Studies On Synthesis Of New High-nitrogen Energetic Materials Derived From Tetrazole

Tetrazole energetic compounds have high nitrogen content,positive enthalpy of formation,detonation velocity,detonation pressure and good thermal stability, which show great prospect in application of the field of energetic materials. The organic combination of tetrazole-ring with multi-nitrobenzene such as 2,4,6-trinitrochlorobenzene can not only increase the enthalpies of formation, but can also enhance the stability of molecular because of the forming of the conjugate system of tetrazole-ring with benzene-ring, which provides possibilities of the synthesis of new energetic materials meeting requirements.Synthesis technology of raw materials 5-aminotetrazole by the method of diazotization and intramolecular cyclization was investigated, the best process condition was for diazo-reaction:pH=2-3,T=20-30℃,t=0.5h; for intramolecular cyclization:pH=8-9,T=85-90℃,t=3.5 h. The yield and purity of 5-aminotetrazole seperately were 77.2% and 99%. Rough materials 5-nitroiminotetrazole,2,4-dinitrochlorobenzene and 2,4,6-trinitrochlorobenzene (commonly knowned as picrylchloride) were synthesized and characterized. The yield and purity of them seperately were:77.2%,99%; 63%,99.4%; 89.9%,99.1%; 63%,99.5%。Reaction of 0.0025 mol 5-aminotetrazole and 0.001 mol picrylchloride in ethanol as solvent under the existence of K2CO3 was investigated, and 1-(2,4,6-trinitro-1-benzeneyl)-5-aminotetrazole (A) was received, the volume of production,yield and purity seperately of A were 0.84 g,28.6%,99.6%; reaction of 0.0025 mol 5-aminotetrazole and 0.001 mol 2,4-dinitrochlorobenzene in enthanol as solvent under the existence of K2CO3/NaF was studied, and 1-(2,4-dinitro-l-benzeneyl)-5-aminotetrazole (B') was produced, the volume of production,yield and purity of B'seperately were 0.62 g,24.8%, 99.2%; reaction of 0.001 mol 5-nitroiminotetrazole and 0.0025 mol picrylchloride in enthanol and DMSO as solvents with the volume ratio 10:1 under the existence of tricthylamine was researched, and 1-(2,4,6-trinitro-1-benzeneyl)-5-nitroaminotetrazole (C') was obtained, the volume of production,yield and purity of C' seperately were 0.85 g,25.0%,98.9%. Reaction temperature and time of the three reactions were respectively researched in different solvents, and possible side reactions,by-products and influence factors of reaction process were discussed. The new compounds were characterized by MS,IR,1H NMR and 13C NMR, and their explosion performances were predicted by theoretical calculation. The results indicated that the energy of A and B'were lower than that of 5-aminotetrazole, while the properties of C'were better than that of 5-nitroaminotetrazole.