Journal
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
Volume 639, Issue 5, Pages 681-688Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/zaac.201300010
Keywords
Tetrazoles; Tetrazines; High energy density materials; Nitrogen-rich compounds; Energetic materials
Categories
Funding
- Ludwig-Maximilian University of Munich (LMU)
- U.S. Army Research Laboratory (ARL)
- RDECOM Ordnance Environmental Program (OEP)
- Strategic Environmental Research and Development Program (SERDP)
- Office of Naval Research (ONR Global) [W911NF-09-2-0018, W911NF-09-1-0120, W011NF-09-1-0056, W911NF-12-1-0467, 10 WPSEED01-002 / WP-1765]
- Navy ManTech program
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Sodium 5-nitrotetrazolate dihydrate (NaNT) is a useful precursor compound for the synthesis of lead-free primary explosives; however, currently employed syntheses for the compound are tedious, dangerous, and plagued by impurities. Through comprehensive analysis, we elucidate the identity of the most detrimental impurities and further report an improved procedure for preparation of NaNT, which greatly improves the purity, while avoiding the handling of acid copper(II) nitrotetrazolate, a highly sensitive explosive intermediate. In the new procedure, 5-aminotetrazole is diazotized with sodium nitrite, cupric sulfate, and nitric acid. Copper is precipitated as its oxide and the aqueous solution evaporated. After soxhlet extraction with acetone, large crystals of NaNT are obtained. The prepared material is suitable for preparation of lead azide replacement DBX-1 [copper(I) 5-nitrotetrazolate] as evidenced by successful use in M55 stab detonators.
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