N-(5,5-二甲基-1,3,2-二氧杂己内磷酰基)取代苯甲醛腙的合成及其阻燃性能

Synthesis and Flame Retardance of N-(5,5-Dimethyl-2-oxo- 1,3,2-dioxaphosphoyl) benzoylhydrazone Derivatives

采用 5 ,5 二甲基 2 氯 2 氧 1,3,2 二氧磷杂己内磷酸酯和水合肼及取代苯甲醛反应 ,合成了N (5 ,5 二甲基 1,3,2 二氧杂己内磷酰基 )取代苯甲醛腙系列化合物 (3a～ 3h)。通过元素分析、IR、1HNMR和MS对其结构进行了表征。对部分化合物的热重和差热分析表明 ,化合物的最大失重速率温区在 2 2 0～4 0 0℃ ,这与大部分高分子材料的热氧降解温区重叠 ,具有很好的阻燃配伍性能。化合物 3a～ 3h在醇酸清漆和环氧树脂 (E 4 4 )中的初步阻燃试验表明 ,有很好的阻燃性能。

The title compounds, 3a～3h, were synthesized from 5,5-dimethyl-2-chloro-2-oxo-1,3,2- dioxaphosphosrinane, hydrazine hydrate and substituted benzaldehydes. The structures of the compounds were confirmed by IR, 1H NMR, MS and elemental analysis. TG and DTA analysis showed that some of the compounds e.g. 3e began to decompose at 220 ℃ and have certain thermal stability. They decomposed rapidly at temperature range 220～400 ℃. Prelimary test showed the title compounds have high flame retardance activity for alkyd resin and epoxy E-44 varnish.