溶剂—非溶剂法制备超细PYX的影响因素

Influence Factors of Preparation of Ultra-fine PYX by Solvent and Non-solvent Technique

采用溶剂—非溶剂法制备出了平均粒径为1 038.0 nm的超细PYX(2,6-二苦氨基-3,5-二硝基吡啶),探讨了制备工艺条件和干燥方式对PYX粒径的影响。通过单因素和正交试验对影响PYX粒径的主要因素进行了研究,并就产品细化前后的能量输出和撞击感度进行了测试。用正交试验得到最佳工艺条件:炸药溶液浓度为0.08 g/mL,炸药溶液与非溶剂的温度差为70℃,搅拌速度为1 600 r/min,滴加速度为1.0 mL/min,干燥方式为真空冷冻干燥。试验结果表明,影响PYX粒径的因素大小的顺序为干燥方式、溶液浓度、温度差、搅拌速度、溶液滴加速度。而干燥方式在较大程度上决定着产品的粒径和分布。PYX细化后的钢凹值提高了9.9%,特性落高提高到原料PYX的2.5倍。

The ultra-fine PYX which average particle size is 1 038.0 nm is prepared by solvent-non-solvent technique, Some of the technical conditions and drying method which have an effect on the parti- cle size of PYX were studied. The major influence factors were studied by means of single factor test and orthogonal one. Both energy output and impact sensitivity before and after ultra-fine PYX were tested. Optimized technological conditions were obtained, such as temperature contrast 70 ℃ between solution and non-solvent, solution concentration 0.08 g/mL, mixing speed 1 600 r/min, adding rate 1.0 mL/min and vacuum refrigerant drying. Experiment results show that the order of factors affecting particle size of PYX is drying method, solution concentration, temperature contrast, mixing speed, solution added rate. Furthermore, drying method is the most important factor to affect particle size of the product. The steel engraving numerical number of the ultra-fine PYX is higher than that of its material by 9.9 %, its characteristic drop-high is 2.5 times of that of its material.