Synthesis, Characterization And Thermal Performance Study Of Fullerene-amine Nitrate/dinitramide Salts

To explore new energetic burning rate catalyst, two types of five kinds of unreported energetic fullerene derivative were synthesized, and their thermal performance were probed preliminary.By controlling the reaction conditions, C60, ICl and Br2 were used as raw materials to synthesize C60Cl6 and three kinds of bromofullerenes: C60Br8, C60Br14 and C60Br24, which then reacted with 4-amino-1, 2, 4-triazole to obtain four kinds of fullerene-amine: C60(NH2)6, C60(NH2)8, C60(NH2)14 and C60(NH2)24. Then four kinds of energetic fullerene derivatives(C60(NH2)6·m HNO3, C60(NH2)8·m HNO3, C60(NH2)14·m HNO3 and C60(NH2)24·m HNO3) were obtained by corresponding fullerene-amine and dilute nitric acid.Both of four kinds of fullerene-amine derivatives and its nitrate were characterized by fourier transform infrared(FT-IR) spectroscopy, ultravioletvisible absorption spectroscopy(UV-Vis), X-ray photoelectron spectroscopy(XPS) and other analytical tools, the results were consistent with the expected structure. At the same time, thermal stability of these four kinds of fullerene-amine nitrate were studied by means of thermal analysis tools DTA, DSC and TG, and thermal decomposition kinetics parameters of these fullerene derivatives were obtained by calculation. Thermal decomposition of four kinds of fullerene-amine nitrate(C60(NH2)6·m HNO3, C60(NH2)8·m HNO3, C60(NH2)14·m HNO3 and C60(NH2) 24·m HNO3) had two distinct stages under air atmosphere respectively, which were almost completely. And their thermal decomposition peak temperature of the first stage of the were 167 ℃, 156 ℃, 155 ℃ and 151 ℃ respectively. Under a nitrogen atmosphere, thermal decomposition of four kinds of amino nitrate fullerene had only a distinct stage respectively, which were incompletely. And under a nitrogen atmosphere, thermal decomposition activation energy four kinds of energetic fullerene amino nitrate fullerene amino nitrate were 151.48 k J ·mol-1、151.07 k J·mol-1、157.55 k J·mol-1 and 153.06 k J·mol-1 respectively. These results showed that four kinds fullerene-amine nitrate had good thermal stability.HSO3NH2 and KOH were used as raw materials to synthesize potassium sulphamate(KSO3NH2), then potassium dinitramide(KDN) was synthesized from KSO3NH2 in HNO3-H2SO4 mixture solution, which continued react with Ag NO 3 to obtain Ag N(NO2)2. C60(NH2)24·m HCl was prepared from C60(NH2)24 and dilute hydrochloric acid(HCl). Afterwards, we obtained fullerene-amine dinitramide salt(C60(NH2)24·m HN(NO2)2) through precipitation reaction by C60(NH2)24·m HCl and Ag N(NO2)2. And then C60(NH2)24·m HN(NO2)2 was characterized by fourier transform infrared(FT-IR) spectroscopy, ultraviolet-visible absorption spectroscopy(UV-Vis), X-ray photoelectron spectroscopy(XPS) and other analytical tools. At the same time, thermal stability of C 60(NH2)24·m HN(NO2)2 was studied by means of thermal analysis tools DTA, DSC and TG. The experimental results indicated that C60(NH2)24·m HN(NO2)2 had a certain thermal stability.Not only can energetic fullerene derivatives provide a carbon propellant component, but also provide some extra energy, it may be a better regulation of the combustion performance of solid propellant. This study belongs to the new energetic combustion catalyst and basic research in solid rocket propellant, which has certain scientific application value.