富勒烯C_(60)接枝马来酸聚合物铅盐的制备与表征

Preparation and Characterization of Fullerene C_(60)-grafted Maleic Acid Copolymer Lead Salt

以富勒烯C60和马来酸为原料合成得到一种新型富勒烯C60接枝马来酸聚合物,C60接枝马来酸聚合物再与硝酸铅反应得到C60接枝马来酸聚合物铅盐。通过单因素方法探讨了pH、反应物物料比、反应温度以及反应时间对C60接枝马来酸聚合物铅盐中铅含量的影响,获得其最佳合成工艺条件为:pH=6.92,C60接枝马来酸聚合物和硝酸铅的摩尔比为1∶7,反应时间2 h,反应温度30℃,该条件所得C60接枝马来酸聚合物铅盐中铅质量分数为56.09%。同时采用FT-IR、UV、GPC、AAS、XRD及XPS等测试手段对产物结构进行了表征。采用差热和热重分析法对C60接枝马来酸聚合物铅盐的热稳定性进行了研究,结果表明,在空气气氛下,DTA分解峰值温度为275、370、462℃,失重率为43.6%,表明产物热稳定性良好。

A novel C60-grafted maleic acid copolymer was prepared using C60 and maleic acid. And then the C60-grafted acid copolymer lead salt additives were prepared using C60-grafted maleic acid copolymer and lead nitrate to modify the burning rates of solid propellants. To obtain the higher content of lead in C60-grafted maleic acid copolymer lead salt, the C60-grafted maleic acid copolymer was coordinated in the presence of lead nitrate. The effect of pH, molar ratio of C60-grafted maleic acid copolymer and lead ni- trate, reaction temperature and time on the content of lead in the C60-grafted maleic acid copolymer lead salt were investigated by a single-factor method. The optimum reaction condition of 56.09% lead content in C60-grafted maleic acid copolymer lead salt was obtained in pH -- 6.92, molar ratio of C60-grafted ma- leic acid copolymer and lead nitrate 1 ： 7, reaction temperature 30 ℃, and reaction time 2.0 h. The chemical structures of the C60-grafted maleic acid copolymer lead salt were characterized by FT-IR, UV- vis, GPC, AAS, XRD and XPS analyses. The thermal stability of the C60-grafted maleic acid copolymer lead salt was also investigated by DSC, DTA and TG analyses. Three discrete regions of thermal decomposition were observed in the DTA curve at 275, 370 and 462 ℃ respectively. The C60-grafted maleic acid copolymer lead salt had three-steps weight loss, overall weight-loss was 43.6% in the TG curve, which showed good thermal stability.