CHINESE JOURNAL OF ENERGETIC MATERIALS
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千克级LLM-105合成和三氟乙酸回收技术
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(西安近代化学研究所, 陕西 西安 710065)

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王友兵(1976-),男,副研究员,主要从事含能材料合成及工艺研究。e-mail: wangyoubing_wang@163.com

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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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    摘要:

    研究了氧化2, 6-二氨基-3, 5-二硝基吡嗪(ANPZ)合成2, 6-二氨基-3, 5-二硝基吡嗪-1-氧化物(LLM-105)的千克级工艺。LLM-105收率为98.3%, 纯度96.4%。降低了三氟乙酸(TFA)用量。采用红外、元素、核磁、质谱表征了LLM-105的结构。采用中和、酸化、蒸馏的方法, 研究了TFA母液回收的千克级工艺, 回收率为85.4%, 纯度99.7%。回收TFA用于ANPZ氧化反应, LLM-105收率为97.8%。探讨了影响氧化反应的因素。最佳工艺参数为: m(ANPZ):V(H2O2)=1:1.8, m(ANPZ):V(TFA) =1:5, 反应温度25~30 ℃, 反应时间14 h; 回收TFA的最佳工艺参数为,质量比m(TFA):V(H2SO4)=1:1.0。

    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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引用本文

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. DOI:10.11943/j. issn.1006-9941.2015.01.006.
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. DOI:10.11943/j. issn.1006-9941.2015.01.006.

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历史
  • 收稿日期: 2013-10-21
  • 最后修改日期: 2014-02-09
  • 录用日期: 2014-03-11
  • 在线发布日期: 2015-01-20
  • 出版日期: 2015-01-20