The dynamic laser method was adopted to measure the solubility and supersolubility of 3, 4-bis(3-nitrofurazan-4-yl)furoxan(DNTF) in V(acetic acid):V(water)=7:3 mixed solvent. The Apelblat equation was used to fit the experimental solubility data. The influence of four main crystallization process factors of initial temperature, stirring speed, cooling rate and the mass of seed crystal were investigated by orthogonal experiments. Results show that the best product was obtained under initial temperature of 85 ℃, stirring speed of 400 r·min^-1, cooling rate of 0.25 ℃·min^-1 and seed crystal mass: solid mass of DNTF=5:95. The yield, purity, crystal density, characteristic height H₅₀ (2 kg drop hammer)of the best product are 91.7%, 99.72%, 1.876 g·cm^-3, 36.38 cm, respectively. The morphology of the product is regular, and the crystal size distribution of the product is narrow. Besides, the result of X-Ray powder diffraction demonstrates that the crystal structure does not change during the crystallization process.