A new method for the preparation of fullerol

Reaction of C-60 with excessive potassium in toluene at refluxing temperature results in black precipitate KaC60 with high conversion, which can completely be hydrolyzed to prepare the fullerol. Investigations including FT-IR. H-1 NMR C-13 NMR, UV-Vis and FABMS of the product were reported.

Hydroxylation of phenol by iron(II)-phenanthroline(Phen)/MCM-41 zeolite

MCM-41 zeolite and Tron (II)-Phen/MCM-41 zeolite have been prepared and characterized by XRD, IR, NH3-TPD, HET and UV-Vis. The Iron( II)-Phen/MCM-41 zeolite+30% H2O2 system is capable for catalyzing hydroxylation of phenol.

Electrochemical behavior of the molybdotungstate heteropoly complex with neodymium, K10H3[Nd(SiMo7W4O39)(2)]center dot xH(2)O in aqueous solution

The electrochemical behavior of the title compound (denoted Nd(SiMo7W4)(2)(13-)) in aqueous solution has been studied using cyclic voltammetry, sampled d.c. voltammetry, differential pulse voltammetry and bulk electrolysis with coulometry, The stable pH range of Nd(SiMo7W4)(2)(13-) is determined with UV-visible spectra. In the potential range between 0.70 and -0.45 V vs. SCE, the anion in pH 3.8 aqueous solution undergoes one-, one-, two- and two-electron steps of four redox processes attributed to electron addition and removal from the molybdate-oxo framework. The adsorption of the anion on the dropping mercury electrode and a self-inhibition influence of the adsorbed anions on the redox process of those anions dissolved in solution are found. The unusual dependence of the formal potentials on pH is explained with the competition of the protonation and ion-pair formation due to the high negative charge of Nd(SiMo7W4)(2)(13-) and its reduced forms. The electrocatalytic effects of the anion on the bromate are investigated.

Studies on preparation, characterization of cobalt(II) phenanthroline and 8-hydroxyquinoline complexes/Y zeolite, and catalytic hydroxylation of phenol

Cobalt(II) phenanthroline and 8-hydroxyquinoline complexes/Y zeolite, denoted as CoPhen/Y and CoOx/Y respectively, were prepared, The formation of the metal complexes mentioned above within the cages of Y zeolite and their crystal structures were determined by elementary analyses, TG-DTA, diffuse reflectance UV-Vis, SEM, BET and XRD methods. The influence of experimental parameters upon phenol conversion and product selectivities was investigated as well.

Hydroxylation of phenol by iron(II)-phenanthroline(Phen) MCM-41 zeolite

MCM-41 mesoporous molecular sieve and iron(II)-Phen/MCM-41 have been prepared and characterized by XRD, IR, NH3-TPD, BET and UV-Vis. The iron(II)-Phen/MCM-41 molecular sieve + 30% H2O2 system is capable of performing hydroxylation of phenol.

铁邻菲咯啉、8-羟基喹啉配合物/Y型分子筛的制备、表征及催化苯酚羟化的研究

制备了铁邻菲咯啉、8-羟基喹啉配合物/Y型分子筛(简记为FePhen/Y,FeO_x/Y).用元素分析,TG-DTA,UV-Vis,IR,SEM,BET,及XRD等方法确定了分子筛笼中金属配合物的生成及其晶体结构,考察了实验参数对苯酚转化率及产物选择性的影响.

STUDIES ON PREPARATION OF IRON, COBALT AND COPPER PHTHALOCYANINES Y ZEOLITE - CHARACTERIZATION AND THEIR CATALYSIS FOR HYDROXYLATION OF PHENOL

Iron, cobalt and copper phthalocyanines/Y zeolite, denoted as FePcY, CoPcY and CuPcY respectively,were prepared. The formation of metal phthalocyanine compounds within the cages of Y zeolite and their crystal structures were determined by elementary analyses, IR, UV-Vis, TG, BET, and XRD methods; The influence of experimental parameters upon phenol conversion and product selectivities was investigated as well.

AN INTEGRATED CALCIUM-FLUORIDE CRYSTAL IR THIN-LAYER CELL AND ITS APPLICATION TO IDENTIFICATION OF ELECTROCHEMICAL REDUCTION PRODUCT OF BILIRUBIN

An integrated CaF2 crystal optically transparent infrared (ir) thin-layer cell was designed and constructed without using any soluble adhesive materials. It is suitable for both aqueous and nonaqueous systems, and can be used not only in ir but also in uv-vis studies. Excellent electrochemical and spectroelectrochemical responses were obtained in evaluating this cell by cyclic voltammetry and steady-state potential step measurements for both ir and uv-vis spectrolectrochemistry with ferri/ferrocyanide in aqueous solution, and with ferrocene/ferrocenium in organic solvent as the testing species, respectively. The newly designed ir cell was applied to investigate the electrochemical reduction process of bilirubin in situ, which provided direct information for identifying the structure of the reduction product and proposing the reaction mechanism.

Characterization of 1:12 Phosphomolybdic Anions Doped Polypyrrole (PMo12/PPy) Film Electrode

1:12 phosphomolybdic anion doped polypyrrole film electrode was characterized by in-situ UV-vis spectroelectrochemistry, X-ray photoelectron spectroscopy(XPS), scan electronic microscopy(SEM) and electron spin resonance(ESR) spectroscopy.

CUPRIC HEXACYANOFERRATE COLLOID DOPED POLYPYRROLE FILM-MODIFIED ELECTRODE

Anionic colloid cupric hexacyanoferrate (CuHCF) was incorporated into polypyrrole (PPy) films in the course of electrochemical polymerization of pyrrole from aqueous solution containing pyrrole and CuHCF colloid. The films obtained were dark brown in color. Three redox peaks appeared in the cyclic voltammogram (CV). The peaks around 0.7 V (vs, SCE) showed cation-selective properties. X-ray photoelectron spectroscopic analysis and ultraviolet-visible (UV-vis) spectroscopic properties of the film were investigated.

INDIGO-CARMINE-MODIFIED POLYPYRROLE FILM ELECTRODE

Functionalized polypyrrole films were prepared electrochemically in the presence of indigo-carmine from aqueous solution. The film shows a couple of reversible redox peaks superimposed on a large background of polypyrrole. The redox reaction is pH dependent. The film has good stability in air and can be cycled between -0.1 and 0.4 V (Ag/AgCl) for several hours without any significant changes in the voltammograms. UV-visible spectra indicate the incorporation of indigo-carmine into the polymer matrix.

5,10,15,20-四(对-乙酯苯基)卟啉LB膜的结构

对卟啉类化合物LB膜的结构、电性质和气敏性的研究已见报道。本文利用膜天平和UV-Vis分光光度计研究了标题化合物在气-液界面上的成膜特性、分子间相互作用和LB膜的结构。5,10,15,20-四(对-乙酯苯基)卟啉(TPEPP)由5,10,15,20-四(对-氰苯基)卟啉和乙醇酯化得到。元素分析测定值与计算值相符。λ(CHCl_3,nm):421,515,550,590,645;ν(KBr压

固载化金属酞菁(MPc)催化性能的研究——Ⅱ.MPc通过配位连接在硅胶上及其对O_2的活化作用

用有机合成的方法在硅胶表面连接上可与MPc配位的有机基团——(CH_2)_3N(C_2H_5)_2,MPc与之配位从而固载在硅胶上。UV-Vis漫反射光谱表明硅胶表面存在MPc。用ESR研究固载化MPc与O_2的作用,证明固载化CoPc、FePc可以与O_2作用产生O_2~-,CuPc则不能。

新型可溶性酞菁铜(Ⅱ)衍生物的合成、结构及其成膜性

合成了两个新型取代酞菁铜(Ⅱ)衍生物:四-4-(2-甲氧基乙氧基-羰基)酞菁铜(Ⅱ)(A)和四-4-(2-正丁氧基乙氧基-羰基)酞菁铜(Ⅱ)(B),以元素分析、ESR、~1H NMR和FT-IR进行了表征。UV-vis光谱表明它们在氯仿溶液(10~(-5)～10(-6)mol/L)中主要以双分子缔合形式存在;X-射线粉末衍射表明配合物的分子以倾斜的方式相互平行排列;热重分析表明酞菁环引入有机基团后其热稳定性略有下降,且取代基越长,热稳定性越差。两个配合物的氯仿溶液在亚相(水)上的π-A曲线表明,它们均有明显的“气”液”“固”的变化过程,并能形成较好的单分子层膜。

LIGHT-ASSISTED OXIDATIVE DOPING OF POLYANILINES

A novel doping phenomenon of fully reduced polyaniline and poly-o-methyl-aniline, "light-assisted oxidative doping", was found for the first time. The doping reaction was followed by FTIR, UV-VIS, ESR and electrical conductivity measurements. It was shown that the fully reduced polyanilines in the form of HCl-salts undergo a spontaneous transition from an insulator or semiconductor to a conductor when exposed to air and light, and their final molecular chain structures are analogous to those found in HCl-doped common polyanilines.