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

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

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8μm,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%.

In order to improve the decomposition performance and dispersibility of ammonium perchlorate(AP),the crude lead ferrocyanide(Pb2 Fe(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 Pb2 Fe(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 quasispherical,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 from446. 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 Pb2 Fe(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%.