化工进展2015，Vol.34Issue(12)：4338-4342,5.DOI:10.16085/j.issn.1000-6613.2015.12.034
3,5-二硝基-1-氧杂-3,5-二氮杂环己烷的分离、热分解及硝解机理分析
Separation and thermal decomposition of 3,5-dinitro-1-oxa-3,5-diazacyclohexane and the nitrolysis mechanism
摘要
Abstract
In order to understand the nitrolysis mechanism of hexamethylenetetramine,we studied the waste water from the preparation of hexogeon(RDX) by nitric acid nitration . The byproducts were enriched by extraction with ethyl acetate,washed with water to neutral,and concentrated. Then they were analyzed by thin layer chromatography(TLC) with the developing solvent of acetone/dichloromethane/glacial acetic acid with a (volume) ratio of 1/6/0.1. Finally silica gel column chromatography was applied to separate the stable byproducts,which was then eluted by mixtures of acetone and dichloromethane with different composition. RDX was confirmed as one of the products by melting point,IR and NMR analysis. The other one product obtained was characterized through IR, NMR,MS,elemental analysis and single crystal diffraction,and then identified as 3,5-dinitro- 1-oxa-3,5-diazacyclohexane. The DSC-TG technique was used to investigate the thermal behavior of 3,5-dinitro-1-oxa-3,5-diazacyclohexane,which showed a pair of sharp peaks at 375.85K (melting) and 519.05K (decomposition),indicating that it is a low melting point compound with good stability. The separation and structure identification of main byproducts provided some reliable proofs for the mechanism of RDX obtained by direct nitration.关键词
3,5-二硝基-1-氧杂-3,5-二氮杂环己烷/分离/色谱/热解/硝解机理/黑索今(RDX)Key words
3/5-dinitro-1-oxa-3/5-diazacyclohexane/separation/chromatography/pyrolysis/nitrolysis mechanism/hexogeon (RDX)分类
军事科技引用本文复制引用
李静,陈丽珍,王建龙,高宇鹏,陈芳..3,5-二硝基-1-氧杂-3,5-二氮杂环己烷的分离、热分解及硝解机理分析[J].化工进展,2015,34(12):4338-4342,5.基金项目
国家自然科学基金(11447219)及国防产品创新项目. （11447219）
