Patent ID: 8350050

Claim:
A method for producing bis-(1(2)H-tetrazol-5-yl)amine ammonium salt comprising the steps of: heating to 50 to 120° C. a solution mixture in which an azide salt in a necessary amount and a dicyanamide salt in an amount corresponding to 1 to 80 wt% of a necessary amount are added to a solvent, adding an acid in an amount of 1.54 to 2.22 chemical equivalents of the dicyanamide salt in the solution mixture to carry out a reaction at 50 to 120° C, adding an acid and a dicyanamide salt solution in which remaining dicyanamide salt is dissolved in a solvent to promote the reaction, heat-treating at 75° C. or greater the obtained metal salt compound, adding a solution of a second acid to form at least one of bis-(1(2)H-tetrazol-5-yl)amine anhydrate and monohydrate, and adding an amine to the obtained at least one of bis-(1(2)H-tetrazol-5-yl)amine anhydrate and monohydrate to convert the at least one of bis-(1(2)H-tetrazol-5-yl)amine anhydrate and monohydrate into bis-(1(2)H-tetrazol- 5 -yl)amine ammonium salt, wherein the bis-(1(2)H-tetrazol-5-yl)amine ammonium salt has a purity of 99.0 wt% or greater on a weight basis and not showing a peak accounting for 0.1 wt% or greater on a weight basis within a relative retention time starting at 2.17 and ending at 2.24 assuming that a retention time to a main peak is 1 as determined according to an area percentage obtained by HPLC analysis, provided that HPLC analysis conditions include: detection with UV220 nm, a column of Inertsil ODS-3 having 4.6 mm ID×250 mm, a column bath temperature of 30° C., a mobile phase of: solution A: 0.1% phosphoric acid solution/acetonitrile/methanol in a ratio of 950/25/25, and solution B: 0.1% phosphoric acid solution/acetonitrile in a ratio of 400/600, a gradient program of: 0-30 minutes: 100-50% solution A, 0-50% solution B, 30-60 minutes: 50% solution A, 50% solution B; a mobile phase flow rate of 1.0 mL/min, and an amount of a sample injected of 20 μL (loop).