二乙氧基丙烯酰胺甲氧基硫代磷酸酯(DAMT)的合成及应用

Synthesis and Application of Diethoxy-Acrylamide Methoxy Thiophosphate

由N-羟甲基丙烯酰胺与二乙氧基硫代磷酰氯合成了新型的含磷、硫、氮的反应型、膨胀型阻燃剂二乙氧基丙烯酰胺甲氧基硫代磷酸酯(DAMT)。通过元素分析、FTIR、1H NMR、MS测试技术表征了标题化合物的结构。结果表明,所合成的标题化合物的结构与预期的一致;当加入与N-羟甲基丙烯酰胺等摩尔的三乙胺作缚酸剂及质量分数为N-羟甲基丙烯酰胺1%的氯化亚铜(CuC l)作催化剂时,DAMT的产率可高达80%,最佳反应温度为0～5℃;当DAMT与丙烯腈的共聚物中所占质量分数为20%时,极限氧指数(LO I)值可达27%。由阻燃聚丙烯腈共聚物燃烧后的炭残渣扫描电子显微镜可见,炭残渣表面有很多泡状结构,而横截面为蜂窝状结构,表明该阻燃剂为膨胀型阻燃剂。

A novel phosphorus, sulfur and nitrogen containing intumscent flame retardant （IFR）, diethoxyacrylamide methoxy thiophosphate （DAMT）, was synthesized by reacting N-hydroxymethyl-acrylamide with diethoxythiophosphoryl chloride. DAMT was characterized by elemental analysis, FFIR, ^1 H NMR, and MS. The structure of DAMT was confirmed. The yield of DAMT was 80% when the molar ratio of acid capturing agent triethylamine to N-hydroxymethyl-acrylamide was 1 ： 1, and the mass fraction of the catalyst CuCl was 1% of N-hydroxymethyl-acrylamide. The optimized reaction temperature ranged from 0 ℃ to 5 ℃. The limiting oxygen index（LOI） value reached 27% when the mass fraction of DAMT in the DAMT-acrylonitrile copolymer was 20%. The SEM micrographs of the char residue of the flame retarded copolymer revealed that the surface of the char residue was bubbly structured, and the cross section was honeycomb structure, indicating DAMT was a intumescent flame retardant.