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Synthesis of LLM-105 and Recycling Technology of TFA on Kilogram Scale
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(Xi′an Modern Chemistry Research Institute, Xi′an 710065, China)

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    Abstract:

    The technology for synthesizing 2, 6-diamino-3, 5-dinitropyrazine-l-oxide (LLM-105) was studied by oxidation of 2, 6-diamino-3, 5-dinitropyrazine(ANPZ) on kilogram scale. The yield of LLM-105 is 98.3% and its purity 96.4%. The dosage of trifluoroacetic acid (TFA) is reduced. The structure of LLM-105 was characterized by IR, elemental analysis, 1H NMR and MS. The recovery technology of TFA mother solution was studied by neutralization, acidification and distillation on kilogram scale. The recovery of TFA is 85.1% and its purity 99.8%. Using the recovery TFA for the oxidation reaction of ANPZ, the yield of LLM-105 can be 97.8%. The factors affecting the oxidation reaction were discussed. The optimum technology parameters of the oxidation reaction are: m(ANPZ):V(H2O2)=1:1.8, m(ANPZ): V (TFA) =1:5, reaction temperature 25~30 ℃, reaction time 14 h.The optimum technology parameter of recycling of TFA is m(TFA):V(H2SO4)=1:1.0.

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王友兵,黄凤臣,张蒙蒙,等.千克级LLM-105合成和三氟乙酸回收技术[J].含能材料,2015,23(1):29-32.
WANG You-bing, HUANG Feng-cheng, ZHANG Meng-meng, et al. Synthesis of LLM-105 and Recycling Technology of TFA on Kilogram Scale[J]. Chinese Journal of Energetic Materials,2015,23(1):29-32.

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History
  • Received:October 21,2013
  • Revised:February 09,2014
  • Adopted:March 11,2014
  • Online: January 20,2015
  • Published: January 20,2015