以4-(2,4,6-三硝基苯胺基)苯甲酸(TABA)为配体,采用溶剂挥发法合成出了一种新型铅配合物:{[PbL2(DMF)H2O]·2(DMF)H2O}n(1)(L=4-(2,4,6-三硝基苯胺基)苯甲酸根,DMF=N,N-二甲基甲酰胺).用X-射线单晶衍射仪测定了它的单晶结构.用TG-DSC测定了其热分解过程.在不同升温速率下测试了配合物1与RDX(质量比1∶1)混合物的DSC曲线.计算了该混合物热分解反应的动力学参数.结果表明,该配合物属于单斜晶系,P2(1)/c空间群,晶体参数为:a=6.900(2)(A),b=19.162(6)(A),c=34.866(11)(A),β=94.261 (4)°,V=4597(3)(A)3,Z=4.以Pb(Ⅱ)为桥联离子与4-(2,4,6-三硝基苯胺基)苯甲酸根配位形成一维配位聚合物链.配合物1的热分解主要经历四个阶段.第一阶段发生在58~84℃,主要失去结晶态、配位态水分子及部分结晶状态的DMF.第二阶段为84~231℃,主要是剩余DMF分子的失去.231~320℃和320~415℃为第三和第四阶段,主要是有机含能配体TABA2-的放热分解,在296℃及335℃出现放热峰.配合物1可促进了RDX的热分解.
以苦基氯为初始原料,经过叠氮化,脱氮环化合成4,6-二硝基苯并氧化呋咱.4,6-二硝基苯并氧化呋咱与无机钠盐反应合成其钠盐.通过红外图谱、1 H-NMR、13C-NMR、元素分析、有机质谱等分析对其结构进行了表征.综述分析上述分析数据并通过C-H相关二维谱的分析基本确定了4,6-二硝基呋咱钠盐的结构为7-羟基-4,6-二硝基苯并氧化呋咱钠.
AlH3是一种性能优异的功能材料,广泛应用于复合固体推进剂,燃料电池,高分子合成等诸多领域,目前已知的7种晶型中α-AlH3最稳定,介绍了α-AlH3相关理化性质以及表征手段,综述了α-AlH3的制备技术,并简要阐述了各种制备方法的利弊,最后提出Brower法具有规模化生产的潜力,以及目前Brower法所要解决的问题.
Nano lead(II) citrate was synthesized by liquid dispersion deposition method using PEG-400 as surfactant and characterized by infrared spectroscopy(IR),elemental analysis and transmission electron microscopy(TEM).The nano lead(II) citrate/RDX composite was prepared via a dissolution/dilution/crystallization method.The structure and thermal decomposition properties of the composite was characterized by TEM,SEM and TG-DSC.The results show that nano lead(II) citrate particles attach to RDX and the composite with particle diameter of 6-10μm is formed.The lead content of the composite is 4.990% according to ICP analysis.The content of combustion catalyst in the composite is calculated to be about 8.602%.
Under acetylene atmosphere and 500℃,carbon/active aluminum composite was prepared with CVD method.The physical phase,morphology and composition of the composite were analyzed and tested by means of X-ray diffroction(XRD),scanning electron microssopy(SEM) and transmission electron microscopy(TEM).The results show that the carbon/active Al composite exhibits a special core-shell structure and excellent anti-water ability.
Perovskite-type Lead zirconate titanate (PZT) powders were synthesized by a modified sol-gel method. In this route, citric acid (CA) was used a chelating agent to keep the metal ions in homogeneous solution without undergoing precipitation. The obtained powders were characterized by XRD, FT-IR, SEM-EDS techniques. Phase-pure perovskite structure was formed at 500 degrees C. Combustion tests were carried out to investigate the effect of PZT powders on the burning rate of NC/RDX/NG propellant. It is found that PZT powders increase the burning rate of the propellant to the extent 50% as well as bring down the pressure exponent n to 0.25 (5-20 MPa).
在相转移催化剂四丁基溴化铵存在下,奥硝唑与碱性溶液反应,脱去HCl,得到1-(2,3-环氧丙基)-2-甲基-5-硝基咪唑。研究了碱性溶液种类、碱性溶液的浓度、催化剂加入量、反应温度对目标产物收率的影响。结果表明,较佳反应条件为:奥硝唑∶四丁基溴化铵(质量比)=0.6,碱性溶液为5%NaOH水溶液,反应温度15℃,反应时间1 h,在此条件下,目标产物收率83.9%,纯度99.4%。对目标产物进行了IR及1H NMR表征,并对催化反应机理进行了分析。
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), H1-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 thechair-chair combined different direction conformationor boat-boat combined different direction conformationare more stable herein.
[Pb(DNI)2(H2O)4] was prepared by mixing the aqueous solution of sodium 2,4-dinitroimidazolate and lead nitrate.The single crystal structure of [Pb(DNI)2(H2O)4] has been determined by single crystal diffraction analysis.The crystal monoclinic space group Cc with crystal parameters of a=6.517(3)×10-1 nm,b=17.131(6) ×10-1 nm,c=14.082(7)×10-1 nm,α= 90.00(3) °,β=97.80(4)°,γ=90.00(4) °,V=1 557.5(12)×10-3 nm3,Z=4,Dc=2.531 g/cm-3,μ=11.001 mm-1,F(000)=1 120.The final deviation factor R is 0.022 6.According to the IR spectra analysis,the element analysis and the X-ray diffraction analysis,the chemical component of the 2,4-DNI lead complex is C6H10O12N8Pb and its formula is [Pb(DNI)2(H2O)4].
通过2,4-二硝基咪唑(2,4-DNI)钠盐的水溶液与硫酸铜的水溶液反应,制备出2,4-二硝基咪唑铜配合物;采用自然挥发法培养出了适于X光结构测定的单晶,X射线衍射测定结果显示,晶体属三斜晶系,空间群为P-1,晶体学参数为:a=7.2560(10)×10-1nm,b=7.762(2)×10-1nm,c=16.685(3)×10-1nm,α=87.13(3)°,β=83.81(3)°,γ=62.25(3)°,V=826.8(3)×10-3nm3,Z=2,Dc=1.871 g.cm-3,μ=1.411 mm-1,F(000)=470,最终偏离因子R为0.0388。根据红外光谱、元素分析和X射线衍射分析结果,确定2,4-二硝基咪唑铜配合物的化学组成为C6H10CuN8O13;分子结构式为[Cu(DNI)2(H2O)2].3H2O。
为解决惰性催化剂加入到固体推进剂中引起能量降低的问题,以咪唑为原料经两步硝化、热重排和复分解反应合成了一种新型含能燃烧催化剂2,4-DNI铅盐(PDNI).测试了其机械感度、相容性等性能,并与PNTO进行了比较.结果表明,PNTO和PDNI与NC/NG体系均具有较好的化学相容性,比PNTO具有更低的机械感度和更好的热稳定性.将其作为含能燃烧催化剂应用于固体推进剂中,考察其对燃烧性能的影响,结果表明,PDNI在螺压改性双基推进剂配方中的燃烧催化作用与2,4-二羟基苯甲酸铅相当.
Two tetrafunctional poly-isocyanate energetic curing agents with different molecular weight (EO03-1 and EO03-3) were synthesized via reaction of azido polyether polyol with hexamethylene diisocyanate (HDI). The reaction conditions and post processing steps were investigated. There was an exothermic peak at 252.89 °C referring to the thermal decomposition of azido group in differential scanning calorimetry (DSC) plot of EO03-3 and the glass transition temperature (Tg) was found at -47.13 °C. Thermal decomposition peak of GAP/EO03-3 elastomer was found to be at 254.56 °C and the Tg was found at -45.78 °C. To estimate the potential utility of EO03 in solid rocket propellants, an nitric acid ester, triethylene glycol dinitrate (TEGDN), was added to GAP/EO03-3 system as an energetic plasticizer. It was homogeneous even as the amount of TEGDN was equal to GAP/EO03-3 system and Tg of GAP/EO03-3/50%TEGDN was found at -69.08 °C. Mechanical properties of GAP/EO03 and GAP/EO03-3/chain extender were also studied.
To improve the mechanical properties of the binder system,a novel azido poly-isocyanate energetic curing agent(EC) was synthesized via additional reaction of azido polyether polyol and hexamethylene diisocyanate(HDI).The material ratio,reaction temperature and post processing steps on the reaction were studied.The DSC results show that for EC,there was an exothermic peak at 252.89℃ and the glass transition temperature(T_g) was found at-47.13℃;for the EC/GAP system,thermal decomposition peak was at 254.56℃ and the glass transition temperature(T_g) was found at-45.78℃.And the EC/GAP/50%TEGDN system have good physical and chemical compatibility,there were two peaks at 213.05℃ and 250.89℃,and the glass transition temperature(T_g) was found at-69.08℃.The tensile strength and break elongation value of GAP/EC system is 0.67MPa and 129%,respectively,which is better than that of 0.5MPa and 56.5% of GAP/N100 system at 20℃.