Salts of 1H‐Tetrazole – Synthesis, Characterization and Properties
作者： Thomas M. Klapötke , Marco Stein , Jörg Stierstorfer
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摘要: The most facile route for the formation of 1H-Tetrazole (1, TZ) is reaction sodium azide with ammonium chloride and orthoethyl formate in glacial acetic acid. 1 was deprotonated using alkali hydroxides carbonates yielding corresponding metal salts LiTZ (4), NaTZ·H2O (5), KTZ (6), RbTZ (7) CsTZ (8). nitrogen rich NH4TZ·H2O (2) N2H5TZ (3) were synthesized by 1H-tetrazole aqueous NH3 N2H4 solutions, respectively. In addition, Sr(TZ)2·5H2O (9) obtained deprotonation Sr(OH)2·8H2O its use as possible energetic ingredient modern pyrotechnic compositions a red component investigated. All compounds characterized vibrational (IR Raman) spectroscopy, multinuclear (1H, 7Li, 13C, 14N, 15N) NMR spectroscopy elemental analysis. structures crystalline state 2, 3, 4, 5, 6, 7, 8 9 determined low temperature X-ray diffraction detailed description given this work. physico-chemical properties all investigated DSC (differential scanning calorimetry) heats calculated combustion bomb calorimetry. Since tetrazoles often are materials, sensitivities 1–9 tested BAM drophammer friction tester. Crystal Data: 2: monoclinic, P21/n, = 7.211(1), b 4.0108(8), c 17.991(4) A, β 91.97(3)°, V 520.0(2) A3, Z ρ 1.343 g cm−3; 3: orthorhombic, Ccca, 6.763(1), 17.7510(4), 16.3160(8) 1958.7(3) 16, 1.385 4: C2221, 13.499(2), 14.389(3), 14.125(3) 2743.6(9) 8, 1.472 5: Pmma, 6.400(2), 5.837(1), 5.608(2) 209.51(9) 1.745 6: hexagonal, , 14.0037(2), 10.7285(2) 1822.03(5) 1.774 7: P63/m, 8.260(2), 11.009(3) 650.5(3) 2.367 8: Pbca, 7.3406(8), 9.610(1), 12.199(1) 860.5(2) 3.118 9: Pnnm, 11.314(2), 13.876(3), 7.121(1) 1117.9(4) 1.877 cm−3.
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