新型耐热含能中间体—4,4′-二氯-2,2′,3,3′,5,5′,6,6′-八硝基偶氮苯(DCONAB)合成工艺改进
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中北大学化工与环境学院,中北大学化工与环境学院,中北大学化工与环境学院,中北大学化工与环境学院,中北大学化工与环境学院,中北大学化工与环境学院

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TJ55

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The Improvement of a New-type Heat-resistant Energetic Intermediate—4,4′-dichloro-2,2′,3,3′,5,5′,6,6′-octanitroazo-benzene(DCONAB)Synthesis Process
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College of Chemical Engineering and Environment,North University of China,Taiyuan,030051,College of Chemical Engineering and Environment,North University of China,Taiyuan,030051,College of Chemical Engineering and Environment,North University of China,Taiyuan,030051,College of Chemical Engineering and Environment,North University of China,Taiyuan,030051

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    摘要:

    介绍了以4-氯苯甲酸为原料经三步合成4,4′-二氯-2,2′,3,3′,5,5′,6,6′-八硝基偶氮苯(DCONAB)的新方法。用浓硫酸和硝酸钠硝化体系代替了原工艺发烟硝酸硝化体系,提升了合成过程的安全性,降低了产物的后处理难度。采用了单因素和正交实验设计方法优化了实验,并确定了最佳工艺条件,,即4-氯-3,5-二硝基苯胺定量5 g,NaNO3用量为31.2g,反应温度95℃,反应时间3.5 h,将收率从53%提高到了78%,纯度≥95.8%(HPLC)。采用红外光谱(FTIR)、元素分析(EA)和高效液相色谱(HPLC)等方法对合成产物4-氯-3,5-二硝基苯甲酸、4-氯-3,5-二硝基苯胺及DCONAB进行了结构表征。

    Abstract:

    A new method in preparation of 4,4′-dichloro-2,2′,3,3′, 5,5′,6,6′- octanitroazo-benzene(DCONAB) by the three step based on 4-chlorobenzoic acid was introduced.The original process of fuming nitric acid nitration system was replaced with concentrated sulfuric acid and sodium nitrate nitration system,improved the synthetic process of security and reduced the difficulty in the product post-processing.The optimum technological conditions were determined with the the method of single factor and orthogonal experiment.The optimum conditions contain 4-Chloro-3,5-dinitroaniline in the quality of 5g and NaNO3 is 31.2 g,raised the yield from 53% to 78% and ensured the purity of DCONAB is 95.8% at least.Besides,the 4-Chloro-3,5- dinitrobenzoic acid,4-Chloro-3,5- dinitroaniline and DCONAB were characterized in the aspect of structure with fourier transform infrared spectrometer(FTIR),elemental analysis(EA) and high performance liquid chromatography(HPLC).

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靳雅蕙,于雁武,刘玉存,等. 新型耐热含能中间体—4,4′-二氯-2,2′,3,3′,5,5′,6,6′-八硝基偶氮苯(DCONAB)合成工艺改进[J]. 科学技术与工程, 2016, 16(32): .
JIN Ya-hui,,LIU Yu-cun, et al. The Improvement of a New-type Heat-resistant Energetic Intermediate—4,4′-dichloro-2,2′,3,3′,5,5′,6,6′-octanitroazo-benzene(DCONAB)Synthesis Process[J]. Science Technology and Engineering,2016,16(32).

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历史
  • 收稿日期:2016-05-23
  • 最后修改日期:2016-07-04
  • 录用日期:2016-07-22
  • 在线发布日期: 2016-11-22
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