氢键构筑的新颖微孔配位聚合物[Co2(Hisor)2·(4,4′-bpy)2(H2O)2]·4,4′-bpy的合成与结构

A novel microporous coordination polymer [Co2(Hisor)2(4,4′-bpy)2(H2O)2]·4,4′-bpy was synthesized by hydrothermal reaction and characterized by single crystal X-ray diffraction, elemental analysis and IR spectrum. The crystal belongs to the monoclinic system and space group is P2/n with a=1.040 6(3) nm, b=1.138 8(4) nm, c=1.854 7(6) nm, β=102.991(6)°, V= 2.141 6(12) nm3, Z=2, Dc=1.443 Mg/m3, Mr=930.62, μ=0.842 mm-1, F(000)=952, GOF= 1.072, R=0.065 4, wR=0.146 8[I>2σ(I)]. There are two crystallographically independent Co(Ⅱ) ions in the title complex. The Hisor2- and 4,4′-bpy link the metal ions into 2D grids with dimension of 0.522 3 nm×1.138 8 nm. There are O—H…O and N—H…O hydrogen bonds in the complex resulting in the formation of 3D network with 1D channels, in which are free 4,4′-bpy molecules.     

Carbon-Supported Silver Catalysts for CO Selective Oxidation in Excess Hydrogen

Carbon materials were used as supports for Ag catalysts that are prepared using the conventional wet impregnation method, and their catalytic properties for CO selective oxidation in excess hydrogen at temperatures below 483 K were tested. A variety of techniques, e.g. N2 adsorption, XPS, TPD, UV-Vis DRS, TEM and SEM, were used to determine the influence of physical and chemical properties of the carbon on the properties of Ag catalyst. It was found that defects on the carbon surface served as nucleation sites for silver ions, while functional groups on carbon surface induced their reduction to the metallic form. The formation of silver particles on carbon was governed by homogeneous and/or heterogeneous nucleation during the impregnation and subsequent activation processes. The best catalytic performance was obtained with a Ag/carbon black catalyst with a uniform size distribution of silver nanoparticles (about 12 nm), moderate BET surface area (with a mesoporous structure), and a limited amount of carbon-oxygen groups. The research indicates that carbon materials are potentially good supports for silver catalysts for preferential oxidation of CO in excess hydrogen.     

连接基团链长度对季铵盐二聚表面活性剂C12-s-C12·2Br在水溶液中胶团化行为的影响

用电导法、稳态荧光法和粘度法研究了二聚表面活性剂C12-s-C12*2Br分子中的连接基团链长度(s=2, 3, 4, 6)对其在水溶液中聚集行为的影响. 实验发现, C12-s-C12*2Br的胶团生成能力远比其单体C12TABr强得多, 前者cmc值较后者降低一个数量级. 胶团聚集数N随表面活性剂浓度c的增大而增大, 其中当s=2时的N值在c=7.7 mmol/L后开始急剧增大. 计算结果表明, 此时胶团形状发生了明显变化, 形成了椭球形的胶团. 粘度测定结果也证实了这一点.     

The Synthesis of Bis（carboxyalkylmethyl） Diselenides by Selenium Transfer Reaction of Aryl Selenoamides

Aryl selenoamides react smoothly with a-haloacetic acid in various alcohol to givecorresponding bis(carboxyalkylmethyl) diselenides in good yields.     

邻羧基苯甲醛苯甲酰腙稀土配合物的合成和抗氧化活性

通过邻羧基苯甲醛与苯甲酰肼在苯中的缩合反应制备了邻羧基苯甲醛苯甲酰腙 (H2 L)。在水中合成了H2 L的 6种稀土配合物 ,并采用元素分析IR ,UV ,1 HNMR和DTA TG对配合物进行了表征。配合物的分子式为RE(HL2 )·4H2 O (RE =La ,Pr,Nd ,Eu ,Gd和Er) ,配体以四齿参与配位 ,配合物是八配位结构。此外用紫外光谱法测定了配合物对O2 -·自由基的清除率。结果表明邻羧基苯甲醛苯甲酰腙稀土配合物有一定的抗氧化活性 ,对O2 -·自由基的清除率在 8%～ 2 5 %范围内     

功能化磁性微粒的合成与表征

以3 氨丙基三甲氧基硅烷与Fe3O4纳米粒子反应,制备了超顺磁性、表面修饰—NH2的功能化磁性微粒,带有氨基的磁性微粒进一步与戊二酸酐反应,可转化为—COOH修饰的功能化磁性微粒.利用X射线衍射、红外光谱、激光粒度散射仪等对磁性Fe3O4粒子以及两种功能化磁性微粒进行定性表征,建立了线性电位滴定和电导滴定的方法分别对磁性复合微粒表面—NH2和—COOH的量进行定量分析.结果表明,功能化磁性复合微粒的平均粒径为3～5μm,红外光谱分析结果中显示了功能基团—NH2和—COOH的特征峰谱,线性电位滴定测定功能化磁性微粒—NH2含量为400±50μmol/g,电导滴定法测定—COOH含量为380±50μmol/g.     

萘的六氮取代衍生物电子结构和非线性光学性质

在量子化学半经验PM3方法优化几何结构的基础上，采用FF／PM3方法，讨论了萘的六氮取代物及其对位被推、拉电子基团取代衍生物电子结构和非线性光学性质的变化．用NDDO方法计算体系的电子光谱，探讨了分子电子结构对电子光谱及非线性光学性质影响的微观本质．     

紫外辐照官能化LLDPE对PA66/LLDPE体系相容性改善的研究

在空气中 ,线型低密度聚乙烯 (LLDPE)通过紫外光辐照后氧以C =O、C -O、OH等基团形式被引入到分子链上。采用FT -IR、凝胶测定、MFR测定和水的接触角测定等方法研究了空气中紫外辐照对LLDPE化学结构和性能的影响。结果表明 :LLDPE分子链上含氧基团的引入量随辐照时间延长而增加 ,其膜的亲水性也相应增强。同时用SEM、Molau实验和力学性能测试等方法研究了官能化的LLDPE对PA6 6 /LLDPE共混体系的界面作用和相容性的影响。结果表明 :共混物体系微相之间的界面作用增强 ,两相的相容性得到明显改善 ,共混体系的力学性能有较大幅度的提高     

新试剂2—羧基—4—硝基苯基重氮氨基偶氮苯的合成及其与镉显色反应的研究

本文报道了新三氮烯试剂２－羧基－４－硝基苯基重氮基偶氮苯的合成及其与镉的显色反应．在非离子表面活性剂ＴｒｉｔｏｎＸ—１００存在下．于ｐＨ１１．０的Ｎａ４Ｂ４ｏ３－ＮａＯＨ缓冲介质中．试剂可与镉生成２：１的红色配合物，其配台物的最大吸收波长位于５２０ｎｍ处，表观摩尔吸光系数ε为１．５６６×ｘ１０５Ｌ·ｍｏｌ－１．ｃｍ－１，镉量在０—１０μｇ／２５ｍｌ范围内符台比尔定律，方法用于标准水样及铝合金标样中微量用的测定，结果满意．     

长毛对虾碱性磷酸酶功能基团的研究

用对－氯汞苯甲酸修饰该酶分子中的巯基，酶活力不受影响，说明该酶不是“巯基酶”．用Ｎ溴代琥珀酰亚胺修饰酶后，活力完全丧失，修饰后的酶在２７５ｎｍ处的紫外吸收峰完全消失，３４０ｎｍ处荧光发射峰也逐渐下降至完全淬灭，说明色氨酸残基是酶活性必需基因之一．用甲醛、醋酸酐修饰氨基，溴代乙酸修饰咪唑基也可以使酶活力完全丧失，说明赖氨酸残基及组氨酸残基也是酶活性功能基因．用乙酰丙酮修饰精氨酸残基，酶活力下降了５０％，精氨酸残基可能与维系酶分子构象有关．