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Application of Internal Seeding and Temperature Cycling for Reduction of Liquid Inclusion in the Crystallization of RDX

机译:内部晶种和温度循环在减少RDX结晶中的夹杂物中的应用

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In the cooling crystallization of cyclotrimethylene trinitramine (RDX) from γ-butyrolactone, an internal seeding method combined with temperature cycling, was applied to suppress liquid inclusion and improve particle size and size distribution for RDX at initial saturation temperatures of 60-80 °C. The process parameters including initial cooling rate, the range of the temperature cycle, and recooling rate during crystal growth period were determined based on direct measurements of size and amount of liquid inclusion of RDX crystals. Crystal size was measured by a dynamic light scattering particle size analyzer. Liquid inclusion was characterized in mass and area measurement based content by gas chromatography and matching refractive index method combined with image analysis. In the present work, RDX particles with average crystal sizes of 169.0-322.0 μm and inclusion area contents of 4.4-5.3% were obtained. Those values imply that the crystal quality of RDX is much improved compared with those of commercial RDXs such as Hanwha-RDX (conventional grade; average crystal size of 158.0 μm and inclusion area content of 9.3%) and I-RDX (reduced sensitivity grade; average crystal size of 218.0 μm and inclusion area content of 5.0%). For instance, the average crystal size of RDX obtained from a saturated solution at 70 °C by the present method is 290.3 μm, which was much larger than that of I-RDX, but the inclusion area content was about 4.6%, which was even lower than that of I-RDX.
机译:在从γ-丁内酯中冷却环三亚甲基三硝胺(RDX)的结晶过程中,采用内部晶种方法与温度循环相结合,以抑制液体的夹杂并改善RDX在60-80°C的初始饱和温度下的粒径和尺寸分布。基于直接测量RDX晶体的尺寸和液体内含物的量,确定了包括初始冷却速率,温度循环范围和晶体生长期间的再冷却速率在内的工艺参数。晶体尺寸通过动态光散射粒度分析仪测量。通过气相色谱和匹配折射率法结合图像分析,在基于质量和面积测量的含量中表征了液体夹杂物。在目前的工作中,获得了RDX颗粒,其平均晶体尺寸为169.0-322.0μm,夹杂物含量为4.4-5.3%。这些值表明,与商用RDX(如韩华RDX(常规级;平均晶体尺寸为158.0μm,夹杂物含量为9.3%)和I-RDX(降低的灵敏度级))相比,RDX的晶体质量有了很大提高。平均晶体尺寸为218.0μm,包含区域的含量为5.0%)。例如,通过本方法从70℃的饱和溶液中获得的RDX的平均晶体尺寸为290.3μm,比I-RDX的平均晶体尺寸大得多,但是包含区域的含量为约4.6%,甚至低于I-RDX。

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