CHINESE JOURNAL OF ENERGETIC MATERIALS
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微流控技术合成DAAF的工艺研究及性能表征
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1.中北大学环境与安全工程学院, 山西 太原 030051;2.陆军步兵学院石家庄校区, 河北 石家庄 050000

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国家自然科学基金资助(22005275)


Synthesis and Characterization of DAAF by Microfluidic Technology
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1.School of Environmental and Safety Engineering,North University of China,Taiyuan 030051, China;2.Shijiazhuang Campus of Army Infantry Academy, Shijiazhuang 050000, China

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    摘要:

    为了改善常规方法合成3,3′-二氨基-4,4′-氧化偶氮呋咱(DAAF)性能上存在的不足,拓宽DAAF的合成途径,设计了微流控反应系统,以3,4-二氨基呋咱(DAF)为主要原料,利用微流控技术合成了DAAF,并设计正交实验优化了合成工艺条件。在温度25 ℃,流速4 mL·min-1,出口结晶管长度5 m下合成了纯度为99.33%,收率为89.96%的DAAF。利用红外、核磁和元素分析表征了合成产物的结构,采用扫描电镜(SEM)、X射线衍射(XRD)、热分析仪(DSC/TG)以及机械感度进行表征。结果表明:DAAF呈团簇花球状,平均粒径为5.36 µm;微流控技术合成对DAAF晶体结构无影响;在10 ℃·min-1的升温速率下,其热分解峰温为262.36 ℃,热分解过程质量损失为82.79%;机械感度测试结果表明,其撞击感度为90 J,摩擦感度为0%。与常规方法合成的DAAF相比,其平均粒径减小7.36 µm,粒度分布均匀且粒径分布范围变窄,晶体结构未变化,热分解峰温提前9.57 ℃,热分解过程质量损失降低6.99%,撞击感度提高5 J,安全性能有所提高。

    Abstract:

    In order to improve the synthesis performance of 3,3′-diamino-4,4′-azoxyfurazan (DAAF) by conventional methods, broaden the synthetic pathway of DAAF. A microfluidic reaction system was designed to synthesize DAAF using 3,4-diaminofurazan (DAF) as the main raw material by microfluidic technology. Orthogonal experiment was designed to optimize the synthesis conditions. DAAF with a purity of 99.33% and a yield of 89.96% was synthesized at 25 ℃, a flow rate of 4 mL·min-1 and a length of 5 m in the outlet crystallizer. The structure of the synthesized product was characterized by infrared, nuclear magnetic and elemental analysis, and was characterized by scanning electron microscope (SEM), X-ray diffraction (XRD), thermal analyzer (DSC/TG) and mechanical sensitivity. The results show that DAAF was clustered flower ball with an average particle size of 5.36 µm; Microfluidic synthesis has no effect on the crystal structure of DAAF. At the heating rate of 10 ℃·min-1, the thermal decomposition peak temperature is 262.36 ℃, and the mass loss rate during thermal decomposition is 82.79%. The mechanical sensitivity test shows that the impact sensitivity is 90 J, and the friction sensitivity is 0%. Compared with the DAAF synthesized by the conventional method, the average particle size decreased by 7.36 µm, the particle size distribution is uniform and the particle size distribution range is narrowed, the crystal structure does not change, the thermal decomposition peak temperature was advanced by 9.57 ℃, the mass loss rate was reduced by 6.99%, the impact sensitivity is increased by 5 J, and the safety performance is improved.

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引用本文

时嘉辉,罗凯,刘淑杰,等.微流控技术合成DAAF的工艺研究及性能表征[J].含能材料, 2022, 30(4):349-355. DOI:10.11943/CJEM2021295.
SHI Jia-hui, LUO Kai, LIU Shu-jie, et al. Synthesis and Characterization of DAAF by Microfluidic Technology[J]. Chinese Journal of Energetic Materials, 2022, 30(4):349-355. DOI:10.11943/CJEM2021295.

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历史
  • 收稿日期: 2021-11-10
  • 最后修改日期: 2022-02-22
  • 录用日期: 2022-01-24
  • 在线发布日期: 2022-02-21
  • 出版日期: 2022-04-25