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  

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

作　　者：靳雅蕙[1] 于雁武[1] 刘玉存[1] 魏华男 高喆[1] 罗进[1] 

机构地区：[1]中北大学化工与环境学院,太原030051

出　　处：《科学技术与工程》2016年第32期224-228,共5页Science Technology and Engineering

基　　金：国家自然联合基金(U1330135)资助

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,Na NO3用量为31.2 g,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。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 5 g and Na NO3 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）.

关 键 词：DCONAB 耐热炸药 制备方法 含能中间体 工艺改进 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术]