Synthesis Of1-AMTN And Investigation Of Industrial Amplification

1-amino-3-methyl-1,2,3-triazolium nitrate (1-AMTN) has physical and chemical properties and explosive performance that are higher than that of TNT, which can be used as a replacement for2,4,6-trinitrotoluene (TNT) for use in melt castable explosives.In this dissertation,1-AMTN was synthesized using hydrazine hydrate and glyoxal as starting materials in four steps including addition-elimination, cyclization, methylation and replacement reaction, the products were characterized by IR, NMR and MS.Technics conditions of addition-elimination, cyclization and methylation were optimized through single factor experiment and orthogonal experiment, so the ideal reaction conditions of glyoxal bishydrazone are the molar ratio3.00:1(hydrazine hydrate:glyoxal), the reaction temperature70℃,40mL of methanol (per mol hydrazine hydrate), the reaction time3h.The ideal reaction conditions of1-amino-1,2,3-triazole(ATZ)are the molar ratio4.00:1(manganese dioxide: glyoxal bishydrazone), the reaction temperature20℃, the reaction time9h.The ideal reaction conditions of1-amino-3-methyl-1,2,3-triazolium methylsulfate (1-AMTMS) are the molar ratio1:1.35(ATZ:Me2SO4), the reaction temperature80℃, the reaction time6h. The overall yield of1-AMTN is62.0%.The seale-up of the synthesis of1-AMTN was studied, and it was performed at the1OOg scale totally, the overall yield was improved to72.1%. Actived manganese oxide and solvent were recycled.The physical and chemical properties and explosive performance of1-AMTN were measured,and the experimental results were compared with the properties of TNT, the results indicated that1-AMTN could be used as high-energy liquid carrier in melt castable explosives.