OPTIMIZATION OF THE PROCESS PARAMETERS FOR SYNTHESIS OF 3,6-BIS(1H-1,2,3,4-TETRAZOL-5-YLAMINO)-S-TETRAZINE

Abstract

3,6-bis(1H-1,2,3,4-tetrazol-5-ylamino)-1,2,4,5-tetrazine (BTATz) is a high-nitrogen energetic material with attractive properties including low sensitivity, excellent gas-generating capacity, and environmentally friendly decomposition. In this work, the synthesis of BTATz from 3,6-bis(3,5-dimethylpyrazol-1-yl)-1,2,4,5-tetrazine (BDT) and 5-aminotetrazole (5-AT) in sulfolane was optimized using the Taguchi method with an L9(3³) orthogonal array, considering three factors: BDT/5-AT molar ratio, reaction temperature, and reaction time. Statistical analysis revealed that the molar ratio of BDT/5-AT was the most influential factor on yield, while reaction time exhibited the least effect. The optimal conditions (BDT/5-AT = 2.8, temperature = 135°C, time = 20 h) afforded a maximum experimental yield of 88.3%, which agreed well with the predicted value of 86.4%. The ignition temperature of ~274°C remained unchanged across all conditions, confirming the consistent quality of the synthesized product. Structural characterization by FT-IR and NMR supported the successful preparation of BTATz. Sensitivity tests indicated relatively low impact and friction sensitivity, highlighting BTATz as a promising candidate for advanced energetic formulations.