超临界GAS法细化级配3-硝基-1,2,4-三唑-5-酮(NTO)

Study on the Particle Gradation of NTO with Supercritical Anti-solvent

采用超临界抗溶剂法(GAS),以丙酮为溶剂,探讨实现3-硝基-1,2,4-三唑-5-酮(NTO)超细化和粒度级配同时完成的过程。通过控制温度、目标压力、压力上升速率等参数,研究了影响NTO结晶颗粒粒度及其分布的主要因素,并从理论上进行分析。在细化的基础上确定适当的条件进行粒度级配实验。结果表明:晶形主要受温度的影响,53℃下,可以得到立方晶形;当目标压力在5MPa时,颗粒粒度在2μm左右且分布窄;压力上升速率越高,沉析颗粒粒度小分布窄。级配实验中,分阶段的改变进气速率是实现粒度级配的关键,级配的结果主要受各阶段的目标压力和压力上升速率的影响。

The ultrafine and particle gradation of NTO can be finished simultaneously in acetone solution using supereriticai CO2 anti-solvent. The influence of the main factors on the particle and particle gradation is discussed through controlling the factors, such as temperature, ulti-pressure, the rate of pressure rising, and theoretic analysis has been made. The results show that the crystal morphology is cube when the experimental temperature is 53℃, when ulti-pressure is 5MPa, the particle size of 2μm can be obtained, and small particle size with narrow size distribution is gained on high rate of pressure rising condition. In the experiment of particle gradation, ulti-pressure and rate of pressure rising in different stage are the principal factors influencing particle gradation.