新型膨胀型阻燃剂聚磷酰氯螺环硼酸二乙醇胺酯的合成与表征

Synthesis and Characterization of a Novel Flame Retardant Poly POSDB

以二乙醇胺和硼酸为原料,甲苯为带水剂,合成中间体硼酸二乙醇胺酯(DEAB),再与三氯氧磷反应合成新型的集磷、氮、硼于一体的阻燃剂聚磷酰氯螺环硼酸二乙醇胺酯(PPCSDB).使用红外光谱和核磁共振对产物的结构进行初步表征.通过TGA评价其热稳定性,热重分析表明:化合物初始分解温度为195℃,800℃残炭率为34.8%.同时探讨反应条件对化合物产率的影响,结果表明化合物合成的较佳条件为:物料摩尔比为1∶1,反应时间10 h,以乙腈为溶剂.

Diethanolamine borate was obtained by boric acid reacting with diethanol amine and using toluene as water carrying agent.Then a novel flame retardant poly phosphorus oxychloridespirocyclic diethanolamine borate（POSDB） was prepared with phosphorus oxychloride containing phosphous nitrogen and boron.The structure of compounds was characterized by Fourier transform infrared（FTIR）1HNMR.The thermal stabilities of the flame retardant were studied by thermogravimetric analysis the initial decomposition temperature of poly（phosphorus oxychloridespirocyclic diethanolamine borate） was 195℃,and residue was 34.8 % at 800 ℃,which indicateds poly（phosphorus oxychloridespirocyclic diethanolamine borate） had excellent charring ability.The result showed that the optimal condition of poly（phosphorus oxychloridespirocyclic diethanolamine borate） reaction was n（PPC） ∶n（DEAB） =1∶1,the reaction temperature about 80 ℃ and reaction time about 10 h with acetonitrile as solvent.