TY - JOUR
T1 - Synthetic process optimization and thermal analysis of 1,1′-diamino-5,5′-azotetrazole
AU - Han, Zhiyue
AU - Yao, Qian
AU - Zhang, Yinghao
AU - Du, Zhiming
AU - Li, Fang
N1 - Publisher Copyright:
© 2015 Akadémiai Kiadó, Budapest, Hungary.
PY - 2015/8/22
Y1 - 2015/8/22
N2 - 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.
AB - 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.
KW - Differential scanning calorimetry (DSC)
KW - Differential thermal analysis (DTA)
KW - Nitrogen-rich compound
KW - Synthetic process optimization
UR - https://www.scopus.com/pages/publications/84937524235
U2 - 10.1007/s10973-015-4612-2
DO - 10.1007/s10973-015-4612-2
M3 - Article
AN - SCOPUS:84937524235
SN - 1388-6150
VL - 121
SP - 951
EP - 957
JO - Journal of Thermal Analysis and Calorimetry
JF - Journal of Thermal Analysis and Calorimetry
IS - 2
M1 - 4612
ER -