O,O-二乙基丙烯酰基膦酸酯的合成、表征及应用

Synthesis,Characterization and Application of O,O-Diethyl-acryloyl Phosphonate

以丙烯酰氯与亚磷酸二乙酯为反应物，合成了新型反应型磷系阻燃剂：O，O-二乙基丙烯酰基膦酸酯，将其与丙烯腈共聚得到了阻燃丙烯腈共聚物。通过元素分析、FTIR、1HNMR、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结构一致；当n（丙烯酰氯）：n（亚磷酸二乙酯）=1．5：1，反应温度在0—5℃时，标题化合物的产率达85％；标题化合物在阻燃丙烯腈共聚物中所占质量分数为20％时，极限氧指数（LOI）值可达26％，阻燃丙烯腈共聚物燃烧后的炭残渣扫描电镜（SEM）照片表明，炭残渣表面及横截面结构致密，符合凝聚相阻燃机理。该阻燃剂的合成及应用已申请中国专利（200808154245．4）。

A novel phosphorus-containing flame retardant, O, O-diethyl-acryloyl phosphonate was synthesized from acryloyl chloride and diethyl phosphite, and the fire-retarding copolyacrylonitrile was obtained through copolymerization of the title compound and acrylonitrile. The title compound was characterized by elemental analysis, FTIR, 1HNMR and MS. Results show that the structure of the title compound is in consistent with the expected one. The yield of the title compound is 85% under the conditions of the molar ratio （ 1.5：1 ） between acryloyl chloride and diethyl phosphite, and the optimized reaction temperature ranges from 0 ℃to 5 ℃. The limiting oxygen index（LOI） value can reach 26% when the mass fraction of the title compound in the copolymer is 20%. The scanning electron microscopy（SEM） photos of the char residue of the flame retarded copolyacrylonitrile show that the surface and the cross section of the char residue have tight structure, which conforms to condensed phase flame reistance mechanism. The synthesis and application of the fire retardants have been applied for patent of the People＇s Republic of China（200808154245.4）.