四硝基并哌嗪在二甲基亚砜中的溶解结晶过程及晶体结构研究

Investigation on Solubility and Crystallization Course of Trans-1,4,5,8-Tetranitro Tetraaza Decalin in Dimethyl Sulphoxide and Its Crystal Structure

采用扫描电子显微镜(SEM)、核磁共振氢谱(1H-NMR)、X射线衍射(XRD)和密度泛函理论(DFT)等测试手段和方法研究一种硝胺化合物四硝基并哌嗪(TNAD)的溶解及结晶过程,表征了其晶体结构;并通过理论分析进一步研究了其晶胞参数和可能存在的分子构型。研究表明,TNAD在二甲基亚砜(DMSO)中溶解性良好,且溶解度曲线采用波尔兹曼函数拟合最合适;从过饱和的DMSO中能得到稳定的TNAD晶体,晶体属于四方晶系。扫描电镜观察晶体形状为规整的长方体。DFT分析表明TNAD可能存在5种不同构型,其中"椅-椅结合式异向构象"和"船-船结合式异向构象"最稳定。

Solubility and crystallization course of a nitroamine compound--trans-1,4,5,8-tetranitro tetraaza decalin（TNAD） was studied, and its crystal structure was characterized by scanning electron microscope（SEM）, H^1-NMR, X-ray diffraction（XRD）, and density functional theory（DFT）. The unit cell parameters and probable molecular configuration were investigated theoretically. It is indicated by study that TNAD has good solubility in dimethyl sulphoxide（DMSO）, and Boltzmann function is a good fit for simulating solubility curves. The stable TNAD crystal can obtained from supersaturated DMSO, and the TNAD crystal belong to the cuboid crystalline system. It is further approved by SEM analysis that the crystal is regular cuboid. It is indicated that there maybe exist five different TNAD molecular configurations through DFT study, and the ＂chair-chair combined different direction conformation＂ or ＂boat-boat combined different direction conformation＂ are more stable herein.