Synthetic process optimization and thermal analysis of 1,1′-diamino-5,5′-azotetrazole

Abstract

1,1′-Diamino-5,5′-azotetrazole (DAZT) has been synthesized using acetic acid (HAc) and 1,1′-diisopropylideneamino-5,5′-azotetrozole (DPrZT) as the raw material. Three of the most important factors which affect the yield of DAZT are the reaction temperature, the reaction time, and n(DPrZT):n(HAc). Based on single-factor experiments, orthogonal experiments were carried out. The most optimal experimental conditions were determined to be: a reaction temperature of 70 °C, a reaction time of 20 min, and a reactant ratio n(DPrZT)–n(HAc) of 1:48. The maximum yield was 97.6 % under optimum reaction conditions. Elemental analysis, IR, and NMR confirmed the structure of DAZT. The morphology was analyzed by SEM. The thermal decomposition behavior of DAZT was investigated by TG-DSC and DTA techniques. The mode of thermal decomposition was analyzed. The kinetic parameters including activation energy and pre-exponential factor were calculated from the Kissinger equation. The mechanical sensitivity on this compound was evaluated. Results suggest that it might be useful as an energetic material.