Nitration of Chitin Monomer: From Glucosamine to Energetic Compound

The nitration of chitin monomer in a mixture of nitric acid and acetic anhydride was conducted and a highly nitrated (3R,4R,6R)-3-acetamido-6-((nitrooxy)methyl)tetrahydro-2H-pyran-2,4,5-triyl trinitrate (1) was obtained. Its structure was fully characterized using infrared spectroscopy, NMR spectroscopy, elemental analysis, and X-ray diffraction. Compound 1 possesses good density (ρ: 1.721 g·cm⁻³) and has comparable detonation performance (V_d: 7717 m·s⁻¹; P: 25.6 GPa) to that of nitrocellulose (NC: V_d: 7456 m·s⁻¹; P: 23 GPa; I_sp = 239 s) and microcrystalline nitrocellulose (MCNC; V_d: 7683 m·s⁻¹; P: 25 GPa; I_sp = 250 s). However, Compound 1 has much lower impact sensitivity (IS: 15 J) than the regular nitrocellulose (NC; IS: 3.2 J) and MCNC (IS: 2.8 J). Compound 1 was calculated to exhibit a good specific impulse (I_sp: 240 s), which is comparable with NC (I_sp: 239 s) and MCNC (I_sp: 250 s). By replacing the nitrocellulose with Compound 1 in typical propellants JA2, M30, and M9, the specific impulse was improved by up to 4 s. These promising properties indicate that Compound 1 has a significant potential as an energetic component in solid propellants.     

沸石分子筛合成由微孔向中孔的飞跃

介绍了沸石分子筛合成由微孔向中孔的发展及中孔分子筛的合成近况, 比较了两类材料在合成、机理及模板作用的特殊性等方面的差异。     

丙烷氧化反应中多组分氧化物Bi－V－Mo－O催化作用的红外光谱研究

迄今对于含有铝、秘复合氧化物催化剂的活性中心和作用机理存在不同看法,本文采用红外光谱法,探讨了复合氧化物钥钒酸秘在丙烷选择氧化反应中的催化作用机理.     

双(甲基环戊二烯基)二(2,6-二氯苯氧基)铪的晶体和分子结构

本文用X-射线衍射法测定了(η⁵CH₉C₅H₄)₅H₁(OC₆H₉Cl₃-2,6)₂的晶体和分子结构.晶体结构属单科晶系,空间群为P²1/c,晶胞参数为a=17.010(2)Å,b=8.577(1)Å,C=16.313(3)Å,β=101.52(3)°,晶胞内分子数Z=4.分子内有非结晶学二次旋转轴对称性,铪原子周围的两个甲基环戊二烯基和两个氧原子构成一个变形四面体.两个环戊二烯基的平面夹角为125.33°.氧-铪-氧键角为103.71°.铪-氧键长为2.004-2.022Å,较铪-氧单键键长为短,表明具有部分双键特性.     

用乙二胺和1,6-己二胺作催化剂合成中孔MCM-41分子筛(英文)

首次在温和条件下,用在传统微孔沸石合成中常作为导向剂的乙二胺或1,6-己二胺替代NaOH作催化剂合成出SiO2基中孔MCM-41分子筛。合成样品用XRD和N2吸附等温线进行表征。实验结果表明,由于这种替代,使相应合成样品及焙烧样品的中孔骨架结构的有序度明显提高。在XRD图中四个衍射峰清晰可辨,是典型的六方紧密堆积,晶胞参数a0分别为4.11nm和3.75nm,且d100值随所用胺分子中碳链的增长逐渐从3．56nm减少到3．24nm,同时产物孔径由中孔转变为微孔。     

傅立叶变换拉曼光谱和红外光谱鉴别塑料

用傅立叶变换拉曼光谱、衰减全反射红外光谱和近红外光谱结合OPUS/Ident软件对添加不同填料、不同助剂的塑料进行鉴别分类。结果表明:分子光谱结合化学计量学鉴别塑料是一种快速可靠的方法。其中拉曼光谱和衰减全反射红外光谱能够直接区分样品,而近红外光谱非常类似,不能直接区分。但是用OPUS/Ident软件中的W ard算法处理这3种光谱后,得到的树形图能够将样品准确分类。     

Up‐conversion luminescence of ytterbium and thulium codoped potassium yttrium double tungstate crystal

Thulium and ytterbium co‐doped double tungstate Yb³⁺,Tm³⁺: NaY(WO₄)₂ single crystals were prepared by using RF‐heating Czochralski (CZ) pulling method. Its polarized transmittance spectra have been recorded in the region of 290‐2000 nm at room temperature. The energy levels transitions were assigned to the corresponding absorption line. The up‐conversion luminescences at 793 nm and 475 nm were measured when the sample were pumped by 972 nm LD and the energy transfer mechanism between Yb³⁺ and Tm³⁺ ions was analyzed.     

求解对流扩散方程的一种高效的有限体积法

考虑无结构三角网格上求解对流扩散方程的有限体积法.引入一种梯度函数的计算方法,将现有方法中计算解变量在网格单元中心和网格单元边界的梯度的两个独立过程改造成一个过程来完成,发展了一种求解对流扩散方程的高效的有限体积法.数值实验结果表明,该方法完全达到了已有方法同样的精度,而在计算速度上有明显的提高.     

超临界CO2萃取、HPLC法测定川芎中的阿魏酸

采用超临界CO2萃取法提取川芎中的阿魏酸,通过试验确定了最佳超临界萃取条件,萃取罐的温度为60℃、萃取压力为35 MPa、萃取时间为2 h。以甲醇-水-冰乙酸(体积比为30∶70∶0.2)为流动相,用HPLC法测定川芎中的阿魏酸,回收率为92.3%~103.4%,相对标准偏差为2.45%(n=6)。     

稀土掺杂La-Al-EU-1分子筛的合成与表征

在HMBr2-Na2O-Al2O3-SiO2-La2O3-H2O体系中,采用水热法合成了高结晶度的La-Al-EU-1分子筛。通过XRD,FT-IR,XPS,TG-DTG和UV-Vis DRS等手段对合成样品进行分析。结果表明:随着原始溶胶中镧的质量分数增加,La-Al-EU-1分子筛晶胞体积膨胀;FT-IR骨架振动频率向低波数方向移动,在约980 cm-1处出现Si-O-La对称伸缩振动谱带;在λ=245 nm分子筛骨架O原子的成键2p电子向骨架四配位的La原子的空d轨道的p-d跃迁产生的特征峰强度增强;La3d3/2和La3d5/2伴峰电子结合能比La2O3高1.0 eV,氧的O1s电子结合能比La2O3高1.1 eV,La3d和O1s的电子结合能同步向高能方向移动,导致La-O键共价性减少,电子云密度降低,La-O键长增加,证明了La原子已经进入了分子筛骨架,并以La3+离子四配位方式存在;当ωLa0.82%,n(SiO2)/n(Al2O3)=50~80时,晶化时间24~41 h,可以合成高结晶度的La-Al-EU-1分子筛。