5,5-二甲基-2-磷杂-1,3-二噁烷-2-基烯丙基磷酸酯的制备

Preparation of 5,5-Dimethyl-2-phospha-1,3dioxan-2-yl-allyl Phosphate

以新戊二醇、三氯氧磷、烯丙醇和金属钠为原料,经过2步反应合成了新型反应型阻燃化合物5,5-二甲基-2-磷杂-1,3-二烷-2-基烯丙基磷酸酯。采用元素分析、FTIR、MS和1H NMR等测试技术对其结构进行了表征。对合成工艺进行了探讨,当n(Na)∶n(烯丙醇)=1∶2,于冰水浴反应2 h,再于30℃反应6 h时,产率可达55.5%。TG分析显示,该化合物的起始分解温度为130.2℃,800℃时仍有23%的残炭率,说明该化合物具有较好的热稳定性和成炭性。

A novel reactive flame retardant,5,5-dimethyl-2-phospha-1,3-dioxan-2-yl-allyl phosphate,was synthesized by reacting neopentyl glycol,phosphorus oxychloride,allyl alcohol with sodium through two steps.The title compound was characterized by elemental analysis,FTIR,MS and 1H NMR.The thermal properties of the title compound were studied by TG and DSC techniques.The results show that the synthesized compound is consistent with the expected structure.The yield of the compound is 55.5% with the molar ratio of allyl alcohol to sodium being 2∶ 1,the reaction temperature being at 0 ℃ using an ice bath for 2 h at first,and then at 30 ℃ for 6 h.The TG curves show that the initial thermal decomposition temperature of the compound is about 130.2 ℃,and there is about 23% char residue left at 800 ℃,indicating that the title compound has a good thermal stability and a char forming capability.