A Polymeric Iodiplumbate(Ⅱ) Templated by Conjugated Quaternary Ammonium: Synthesis, Band Structure and Optical Properties

A new lead(Ⅱ) iodide coordination polymer [(npq)(PbI3)]n 1 (npq = N-propyl- quinolinium) has been synthesized in the presence of npq as structure-directing reagent (SDA). Compound 1 crystallizes in the orthorhombic system, space group Pbca, with a = 19.158(4), b = 7.9909(16), c = 22.929(5) (A), V = 3510.2(12) (A)3, Z = 8, Dc = 2.877 g/cm3, F(000) = 2672, C12H14I3NPb, Mr = 760.14, μ(MoKα) = 14.872 mm-1, the final R = 0.0431 and wR = 0.1021 for 3678 observed reflections with I＞2σ(I). Structure determination indicates that the [PbI3]-n infinite chains in each unit cell shape the sketch of 1, which could be described as the result of face-sharing distorted PbI6 octahedra running along the b axis. Electrostatic interaction between conjugated organic counter-cations and inorganic moieties presents and contributes to the crystal packing. 1 was further characterized with IR and elemental analysis. Based on the crystal structure data, quantum chemical calculation with DFT method was used to reveal the electronic structure and optical property of 1.     

Determination of human IgG by solid-substrate room-temperature phosphorescence immunoassay based on an antibody labeled with nanoparticles containing rhodamine 6G luminescent molecules

Luminescent 50-nm silicon dioxide nanoparticles containing both types of rhodamine 6G (R; particles denoted R-SiO₂) were synthesized by the sol–gel method. In the presence of Pb(Ac)₂ as a heavy atom perturber the particle can emit the intense and stable room-temperature phosphorescence (RTP) signal of R on a polyamide membrane, with _ex^max/_em^max=470/635 nm for R. Our research indicates that the specific immune reaction between goat-anti-human IgG antibody labeled with R-SiO₂ and human IgG can be carried out quantitatively on a polyamide membrane, and the phosphorescence intensity was enhanced after the immunoreaction. Thus a new method for solid-substrate room-temperature phosphorescence immunoassay (SS-RTP-IA) for determination of human IgG was established on the basis of antibody labeled with the nanoparticles containing binary luminescent molecules. The linear range of this method is 0.0624–20.0 pg spot^–1 of human IgG (corresponding to a concentration range of 0.156–50.0 ng mL^–1, sample volume 0.40 L spot^–1). The regression equations of the working curves are I_p=71.27+7.208m_IgG (pg spot^–1) (r=0.9996). Detection limits calculated as 3S_b/k are 0.022 pg spot^–1. Compared with the same IA using fluorescein isothiocyanate (FITC) as the marker the new method was more sensitive and had a wider linear range. After elevenfold replicate measurement RSD are 4.5 and 3.6% for samples containing 0.156 and 50.0 ng mL^–1 IgG, respectively. This method is sensitive, accurate, and of high precision.     

镉与2—[（邻羟苄叉）氨基]酚和吡啶配合物的表征和晶体结构

合成了镉与2-[(邻羟苄叉)氨基]酚(H_2Sap)和吡啶配合物,Cd_2(C_(13)H_9No_2)_2(C_5H_5N)_6.测定其晶体属单针晶系,P2_1/c空间群,的配位构型为八面体.用红外、核磁、热分析等枝术进行了表征.     

新型聚芳醚酮与热致性液晶高聚物共混物流变性能和力学性能的研究

本文研究了新型聚芳醚酮与热致性液晶高聚物(PEK-C/LCP)共混物的流变性能及力学性能。结果表明:由于LCP的加入,PEK-C的熔体粘度降低;随着剪切速率的增加,共混物熔体流动活化能从223.5KJ/mol降为102.2KJ/mol。共混物的玻璃化转变温度从纯PEK-C的218℃降为199℃;除模量增加外,其它力学性能均有所下降。同时利用SEM观察了共混物冲击断面形貌,未发现有LCP微纤维生成。     

Synthesis, Crystal Structure and Electrochemical Properties of One-dimensional Chain Coordination Polymer [Co(Ⅱ)(C6H5CH=CHCOOH)2(4,4''-bipy)(H2O)5]n

A one-dimensional chain coordination polymer [Co(Ⅱ)(C6H5CH=CHCOOH)2(4,4'-bipy)(H2O)5]n has been synthesized with cinnamylic acid, 4,4'-bipy and cobaltous chloride as raw materials. Crystal data for this complex: monoclinic, space group P21/c, a - 1.1481(3), b =1.1230(2), c = 1.1759(3) nm, β = 97.054(4)°, V = 1.5046(6) nm3, Mr= 617.50, Dc = 1.363 g/cm3, Z= 2, μ(MoKα) = 0.627 mm-1, F(000) = 646, S = 1.062, R 0.0443 and wR = 0.1178. The crystal structure shows that two neighboring cobalt(Ⅱ) ions are linked together by one 4,4'-bipy, and the whole complex molecule adopts a one-dimensional chain structure. Each cobalt(Ⅱ) ion is coordinated with two nitrogen atoms from two 4,4'-bipy molecules and four oxygen atoms from four water molecules, giving a distorted octahedral coordination geometry. The electrochemical properties were analyzed by combining with the crystal structure.     

微层共挤出(PP+EVOH)/PP阻隔材料的结构与性能研究

利用微层共挤出技术制备了具有交替层状结构的(PP+EVOH)/PP复合材料,其中PP为聚丙烯,EVOH为乙烯-乙烯醇其聚物.通过扫描电子显微镜观察、气体渗透实验、差示扫描量热仪分析以及力学性能测试研究了微层共挤出复合材料的形态结构及其对复合材料气体阻隔性能、力学性能以及结晶性能的影响.研究结果表明,通过微层共挤出技术,PP层和(PP+EVOH)层沿挤出方向交替排列,EVOH在PP基体中的的分散形态由零维球形变为一维纤维状,进而演变为二维片状.这些形态导致微层共挤出材料的氮气渗透系数和断裂伸长率较普通共混物分别下降了两个数量级和提高了27倍,并且显著影响其结晶行为.当层数超过64层后,由于PP层减薄,界面增多,EVOH不仅对(PP+EVOH)层中PP相存在结晶成核作用,而且对PP层也有结晶成核作用.     

YVO4∶Sm3+红色发光材料的熔盐法合成与光谱性能

采用熔盐法合成了YVO4∶Sm3+红色发光材料. 用X射线粉末衍射对其结构进行表征, 证实样品为具有锆石结构的YVO4相; 测定了样品的激发与发射光谱; 分析了不同的掺杂浓度和烧结温度对样品发光强度的影响. 研究结果表明, 采用熔盐法合成的样品均可以产生Sm3+的特征发射, 但是与其它方法相比, 熔盐法合成样品位于647 nm处Sm3+的4G5/2-6H9/2发射明显得到加强, 从而使得样品发出明亮的红光, 而不是其它合成方法获得的橙色光. 当掺杂浓度为1%(摩尔分数)且在500 ℃下烧结5 h后, 熔盐法得到的YVO4∶Sm3+荧光粉的发光强度最大.     

Synthesis, Structure and Luminescent Property of a Zinc(Ⅱ) Coordination Polymer Incorporating Flexible Cyclohexane-1,2,3,4,5,6-hexacarboxylate Ligand

The hydrothermal reaction of Zn(NO3)2·4H2O, cyclohexane-1,2,3,4,5,6-hexacarboxylic acid hydrate (H6LI·H2O, cis-conformation LI: a,e,a,e,a,e) and 2,2'-bpy yielded a new coordination polymer [Zn2(H2LII)(2,2'-bpy)]·2H2O(trans-conformation LII: e,e,e,e,e,e), which was characterized by single-crystal X-ray diffraction, elemental analysis, IR and XRPD(X-ray powder diffraction). This complex crystallized in the triclinic system, with P1 space group and parameters a=0.66922(5) nm, b=0.97291(8) nm, c=1.22184(9) nm, ...     

系列Sm3+配合物的合成、结构及光物理性能

采用水热方法合成了4种Sm³⁺配合物, 即{[SmZn(2,5-pdc)₂(tp)_0.5(H₂O)]·2H₂O}_n(1), [Sm₂Zn₂(C₆H₅COO)₁₀(Imh)₂(H₂O)₂](2), {[Sm₂(NO₂C₆H₄COO)₆(H₂O)₄]·H₂O}_n(3)和{[SmN(CH₂COO)₃(H₂O)₂]·H₂O}_n(4)[2,5-pdc=2,5-吡啶二羧酸根, tp=对苯二甲酸根, C₆H₅COO=苯甲酸根, Imh=咪唑, NO₂C₆H₄COO=对硝基苯甲酸根, N(CH₂COO)₃=氨三乙酸根]. 通过单晶X射线衍射确定了其晶体结构. 在室温下测定了其红外光谱、 紫外-可见-近红外光谱以及在近红外区和可见区的发射光谱. 结果表明, 4种配合物在近红外区或可见区均出现Sm³⁺离子的特征发射. 这是形成配合物后, Zn-配体部分和配体对Sm³⁺离子发光的敏化作用所致. 此外, 讨论了不同有机配体或d过渡金属离子对Sm³⁺离子发光的影响, 并分析了配合物中Sm³⁺离子的近红外发射带位移、 劈裂和加宽的原因.     

A facile synthesis of a novel energetic surfactant 1-amino-3-dodecyl-1, 2, 3-triazolium nitrate

1-Amino-3-dodecyl-1,2,3-triazolium nitrate, as a novel energetic surfactant, has been synthesized in four steps, namely addition-elimination, cyclization, alkylation and metathesis. Its structure was confirmed by 1H NMR, IR, and MS. The effects of various reaction parameters, including stoichiometry, reaction temperature and time, were investigated in details. In addition, the physical and chemical properties of this energetic surfactant were measured.