超临界二氧化碳GAS重结晶制备HMX微细颗粒的研究

Microparticle Formation of HMX by Supercritical Carbon Dioxide Antisolvent Recrystallization

比较了ＣＯ２对丙酮、环己酮、二甲基亚砜体积膨胀的影响和ＨＭＸ（奥克托金）在上述三种溶剂中ＧＡＳ重结晶时的析晶率。以丙酮为溶剂用ＣＯ２ＧＡＳ重结晶，在一定的条件下可获得２～１３μｍ。β－型ＨＭＸ微细颗粒。考察了压力、温度、溶液初始浓度及溶液膨胀速率对ＧＡＳ重结晶过程、晶粒大小和晶型的影响以及晶体的增长。结果表明，在８．０～１２．０ＭＰａ、较低的温度和较低的溶液初始浓度条件下，可获得微细的β－型ＨＭＸ颗粒。

The recrystallization ratio of 1, 3, 5, 7-tetranitro-1, 3, 5, 7-tetraazacyclooctane (HMX) in acetone,cyclohexanone and dimethylsulphoxide solution using supercritical carbon dioxide antisolvent(GAS)was compared. By using GAS process in acetone solution , microparticles of β-HMX within 2～13μm can be obtained.Effects of pressure ,temperature, initial feed concentration of HMX solute,expansion speed of solution and growth of crystal on the GAS process have been studied.Under all experimental pressures of 8. 0～12.0 MPa tested,lower test temperature and lower concentration of feed solution were preferable for obtaining β-HMX andmicroparticles.