聚丙烯的阻燃应用

Synthesis of Novel Phosphorus-Silicon Flame Retardant and Application for Polypropylene

以苯基膦酰二氯(BPOD)和甲基硅酸季戊四醇酯(MSPTA)为原料,制备了一种新型的磷-硅协同阻燃剂含硅二笼环苯基膦酸酯(BMSPTPP),即二(1-甲基-1-硅杂-2,6,7-三氧杂双环-[2,2,2]辛烷基-4-甲氧基)苯基膦酸酯。研究了反应时间、原料摩尔比、反应温度等因素对产率的影响,筛选出最合适的反应条件,将四氯乙烷作为溶剂,n(甲基硅酸季戊四醇酯):n(苯基膦酰二氯)=2.2∶1,在140℃下,反应10 h,最终产物收率能达到最高值91.8%。并通过对红外光谱、核磁共振谱和极限氧指数进行测试,表征了产品的结构和阻燃性能,结果表明,含硅二笼环苯基膦酸酯的热稳定性较好,应用于聚丙烯PP中,可以发挥出良好的协同阻燃效果和成炭性能。

A novel phosphorus-silicon synergistic flame retardant silicon-containing caged phenyl phosphate,bis(1-methyl-1-siza-2,6,7-trioxyheterobicyclo-[2,2,2]octanyl-4-methoxy)phenyl phosphonate(BMSPTPP),which was a new phosphorus-silicon flame retardant,was synthesized from phenylphosphoryl dichloride(BPOD)and 1-methyl-4-(hydroxylmethy1)-1-siliconhetero-poly-2,6,7-three-oxabicyclo-[2,2,2]-octane(MSPTA).The effect of reaction time,mole ratio of substance and temperature on the product yield was discussed.The optimal conditions for preparation were selected as follows:Tetrachloroethane as solvent,n(methyl silicate pentaerythritol)∶n(phenyl phosphoryl dichloride)=2.2∶1,reaction time was 10 h at 140℃,the yield of the final product was 91.8%.And the molecular structures of silicon-containing caged phenyl phosphate and its related performance measurement were determined by means of FTIR,1 H NMR spectrum and LOI technique.The results showed that,silicon-containing caged phenyl phosphate had good thermal stability,and the application of silicon-containing caged phenyl phosphate in PP,could play a good synergistic flame retardant effect and charring performance.