5,5-二甲基-2-磷杂-1,3-二噁烷-2-基丙烯酰胺甲氧基磷酸酯的合成

Synthesis of 5,5-dimethyl-2-phospha-1,3-dioxan-2-yl acrylamide methoxy phosphate

摘要:

以新戊二醇、三氯氧磷及N-羟甲基丙烯酰胺为原料，在三乙胺作为缚酸剂、氯化亚铜作催化剂的条件下，合成了新型膨胀型阻燃剂5,5-二甲基-2-磷杂-1,3-二噁烷-2-基丙烯酰胺甲氧基磷酸酯，采用元素分析、FTIR、1H NMR等分析测试技术对其结构进行了表征。当n(N-羟甲基丙烯酰胺):n(三乙胺)=1:1，CuCl占N-羟甲基丙烯酰胺质量分数1.5%时，先冰水浴反应2h，再室温反应10h，产物产量达到75.3%。并利用TG、DSC热分析技术对该化合物的热性能进行了分析。TG曲线显示其初始分解温度是210℃，800℃时的残炭率约40%，说明该化合物具有较好的热稳定性和成炭性。

Abstract:

A novel intumescent flame retardant (IFR) 5,5-dimethyl-2-phospha-1,3-dioxan-2-yl acrylamide methoxy phosphate was synthesized with neopentyl glycol, phosphorus oxychloride and N-hydroxymethyl acrylamide, using triethylamine as acid acceptor and CuCl as catalyst. The structure of the compound was characterized by elemental analysis, FTIR and 1H NMR. The yield of the compound was 75.3% with the molar ratio of N-hydroxymethyl acrylamide to triethylamine being 1:1, the mass fraction of CuCl being 1.5% N-hydroxymethyl acrylamide, and the reaction in ice-water bath for 2 h at first and then in room temperature for10 h. And the thermal properties of the compound were tested by TG and DSC techniques. The TG curves of the compound indicates that the initial thermal decomposition temperature is about 210℃, and there is about 40% char residue left at 800℃, indicating that the title compound has a good thermal stability and a char forming capability.