C_(60)丙二酸二(2,4,6-三硝基苯乙基)酯马来酸聚合物铅盐的合成

New method for synthesizing the lead salt of C_(60)-bis malonate maleic acid copolymer

以TNT和甲醛为原料,首先得到2,4,6-三硝基苯乙醇(TNPE),TNPE和丙二酰氯经酯化反应合成得到丙二酸二(2,4,6-三硝基苯乙基)酯(TNPEM),TNPEM与C60通过Bingel反应制备了C60丙二酸二(2,4,6-三硝基苯乙基)酯(FTNPEM)。FTNPEM再与马来酸和硝酸铅通过共聚合成盐反应得到含能的C60丙二酸二(2,4,6-三硝基苯乙基)酯马来酸聚合物铅盐5。采用FT-IR、UV-Vis、GPC、XPS、XRD等表征方法对聚合物及其铅盐的结构进行了分析。利用差热分析法(DTA)和热重分析法(TGA)对聚合物铅盐5的热稳定性及其对RDX的热分解催化作用进行了研究。结果表明,在空气气氛下,聚合物铅盐5初始分解峰值温度为239℃,表明产物热稳定性良好。对RDX热分解催化作用研究结果表明,聚合物铅盐5能加速RDX的分解,并使RDX分解峰温降低6℃。

The paper is inclined to bring about a new approach to synthesizing the lead salt of C60-bis（2,4,6-Trinitrophenethyl） Malonate maleic acid copolymer. To be exact,the bis（2,4,6-trinitrophenethyl） malonate（TNPEM） with a yield of 65% can be synthesized through esterification of malonyl dichloride and 2,4,6-trinitrophenyl ethanol（TNPE） through the reaction of TNT and the formaldehyde under a weak base condition. The new synthesis method we have developed can be stated in following steps. First of all,the synthesis can be done by using C60-bis（2,4,6-trinitrophenethyl）malonate（FTNPEM） with a yield of 37%（based on the consumed C60） through Bingel reaction of TNPEM and C60. C60-bis（2,4,6-trinitrophenethyl） malonate maleic acid copolymer with FTNPEM and maleic acid via copolymerization. And,next,we have prepared the aforementioned lead salt with C60-bis malonate maleic acid copolymer and lead nitrate. And now,it is necessary to identify and characterize the TNPEM and FTNPEM that we have prepared by using FT-IR,UV-Vis,1H NMR,13 C NMR,ESI-MS and the elementary analysis whereas the chemical structures of C60-bis（2,4,6-trinitrophenethyl） malonate maleic acid copolymer and the lead salt of C60-bis（2,4,6-trinitrophenethyl） malonate maleic acid copolymer can be analyzed and determinated by FT-IR,UV-Vis,GPC,AAS,XRD and XPS. And,afterwards,we have managed to test the thermal stability of the lead salt of C60-bis malonate maleic acid copolymer by using the DTA and TGA in the air. The DTA curve we have worked out indicates that the desired product should enjoy high thermal stability with its initial decomposition peak temperature being 239 ℃.At the same time,the DTA in the air can also determine the catalyst behavior of the lead salt of C60-bis malonate maleic acid copolymer.In addition,while the peak temperature of the thermal decomposition of RDX is falling by 6 ℃,it would be possible for the thermal decomposition reaction of RDX to be accelerated by the lead salt of C60-bis malonate maleic acid copolymer,because the lead salt of C60-bis malonate maleic acid copolymer contains lead and C60,which can help to catalyze the combustion of propellant and thus improve the dispersion of lead and carbon at the molecular level.