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兵工学报 ›› 2019, Vol. 40 ›› Issue (11): 2220-2228.doi: 10.3969/j.issn.1000-1093.2019.11.006

• 论文 • 上一篇    下一篇

超细亚铁氰化铅/高氯酸铵复合粒子的制备及热分解、防团聚性能研究

张正金1, 郭效德1, 刘杰1, 梁力1, 李宽宽1, 夏亮1, 常志鹏1, 田淑宝2, 黄东彦2, 杨雪芹2   

  1. (1.南京理工大学 国家特种超细粉体工程技术研究中心, 江苏 南京 210094;2.山西北方兴安化学工业有限公司, 山西 太原 030008)
  • 收稿日期:2019-01-11 修回日期:2019-01-11 上线日期:2019-12-31
  • 通讯作者: 郭效德(1968—),男,研究员,博士生导师 E-mail:guoxiaodenj@163.sina.com
  • 作者简介:张正金(1995—),男,硕士研究生。E-mail: 2587077960@qq.com
  • 基金资助:
    国家自然科学基金项目(51606102)

Preparation of Ultrafine Lead Ferrocyanide/ammonium Perchlorate Composite Particles and Study of Their Thermal Decompositionand Anti-agglomeration Performance

ZHANG Zhengjin1, GUO Xiaode1, LIU Jie1, LIANG Li1, LI Kuankuan1, CHANG Zhipeng1, XIA Liang1, TIAN Shubao2, HUANG Dongyan2, YANG Xueqin2   

  1. (1.National Special Superfine Powder Engineering Research Center of China, Nanjing University of Science and Technology, Nanjing 210094,Jiangsu, China;2.Northern Xing'an Chemical Industry Co., Ltd., Taiyuan 030008, Shanxi, China)
  • Received:2019-01-11 Revised:2019-01-11 Online:2019-12-31

摘要: 为提高高氯酸铵(AP)的分解性能,改善AP的团聚问题,采用配位沉淀法合成亚铁氰化铅(Pb2Fe(CN)6),并通过立式搅拌球磨机对其进行粉粹纳米化,分别采用直接研磨法、超声辅助法、溶剂非溶剂法3种不同的方法制备超细Pb2Fe(CN)6/AP复合粒子。通过扫描电镜、激光干法粒度仪、X射线衍射仪、红外光谱仪、差示扫描量热对所制备的复合粒子形貌、粒度分布、晶体结构、热分解性能进行表征,并研究了样品的防团聚性能等。结果表明:溶剂非溶剂法合成复合粒子形貌为准球形,粒径约8 μm,分散较为均匀,复合效果较好;AP在纳米Pb2Fe(CN)6的催化下,直接研磨法所制备的复合粒子高温分解温度由原来的446.3 ℃降低至390.4 ℃,超声辅助法降低至391.2 ℃, 溶剂非溶剂法降低至379.1 ℃;Pb2Fe(CN)6/AP复合粒子较纯AP高温分解活化能降低了14.2%,速率常数提高了28.6倍;Pb2Fe(CN)6与AP复合后能有效地阻止AP 的团聚,同时Pb2Fe(CN)6/AP 复合粒子相比于同粒径的纯AP松装堆积密度提高了6.16%,振实堆积密度提高了10.4%.

关键词: 亚铁氰化铅, 高氯酸铵, 复合粒子, 热分解, 防团聚

Abstract: In order to improve the decomposition performance and dispersibility of ammonium perchlorate (AP), the crude lead ferrocyanide (Pb2Fe(CN)6) was synthesized by using the coordination precipitation method, and the nanometer-scale particles were pulverized by using a vertical stirring ball mill. Ultrafine Pb2Fe(CN)6/AP composite particles were prepared by using direct grinding method, ultrasonic assisted method and solvent-nonsolvent method. The morphology, particle size, crystal structure and thermal decomposition performance of the prepared composite particles are characterized by using scanning electron microscope, dry laser granulometer, X-ray diffractometer, infrared spectrometer and differential scanning calorimetry. The morphology of composite particles synthesized by solvent-nonsolvent method is quasi-spherical, the particle size is about 8 μm, the dispersion is relatively uniform, and the coating effect is better. Compared with pure AP, the pyrolysis temperatures of the composite particles prepared by direct grinding method, the ultrasonic assisted method and the solvent non-solvent method are reduced from 446.3 ℃ to 390.4 ℃,391.2 ℃and 379.1 ℃, respectively. The activation energy of pyrolysis is reduced by 14.2%, and the rate constant k is increased by 28.6 times. The combination of AP and Pb2Fe(CN)6 can effectively prevent AP agglomeration, meanwhile, the apparent bulk density is increased by 6.16%,and the tap density is increased by 10.4%. Key

Key words: leadferrocyanide, ammoniumperchlorate, compositeparticle, thermaldecomposition, anti-agglomeration

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