【摘要】 为了探索多硝基含能化合物的合成及其热分解性能，以4-氯-3,5-二硝基苯胺为原料，在乙酸酐溶液中加入4-氯-3,5-二硝基苯胺，乙酰化反应生成4-氯-3,5-二硝基乙酰苯胺（化合物Ⅰ）,收率为91.7%;化合物Ⅰ在室温下硝化2h,制得4-氯-1-硝氨基-2,3,5,6-四硝基苯（化合物Ⅱ）,收率为69.1%;采用傅里叶变换红外光谱（FT-IR）、核磁共振光谱（NMR）和元素分析（EA）对两种物质的结构进行了表征；培养了两种化合物的单晶，通过X-射线单晶衍射（SC-XRD）测定化合物的晶体结构；采用氮当量公式（NE）和修正氮当量公式（MNE）计算了化合物Ⅱ的爆轰性能，采用DSC和TG测试了化合物Ⅱ的热分解过程，并根据Kissinger法和FWO法计算了化合物Ⅱ的表观活化能（E）和指前因子（A）,计算了放热分解过程的初始分解温度(T_p0)、自由活化能（ΔG^≠）、活化焓（ΔH^≠）、活化熵（ΔS^≠）,并估算了热爆炸临界温度(T_bp0)。结果表明，化合物Ⅰ的相对分子质量为259.61,空间群为C2,化合物Ⅱ的相对分子质量为352.5,空间群为C2/c,两种化合物的晶体结构均属单斜晶系；DSC显示，化合物Ⅱ在438.20K时达到最大放热峰，具有较好的热稳定性，爆轰参数表明该物质能量较高，有望成为极具前途的高能量高密度含能化合物。更多还原

【Abstract】 In order to explore the synthesis and thermal decomposition properties of polynitro energetic compounds, 4-Chloro-3,5-dinitroacetaniline（compound Ⅰ） was synthesized by acetylation of 4-chloro-3,5-dinitroaniline with the yield of 91.7% by using 4-chloro-3,5-dinitroaniline as raw material. 4-Chloro-1-amino-2,3,5,6-tetranitrobenzene（compound Ⅱ） was obtained by the nitrification of compound I for 2h at room temperature with the yield of 69.1%. The structures of two compounds were characterized by Fourier transform infrared spectroscopy（FT-IR）, nuclear magnetic resonance spectroscopy（NMR） and elemental analysis（EA）. The single crystals of the two compounds were cultivated, and the crystal structure of two compounds were determined by single crystal X-ray diffraction（SC-XRD）. The detonation performance of compound Ⅱ was calculated by using nitrogen equivalent formula（NE） and modified nitrogen equivalent formula（MNE）. The thermal decomposition process of compound Ⅱ was studied by DSC and TG, and the apparent activation energy（E） and pre-exponential factor（A） of compound Ⅱ were calculated by Kissinger method and FWO method. The initial decomposition temperature(T_p0), free energy of activation（ΔG^≠）, activation enthalpy（ΔH^≠）, and activation entropy（ΔS^≠） of the exothermic decomposition process were also calculated, and the critical temperature of thermal explosion(T_bp0) was estimated. The results show that the molecular mass of compound Ⅰ is 259.61 with the space group of C2, the molecular mass of compound Ⅱ is 352.5 with the space group of C2/c, and the crystal structure of both compounds belong to the monoclinic system. DSC study shows that compound Ⅱ reaches the maximum exothermic peak at 438.20K, implying its good thermal stability. The good detonation parameters indicate that it is expected to be a promising high energy density compound.更多还原