Synthesis and Structure of Dimolybdenum Carbonyl Thiolate Compound [Et4N]2[Mo2（CO）8（SC6H4—CH3—m）2]

1 INTRODUCTION In 1984, thiolate ligand was successfully introduced into molybdenum carbonyl compound by the reaction of Mo(CO)6 with [Et4N]SR( R = C6H5, But) in a moderate condition[1]. From then on, a series of dinuclear molybdenum(0) carbonyl thiolate compounds have been synthesized and characterized by using a variety of thiolate ligands in our research group. It was found that a planar Mo2S2 unit is in the compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-p)2][2] (2) and a "butterfly" t…     

Sm2O3对CuO-γ-Al2O3催化剂性能的影响

在色谱微反流动法实验装置上考察了负载Ｓｍ２Ｏ３对ＣｕＯγＡｌ２Ｏ３催化剂ＣＯ氧化活性的影响，并运用Ｘ射线衍射（ＸＲＤ）、程序升温还原（ＴＰＲ）及程序升温脱附（ＴＰＤＭＳ）技术研究了Ｓｍ２Ｏ３对ＣｕＯγＡｌ２Ｏ３催化剂的物相结构、氧化还原特性及表面氧的脱附与恢复行为的影响。结果表明，负载适量的Ｓｍ２Ｏ３对ＣｕＯγＡｌ２Ｏ３催化剂表面氧的脱出与恢复有促进作用，可使部分γＡｌ２Ｏ３相变成γＡｌ２Ｏ３和θＡｌ２Ｏ３的混合型。负载适量的Ｓｍ２Ｏ３能改善催化活性，而负载过量的Ｓｍ２Ｏ３则使ＣｕＯ催化剂上ＣｕＯ的晶粒增大，从而对催化活性起了抑制作用。     

钯催化下有机锡化合物的偶联反应在碳-碳键形成过程中的应用

本文述评了最近几年来钯催化的有机锡化合物与有机亲电试剂的交叉偶联反应在有机合成中用于碳-碳键形成的主要研究成果。主要讨论了直接交叉偶联反应,CO或烯键插入的交叉偶联反应和机理。     

均匀沉淀法制备Co(OH)2及其超电容特性

以氯化钴为原料、氨水(28wt%)为沉淀剂采用均匀沉淀法成功地合成了Co(OH)₂。X-射线衍射(XRD)、扫描电镜(SEM)测试表明，表面活性剂Tween-80的加入使所制备的α-Co(OH)₂呈现出类似花朵的形貌;循环伏安、恒电流充放电、交流阻抗和循环寿命等电化学测试表明，该材料的电化学性能也得到一定的提高，其单电极比电容可达到370 F·g^-1。     

A convenient synthesis of 2-aryl substituted benzo[f] [1,2,4]triazolo[1,5-a]azepine derivatives

A convenient synthetic pathway to 2-aryl-5,6-dihydro-4H-benzo[f][1,2,4]triazolo[1,5-α]azepine derivatives 7 was developed. The synthesis was based on the cycloaddition of the 1,2,3,4-tetrahydronaphthalene a-acetoxy azo compounds 3 with Ar-CN in the presence of AlCl3 and the consecutive ring enlargement.     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

纳米SrTiO3对高铁酸盐电化学性能影响研究

Two ferrates, K₂FeO₄ and BaFeO₄, had been prepared and characterized by XRD, IR and SEM. The electrochemical tests of the samples were carried out in the voltage range of 0.8～2.0 V and current density of 0.5～3.0 mA·cm^-2. The results indicated that performance of Zn-BaFeO₄ battery was superior to that of Zn-MnO₂ and Zn-K₂FeO₄ batteries. Nanometer SrTiO₃ prepared by Sol-gel methode with different ratio was added to the BaFeO₄ cathode in order to improve the discharge performance. The discharge capacity of the BaFeO₄ cathode was increased from 224 mAh·g^-1 to 246 mAh·g^-1 by addition of 5% nanometer SrTiO₃. The reason of enhancing BaFeO₄ electrochemical performance was discussed.     

PREPARATION AND CHARACTERIZATION OF SHISH-KEBAB TYPE LIQUID CRYSTALLINE POLY（p-PHENYLENEVINYLENE）

Novel shish-kebab type liquid crystalline poly（p-phenylenevinylene） derivatives were synthesized by Stille coupling reaction from 2,5-bis[（4-n-alkoxyl）benzoyloxy]1,4-dibromobenzene （monomer l） and 1,2-bis（tributylstannyl） ethylene （monomer 2）. The polymers with alkoxy groups are soluble in common organic solvents and exhibit blue fluorescence. Both the cast film and the annealed film have large red-shifts in fluorescence spectra and show yellow fluorescence. The polymers with CN and NO2 groups show poor solubility and green fluorescence. All the polymers possess liquid crystalline smectic phases. The melting point （Tm） of the polymers decreases when the length of the alkoxy tails of the mesogenic units increases. The polymers are easily aligned under a magnetic field of 10 Tesla. It is found that the conjugated backbone and LC side chain are aligned perpendicular and parallel to the magnetic field, respectively. The polymers show optical dichroism in fluorescence spectra, suggesting that they are available for advance materials with linear optical polarization.     

氟掺杂锐钛矿型TiO2溶胶的制备、表征及催化性能

以四氯化钛为前驱物, 采用改性的沉淀-溶胶-水热晶化法制备了一种具有锐钛矿型结构的氟掺杂的二氧化钛(F-TiO₂)溶胶. 研究了氟掺杂、水热晶化的温度、时间及介质pH值对溶胶粒子的晶型和晶化度的影响. 采用XRD, TG-DTA, TEM, UV-Vis-DRS, FTIR, XPS技术及吸附、表面酸度测定手段对溶胶粒子的结构进行了表征. XRD分析结果表明: 氟的掺入可以降低水热晶化反应的温度或减少反应时间、提高粒子的晶化度, 溶胶粒子具有锐钛矿型结构; TEM分析显示: 粒子呈圆球型, 平均粒径大约为6.5 nm. XPS测定结果表明; 氟在溶胶粒子中以吸附态和结合态两种形式存在; 吸附、表面酸度及光催化活性测定表明: 与P25型TiO₂及纯TiO₂溶胶粒子相比, F-TiO₂溶胶粒子具有更大的吸附能力、更强的表面酸度及更高的光催化活性. 还从光生载流子分离效率等方面探讨了掺杂对催化剂活性影响的机理.     

苯并三氮唑及其羧酸酯衍生物对铜缓蚀机理的分子动力学模拟研究

用分子动力学(MD)方法, 模拟计算了5种铜缓蚀剂[苯并三氮唑(BTA)、苯并三氮唑-5-羧酸甲酯(MBTC)、苯并三氮唑-5-羧酸丁酯(BBTC)、苯并三氮唑-5-羧酸己酯(HBTC)、苯并三氮唑-5-羧酸辛酯(OBTC)]与Cu₂O晶体的相互作用. 结果发现, 中性条件下缓蚀剂分子与Cu₂O晶体的结合能均大于酸性条件下的数值, 但两种条件下结合能的大小排序均为OBTC＞HBTC＞BBTC＞MBTC＞BTA. 对体系各种相互作用以及对关联函数g(r)的分析表明, 体系结合能主要由库仑作用提供, Cu₂O晶体中的Cu原子与缓蚀剂分子中的N原子之间形成了配位键. 在与Cu₂O(001)晶面结合过程中, BTA及其衍生物分子发生了扭曲变形, 但形变能远小于体系的非键相互作用能.