Studies On The Hundred Grams-scale Preparation And Technology Of High-purity DAOAF

Furazan derivative 3,3?-diamino-4,4?-azoxyfurazan?DAOAF?is a kind of insensitive high explosive with excellent performance.With its excellent detonation performance and low sensitivity,DAOAF is expected to be used as an initial explosive for the fourth generation of impactor detonators,which will greatly enhance the performance of new generation of impactor detonators.Although there are many methods for synthesizing DAOAF,most of them are not suitable for process amplification and cannot guarantee the quality of DAOAF synthesized.In order to meet the high purity requirement of the explosive detonators for explosives,in this paper,a synthetic process of 100-gram high-purity DAOAF was designed starting from glyoxal.The main research contents are as follows:?1?The key intermediate 3,4-diaminofurazan?DAF?was synthesized by one-step synthesis from glyoxal and hydroxylamine hydrochloride under atmospheric pressure and the reaction was scaled up.Using DAF as substrate,3,3'-diamino-4,4'-azoxyfurazan?DAOAF?was successfully synthesized from the reaction of potassium persulfate?KHSO₅·0.5KHSO₄·0.5K₂SO₄?as oxidant in the sodium bicarbonate solution,and the synthesis process was scaled up to100-grams.The effects of reactant ratio,reaction time and reaction temperature on the yield of DAF and DAOAF were investigated respectively,and the reaction mechanism was discussed.The optimal synthesis conditions were selected and crude DAOAF with high quality was obtained.The structure of the compound s were confirmed by IR,¹H NMR,¹³C NMR,MS spectra and other analytical tests.?2?3-Amino-4-nitrofurazan?ANF?and 3,3'-diamino-4,4'-azofurazan?DAAF?were synthesized in the laboratory as the control of impuritises.The purity of them can reached 99.5%after purification.Reliable liquid chromatographic analysis conditions were used to determine the purity of the compound by area normalization method,and to determine the qualitative and quantitative analysis of the impurities in the crude DAOAF.?3?Based on the difference of the solubility of DAOAF and impurities,recrystallization was used to remove the impurities in crude DAOAF.The effects of different solvents on the recrystallization effect were investigated.Finally,N,N-dimethylformamide?DMF?was selected as the recrystallization solvent,and the preparation of high-purity DAOAF?purity>99.5%?was achieved.