三嗪三苯基次膦酸仲丁酯化合物的制备及其应用

Preparation and Application of Sec-butyl Triazine and Three Phenyl Hypophosphorous Acid Compound

以三聚氯氰和苯基次膦酸二仲丁酯为原料合成了磷、氮协同阻燃剂2,4,6-三(O-仲丁基-苯基次膦酰基)-1,3,5-三嗪化合物,对各步反应进行了优化;用红外光谱、核磁等表征了产物的结构,并用极限氧指数方法测试了产物的阻燃性能等。结果表明,最佳反应条件为:三聚氯氰和苯基次膦酸二仲丁酯的摩尔比为1∶3.2,100℃持续反应5h,同时分馏出反应生成的2-氯丁烷,蒸馏出有机溶剂,重结晶得2,4,6-三(O-仲丁基-苯基次膦酰基)-1,3,5-三嗪,产率为89.4%;该产物阻燃聚对苯二甲酸丁二醇酯(PBT)以及该产物和三聚氰胺氰尿酸盐(MCA)、三聚氰胺聚磷酸盐(MPP)分别阻燃PBT的最高极限氧指数分别为21%、30%、26%,且融滴均较慢,成炭性均较好。

A new phosphorus and nitrogen synergistic flame retardant,2,4,6-three(O-sec-butylphenyl phosphinic acyl)-1,3,5-triazine,was prepared from tricyanogen chloride and Phenyl hypophoaphoeous acid two sec-butyl.Each reaction condition was optimized.The optimal reaction condition was as follow:n(tricyanogen chloride):n(phenyl hypophoaphoeous acid dibutyl)was 1∶3.2,reaction time was 5h at 100 ℃ with fractionating the 2-chlorobutane generated by the reaction,the target product was obtained after distilling organic solvents and recrystallization with ayield of 89.4 %.The structure of the product was characterized by FTIR,1 H-NMR and the flame retardant properties of the product were measured by limited oxygen index technique.The highest limited oxygen index of the product flame retarded PBT,the product and MCA flame retarded PBT,the product and MPP flame retarded PBT were 21 %,30 %,26 %,respectively.