含能材料2025,Vol.33Issue(5):485-496,12.DOI:10.11943/CJEM2025018
DNTF的合成新工艺
New Synthesis Process of DNTF
摘要
Abstract
To improve the safety and reduce the toxicity of the synthesis process for 3,4-bis(4-nitro-1,2,5-oxadiazol-3-yl)-1,2,5-oxadiazole-2-oxide(DNTF),a four-step route was developed starting from 1,3-acetonedicarboxylic acid,involving oxima-tion,cyclization,oxidation,and nitration.The synthesis employed two critical intermediates:3-amino-4-(carboxymethyl)fura-zan(formed after cyclization)and 3-nitro-4-(carboxymethyl)furazan(generated during nitration).The process achieved an overall yield of 22%with the final product purity exceeding 98%.The structures of key intermediates and products were charac-terized by single-crystal X-ray diffraction,nuclear magnetic resonance,and infrared spectroscopy.The optimal synthesis process was determined through single-factor experiments,with an oxidation reaction yield of 97%and a nitration reaction yield of 56.5%.The process safety risks of oxidation and nitration reactions were studied by DSC,ARC,and RC1.The results showed that the oxidation reaction process had a high hazard level,while the nitration reaction process was classified as level 2.This synthesis route has promising potential for industrial-scale application.关键词
含能材料/DNTF/合成/工艺优化/安全风险评估Key words
energetic materials/DNTF/synthesis/process optimization/safety risk assessment分类
武器工业引用本文复制引用
桑梁,叶子鸿,陆明,许元刚..DNTF的合成新工艺[J].含能材料,2025,33(5):485-496,12.基金项目
国家自然科学基金(22475102,22105102,22135003) National Natural Science Foundation of China(Nos:22475102,22105102,22135003) (22475102,22105102,22135003)