La[B5O8(OH)(H2O)]NO3•2H2O的合成与结构

采用熔融硼酸法合成了一种具有层状结构的新型水合稀土多硼酸盐, La[B₅O₈(OH)(H₂O)]NO₃•2H₂O, 并利用单晶X射线衍射技术确定了它的结构. 它属于单斜晶系, P21/n空间群. 其基本构建单元 (fundamental building block, 简称FBB)是由三个BO4和两个BO3基团所构成的一个双三元环[B5O12]基团. 结构中每一个FBB通过共顶点氧原子与周围四个同样的单元连接成具有九元环窗口的二维[B5O10]层, La³⁺位于九元环中心附近. [B5O10]层沿着b方向进行堆积, 硝酸根离子和结构中部分结晶水分子位于相邻的[B5O10]层之间.     

Development of the FTIR properties of nano-structure silica gel doped with different rare earth elements,prepared by sol-gel route

Structural characteristics of pure silica gel (silica-xerogel, SiO₂) and silica gel doped with some rare earth elements (REEs) such as, praseodymium Pr³⁺, and Europium Eu³⁺, Erbium Er³⁺ and Holmium Ho³⁺ ions, with different concentrations ranging from 1 up to 6%, in the form of monolith materials were prepared by sol-gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural features of sol-gel derived monolith are analyzed, namely the structure of nano-particle momolith samples, based on X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR). We show that the XRD spectra of α-crystobalite are obtained for the pure samples at 1100°C and even by doping with the four REEs ions.     

α－芳甲酰基烯酮二硫缩醛的新合成方法

以碳酸钾为碱，芳甲酰丙酮（１）与二硫化碳、卤代烃反应得到２－乙酰基－２－芳甲酰基烯酮硫代缩醛（２），２在乙硫醇钾作用下脱乙酰基生成标题化合物（３）。１→３的转化具有反应条件温和、产物产率高及对３中各种缩醛基均可通用等特点。     

锌的平面三配位[Bu_4N][Zn(SC_6H_2Pr_3~i-2,4,6)_3]·Pr~iOH配合物的合成与晶体结构

在许多重要的金属蛋白中,都存在ⅡB金属与半胱氨酸残基配位的活性中心M(Cys-S)_n.锌、镉、汞与含硫配体的配位化学作为M(Cys-S)_n中心的化学基础,三配位的[M(SR)_3]被认为是金属蛋白中ⅡB金属的一种配位形式.而近年来,Koch报道了平面三配位的锌、镉、汞的硫酚配合物[(n-Pr)_4N][Zn(SC_6HMe_4-2,3,5,6)_3]和[PPh_4][Cd(SC_6H_2Pr_3~i-2,3,6)_3]及[(n-Pr)_4N][Hg(SC_6H_2Pr_3~i-2,4,6)_3]的晶体结构.他们在实验中由于晶体迅速失去溶剂而未能测定以2,4,6-三异丙基硫酚为配体的锌配合物的晶体结构.最近我们合成了这个配合物,并测定了其晶体结构.     

ZrO2对合成二甲醚双功能催化剂表面结构及催化性能的影响

采用共沉淀沉积法制备了Cu基双功能催化剂，并进行了合成气一步法制取二甲醚实验．XRD、XPS以及BET表征结果表明，催化剂中ZrO2以无定形状态存在，且随着其含量的增加，Zr^4 逐渐溶进CuO晶格，两者之间的电子交换使得Cu^2 在活化过程中很难被彻底还原为Cu^0，而是以Cu^0/Cu^ 的形式共存．活性评价结果表明，Cu^ 离子表现出优异的CO转化率和DME选择性．同时，ZrO2的存在能有效调节催化剂表面的Cu／Zn摩尔比以及促进Cu元素在表面的富集，从而改善催化剂性能．     

Solvothermal Synthesis, Crystal Structure and Electrochemical Property of Complex [Co(p-MBA)2(2,2''-bipy)(H2O)]·(H2O)

One novel complex [Co(p-MBA)2(2,2'-bipy)(H2O)]·(H2O) has been synthesized by the reaction of p-methylbenzoic acid with 2,2'-bipyridine in the solvent mixture of water and methanol. It crystallizes in triclinic, space group P-1 with a=0.70479(14), b=1.1211(2), c=1.6718(3) nm, α=103.806(3), β=90.795(3), γ=104.207(3)°, V=1.2399(4) nm3, Mr=512.41, Dc=1.373 g/cm3, Z=2, F(000)=532, μ=0.733 mm-1, R=0.0432 and wR=0.0957. The crystal structural analysis shows that the cobalt atom is coordinated with three oxygen atoms from two p-methylbenzoic acids and one water molecule and two nitrogen atoms from one 2,2'-bipyridine,forming a distorted square-pyramidal coordination geometry. The cyclic voltammetry behavior of the complex is also reported.     

含L－氨基酸结构的手性液晶化合物的合成及其相变行为

合成了９种具Ｌ－氨基酸衍生物结构的介晶化合物（Ｉ－Ⅲ，Ⅳａｂ，Ⅴａ，ｂ，Ⅵａ，ｂ）、４种氨基酸衍生物（Ａ１－４）和６种介晶化合物（Ｍ１－６）．新化合物（Ⅰ－Ⅲ，Ⅳａ，ｂ，Ⅴａ，ｂ，Ⅵａ，ｂ，Ａ４，Ｍ３－６）的化学结构通过ＩＲ、１ＨＮＭＲ和元素分析证实；并用偏光显微观察和ＤＳＣ分析研究了其相变行为，结果表明有８种化合物（Ｍ３－６，Ⅵａ，ｂ，Ⅴｂ，Ⅵｂ）呈现液晶相变。测定了它们的比旋光度。通过Ｘ射线衍射研究了化合物Ⅵｈ１２０～１３０℃和Ⅵｂ１７０～１８０℃的近晶结构，Ⅵｂ显，Ⅵｂ呈。测定了化合物Ⅳｂ的电滞回线，证明其具铁电性。     

新型芳基双西佛碱及其Ni（Ⅱ）,Fe（Ⅲ）配合物的合成

新型芳基双西佛碱及其Ｎｉ（Ⅱ），Ｆｅ（Ⅲ）配合物的合成蓝仲薇，严洪兴，李莉，余孝其（四川大学化学系，成都６１００６４）关键词西佛碱，合成，催化活性西佛碱除广泛用作螯合剂、稳定剂、分析试剂和生物活性剂以外。近年研究表明，其单核和双核金属配合物对于催化作...     

A novel approach to study the isothermal behaviour of substances after 0.01–1 s from the chemical process initiation

New modifications of a contact heater are suggested for investigating thermal decomposition processes, as well as for determining kinetic characteristics of substances under conditions of intense heating to a fixed constant temperature.

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Zusammenfassung Zur Untersuchung von thermischen Zersetzungsprozessen und der Bestimmung der Reaktionskinetik von Substanzen bei intensivem Erhitzen auf vorgegebene konstante Temperaturen wird eine neue Abart von Kontakterhitzern beschrieben.

     

Local and non-local sources of airborne particulate pollution at Beijing--The ratio of Mg/Al as an element tracer for estimating the contributions of mineral aerosols from outside Beijing

A new element tracer technique has firstly been established to estimate the contributions of mineral aerosols from both inside and outside Beijing. The ratio of Mg/Al in aerosol is a feasible element tracer to distinguish between the sources of inside and outside Beijing. Mineral aerosol, inorganic pollution aerosol mainly as sulfate and nitrate, and organic aerosol are the major components of airborne particulates in Beijing, of which mineral aerosol accounted for 32%―67% of total suspended particles (TSP), 10%―70% of fine particles (PM2.5), and as high as 74% and 90% of TSP and PM2.5, respectively, in dust storm. The sources from outside Beijing contributed 62% (38%―86%) of the total mineral aerosols in TSP, 69% (52%―90%) in PM10, and 76% (59%―93%) in PM2.5 in spring, and 69% (52%―83%), 79% (52%―93%), and 45% (7%―79%) in TSP, PM10, and PM2.5, respectively, in winter, while only ～20% in summer and autumn. The sources from outside Beijing contributed as high as 97% during dust storm and were the dominant source of airborne particulates in Beijing. The contributions from outside Beijing in spring and winter are higher than those in summer, indicating clearly that it was related to the various meteorological factors.