UHPLC-QTOF-MS高效检测CL-20合成过程的杂质  

UHPLC⁃QTOF⁃MS High Efficiency Eetectionof Impurities in a Typical CL⁃20Synthesis Process

作　　者：苏鹏飞 鄂秀天凤[1] 马婷婷 胡银 王民昌 张皋[2] 孟子晖 SU Peng-fei;E Xiu-tian-feng;Ma Ting-ting;HU Yin;WANG Min-chang;ZHANG Gao;MENG Zi-hui(College of Chemistry and Chemical Engineering,Beijing Institute of Technology,Beijing 100081,China;Xi'an Modern Chemistry Research Institute,Xi'an 710065,China;Yangtze Delta Region Academy of Beijing Institute of Technology,Jiaxing 314003,China)

机构地区：[1]北京理工大学化学与化工学院,北京100081 [2]西安近代化学研究所,西安710065 [3]北京理工大学长三角研究院,嘉兴314003

出　　处：《含能材料》2023年第7期688-698,共11页Chinese Journal of Energetic Materials

基　　金：国家自然科学基金资助(22105024)。

摘　　要：为了快速准确检测和分析六硝基六氮杂异伍兹烷(CL-20)合成过程中产生的中间体和杂质,控制CL-20纯度或品质,保证其感度及爆轰性能,采用核磁共振(NMR)和超高高效液相色谱-四极杆飞行时间质谱(UHPLC-QTOF-MS)技术快速、高效分析检测了CL-20典型合成工艺过程中组分及杂质。结果表明,六苄基六氮杂异伍兹烷(HBIW)中的杂质为1,3-二苄基咪唑,四乙酰基二苄基六氮杂异伍兹烷(TADB)中的杂质为低酰基化的三乙酰基三苄基六氮杂异伍兹烷(TATB),四乙酰基六氮杂异伍兹烷(TAIW)中的杂质为未完全反应的TADB,CL-20中的杂质为未完全硝化的一乙酰基五硝基六氮杂异伍兹烷(MPIW)和二乙酰基四硝基六氮杂异伍兹烷(DATN)。Quickly and accurately detect and analyze the intermediates and impurities produced in the synthesis of Hexanitro-hexaazaisowurtzitane(CL-20),is important for controlling the purity or quality of CL-20,and ensuring its sensitivity and detona-tion performance.In this study,nuclear magnetic resonance(NMR)and ultra-high performance liquid chromatography-Quadrupole time-of-flight mass spectrometry(UHPLC-QTOF-MS)were used to rapidly and efficiently analyze the impurities in the typical synthesis process of CL-20.The results showed that the impurity in HBIW was 1,3-dibenzyl imidaz-ole,the impurity in tetraacetyl dibenzyl hexazepane(TADB)was low acylated triacetyl tribenzyl hexazepane(TATB),and the impurity in tetraacetyl hexazepane(TAIW)was incomplete TADB.The impurities in CL-20 were not fully nitrated monoacetyl pentanitrohexazazine(MPIW)and diacetyl tetranitrohexazazine(DATN).

关 键 词：CL-20 中间体 杂质 UHPLC-QTOF-MS NMR 

分 类 号：TJ55[兵器科学与技术—军事化学与烟火技术] O65[理学—分析化学]