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930 邵艳丽,王乾,王鹏程,张晓鹏,姜振明,陆明
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Preparation Process and Mechanism of Cutting off the C─N Research of Sodium Pentazole Salt
SHAO Yan⁃li ,WANG Qian ,WANG Peng⁃cheng ,ZHANG Xiao⁃peng ,JIANG Zhen⁃ming ,LU Ming 1
2
1
1
2
1
(1. School of Chemical Engineering,Nanjing University of Science and Technology,Nanjing 210094,China;2. The Gansu Yinguang Chemical Industry Group
Co. LTD,Baiyin 730999,China)
Abstract:Sodium pentazole salt was prepared by treating 2,6⁃dimethyl⁃4⁃(2H⁃pentazol⁃2⁃yl)phenolate with m⁃chloroperbenzo⁃
ic acid (m⁃CPBA) and ferrous bisglycinate [Fe(Gly) 2 ] under low⁃temperature conditions,thereinto,m⁃CPBA and Fe(Gly) 2
were oxidizer and catalyst,respectively. The synthetic conditions were optimized,as following:the molar ratio between aryl⁃
pentazole,Fe(Gly) 2 and m⁃CPBA was 1∶3∶4.5,the reaction time was 24 h and the reaction temperature was -45 ℃(crude
yield of 28%). The effect of different oxidizing cleavage reagents on the yield of sodium pentazole salt was studied and the rea⁃
son for the low yield of sodium pentazole salt was analyzed. In addition,sodium pentazole salt and the reaction by⁃product
(2,6⁃dimethylcyclohexa⁃2,5⁃diene⁃1,4⁃dione)were characterized by X⁃ray single crystal diffractometer(XRD),NMR( NMR
15
1
and H NMR),FT⁃IR,mass spectrometry and elemental analysis. Based on these results,the mechanism of oxidizing cleavage
of the C─N bond in arylpentazole by m⁃CPBA and Fe(Gly) 2 was speculated.
Key words:ionic total nitrogen energetic materials;sodium pentazole salt;preparation process;cutting off the C─N bond mechanism
CLC number:TJ55;O62 Document code:A DOI:10.11943/CJEM2018117
Chinese Journal of Energetic Materials,Vol.26, No.11, 2018(925-930) 含能材料 www.energetic-materials.org.cn