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Engineering the Morphology and Particle Size of HighEnergetic Compounds Using Drop-by-Drop and Drop-to-Drop Solvent–AntisolventInteraction Methods

机译:工程高形貌和粒径使用逐滴和逐滴溶剂-反溶剂的高能化合物互动方式

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摘要

Morphology-controlled precipitation of three powerful organic high energetic compounds (HECs) viz. cyclotrimethylenetrinitramine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX), and 2-methyl-1,3,5-trinitrobenzene (TNT) was achieved by two different processes, namely, drop-by-drop (DBD) and drop-to-drop (DTD) solvent–antisolvent interaction methods. Effect of different experimental parameters on the mean size and morphology of the prepared submicron-sized particles of HECs was investigated thoroughly. The DBD method favors the formation of nanosized particles of RDX and TNT at lower concentrations (5 mM). However, a significant increase in the mean particle size occurred at higher concentrations (25 and 50 mM). Formation of facetted crystals of RDX, HMX, and nanorods of TNT was observed at higher concentrations because of the interaction of crystal facets with the antisolvent. Relatively, smaller sized, spherical particles of RDX and HMX could be prepared through the DTD method even at higher concentrations (25 mM). The DTD method is a continuous process and hence is a facile method forindustrial applications. X-ray diffraction and Fourier transform infraredspectroscopy studies revealed that RDX, HMX and TNT were precipitatedin their most stable polymorphic forms α, β, and monoclinic,respectively. Differential scanning calorimetry showed that the thermalresponse of the nano-HECs was similar to the respective raw-HECs.A slight decrease in crystallinity and the melting point was observedbecause of the decrease in the mean particle size.
机译:三种强有机高能化合物(HEC)的形态控制沉淀。环三亚甲基三硝胺(RDX),八氢-1,3,5,7-四硝基-1,3,5,7-四唑啉(HMX)和2-甲基-1,3,5-三硝基苯(TNT)通过两种不同的方法获得过程,即逐滴(DBD)和逐滴(DTD)溶剂-反溶剂相互作用方法。彻底研究了不同实验参数对制备的HEC亚微米级颗粒平均尺寸和形态的影响。 DBD方法有利于在较低浓度(5 mM)下形成RDX和TNT纳米颗粒。但是,在较高浓度(25和50 mM)下,平均粒径显着增加。由于结晶面与抗溶剂的相互作用,在较高浓度下观察到RDX,HMX和TNT纳米棒的结晶面形成。相对而言,即使在较高浓度(25 mM)下,也可以通过DTD方法制备较小尺寸的RDX和HMX球形颗粒。 DTD方法是一个连续过程,因此是一种简便的方法工业应用。 X射线衍射和傅立叶变换红外光谱研究表明RDX,HMX和TNT沉淀以最稳定的多态形式α,β和单斜晶系分别。差示扫描量热法显示纳米-HEC的响应类似于各自的原始-HEC。观察到结晶度和熔点略有下降因为平均粒径的减小。

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