摘要
含能化合物的能量和安全存在本质矛盾,设计和合成具有高密度、高能量、良好热稳定性和钝感等综合性能优异的新型含能化合物是最具挑战性的工作之一.本课题组近期报道了一种新型化合物4-氨基-7,8-二硝基吡唑-[5,1-d][1,2,3,5]-四嗪-2-氧化物(BITE-101)的合成,其密度、分解温度、爆轰性能和安全性等综合性能均优于传统单质炸药HMX,具有良好的应用潜力.为了进一步推动其应用研究,本研究对其制备放大的工艺进行了优化,着重研究了氧化反应中酸的种类、与双氧水的配比以及反应温度对产率的影响,经改进和放大工艺优化后得到了最优的氧化工艺条件:投料中间体1(60 g,0.26 mol),浓硫酸(120 mL)与H_(2)O_(2)(360 mL),反应温度为50℃时,氧化反应产率可达28.9%,最终实现了BITE-101的15 g量级的放大工艺,为其进一步应用研究提供了一定的参考.
The inherent contradiction between the energy and safety of energetic compounds makes the design and synthesis of novel energetic compounds with high density,high energy,strong thermal stability,and high sensitivity characteristics a significant and big challenge.Recently,4-amino-7,8-dinitropyrazole-[5,1-d][1,2,3,5]-tetrazine-2-oxide(BITE-101),which was characterized to possess superior integrated properties over traditional explosive HMX,was reported by our group.To promote its further applications,the optimized and scale-up preparation of BITE-101 was accomplished in this study,and the effects of acids,the ratio of hydrogen peroxide to acids,and reaction temperature in the oxidation reaction were studied and discussed.The following oxidation conditions were found to be optimal,as follows:compound 1(60 g,0.26 mol),concentrated sulfuric acid(120 m L)and H_(2)O_(2)(360 mL).The reaction temperature was 50°C,and a yield of 28.9%was obtained.The BITE-101 preparation procedure was scaled up to 15 g.This study serves as a reference for further research on the application of BITE-101.
作者
李杰
何春林
庞思平
LI Jie;HE ChunLin;PANG SiPing(School of Materials Science&Engineering,Beijing Institute of Technology,Beijing 100081,China;State Key Laboratory of Explosion Science and Technology,Beijing Institute of Technology,Beijing 100081,China)
出处
《中国科学：技术科学》
EI
CSCD
北大核心
2023年第9期1567-1573,共7页
Scientia Sinica(Technologica)
基金
国家自然科学基金重点项目(批准号:22235003)
国家自然科学基金面上项目(批准号:21875020)资助。
关键词
含能材料
热稳定性
共轭稠环
工艺优化
energetic materials
thermal stability
conjugated fused ring
synthesis optimization
作者简介
何春林,E-mail:chunlinhe@bit.edu.cn;庞思平,E-mail:pangsp@bit.edu.cn。
