The invention relates to the technical field of energetic materials, and particularly discloses 3, 3 '-diamino-4, 4'-azofurazan and a preparation method thereof.The target object is synthesized through ionic electrocouple oxidation, the preparation method comprises the following steps that 1, an acid solution of 3, 4-diaminofurazan is prepared, the
molar concentration of 3, 4-diaminofurazan in the acid solution is 0.03-0.05 mol / L, and a first solution is obtained; 2, an acid solution of Ce < 4 + > is prepared, the
molar concentration of Ce < 4 + > in the acid solution is 0.09-0.25 mol / L, and a second solution is obtained; 3, the
reaction temperature is controlled to range from-5 DEG C to 25 DEG C, the first solution is added into the second solution, stirring, centrifuging, filtering, washing,
drying and
grinding are carried out, and a final sample 3, 3 '-diamino-4, 4'-azofurazan.The synthesis method is easy to operate, low in cost, easy in
raw material obtaining and easy to produce, conforms to the
green chemistry concept and has the high reaction yield and the high purity.