Optimization and Thermal Risk Analysis of 3,4-bis(4-Aminofurazano-3-yl) Furoxan Synthesis Process Based on Reaction Mechanism

3,4-bis(4-Aminofurazano-3-yl) furoxan (DATF) is a key precursor for the high-energy explosive 3,4-bis(4-nitrofurazano-3-yl) furoxan (DNTF), and it is also a high-nitrogen content energetic material. In this paper, the synthesis process of DATF was characterized using the HPLC technique, and the effects of four reaction parameters have been thoroughly studied. The thermal risk analysis for DATF synthesis was conducted with a reaction calorimeter (RC1) and an accelerating rate calorimeter. It was found that extracting the intermediate 3-amino-4-oxycyanofurazan from the aqueous to organic phases was an important way to improve the yield of DATF. Therefore, hydrophobic ethyl acetate was selected as one reaction solvent. The higher yield of DTAF obtained was about 60%. In addition, HPLC monitoring and reaction calorimetry results indicated that the rate of diazotization and decomposition of diazonium salt was feeding-controlled, and the cycloaddition reaction was a slow process. Most of the reaction heat has been released by the diazotization and decomposition of diazonium salt, while the heat effect of cycloaddition was not significant. Thermal stability analysis supported the conclusion that the decomposition of the reaction mixture was hardly possible to be triggered by the reaction heat. The thermal risk of DATF synthesis was low.