CHINESE JOURNAL OF ENERGETIC MATERIALS
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Optimization on Synthesis Process and Characterization of 1-Methyl-3,4-dinitropyrazoles
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(1. College of Chemical Engineering & Environment, North University of China, Taiyuan 030051, China; 2. State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China)

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    Abstract:

    1-Methyl-3, 4-dinitropyrazole(MDNP) was synthesized using 3-nitropyrazole as starting material via nitration and methylation, and its structrue was characterized by infrared spectrum(IR), proton nuclear magnetic resonance(1H NMR) and differential scanning calorimetry(DSC).The methylation reaction conditions were optimized.Results show that its thermal decomposition temperature is 298 ℃, and melting point is 20 ℃, having good thermal stability.The optimum conditions of methylation reaction is as follows:the reaction temperature 90 ℃, the reaction time 6.5 h, the molar ratio of 3, 4-dinitropyrazoles, DMC(dimethyl carbonate) to anhydrous potassium carbonate 1:10.5:1.5, and the yield of target product is 55.6%.

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张巧玲,李雅津,焦清介,等.1-甲基-3,4-二硝基吡唑合成与表征[J].含能材料,2015,23(3):222-225.
ZHANG Qiao-ling, LI Ya-jin, JIAO Qing-jie, et al. Optimization on Synthesis Process and Characterization of 1-Methyl-3,4-dinitropyrazoles[J]. Chinese Journal of Energetic Materials,2015,23(3):222-225.

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History
  • Received:January 25,2014
  • Revised:April 29,2014
  • Adopted:May 06,2014
  • Online: March 09,2015
  • Published: March 10,2015