Synthesis of metal oxide nanorods using carbon nanotubes as templates

Nanorods of several oxides, with diameters in the range of 10-200 nm and lengths upto a few microns, have been prepared by templating against carbon nanotubes. The oxides include V2O5, WO3, MoO3 and Sb2O5 as well as metallic MoO2, RuO2 and IrO2. The nanorods tend to be single-crystalline structures. Nanotube structures have also been obtained in MoO3 and RuO2.

Solution cation-binding properties of segmented polyethylene oxide-A C-13 NMR spectroscopic study

Two segmented polyethylene oxides, SPEO-3 and SPEO-4, were prepared using a novel transetherification methodology. Their structures were confirmed by H-1 and C-13 NMR spectroscopy. The complexation of these SPEO's with alkali-metal ions in solution was investigated by C-13 NMR spectroscopy. The mole-fraction method was used to determine the complexation ratio of SPEO with LIClO4 at 25 degrees C, which showed that these formed 1:1 (polymer repeat unit/salt) complexes. The association constant, K, for the complex formation was calculated from the variation of the chemical shift values with salt concentration, using a standard nonlinear least-square fitting procedure. The maximum change in chemical shift (Delta delta) and the K values suggest that both SPEO-3 and SPEO-4 formed stronger complexes with lithium salts than with sodium salts. Unexpectedly, the K values were found to be different, when the variation of delta of different carbons was used in the fitting procedure. This suggests that several possible complexed species may be in equilibrium with the uncomplexed one. Structurally similar model compounds were also prepared and their complexation studies indicated that all of them also formed 1:1 complexes with Li salts. Interestingly, it was observed that the polymers gave higher K values suggesting the formation of more stable complexes in polymers when compared to the model analogues. (C) 2000 John Wiley & Sons, Inc.

Selective para metalation of unprotected 3-methoxy and 3,5-dimethoxy benzoic acids with n-butyl lithium-potassium tert-butoxide (LIC-KOR): synthesis of 3,5-dimethoxy-4-methyl benzoic acid

The potassium salt of 3-methoxy and 3,5-dimethoxy benzoic acids undergoes deprotonation at the position para to the carboxylate group selectively when treated with LIC-KOR in THF at -78 degrees C and it has been extended to the synthesis of 3,5-dimethoxy-4-methyl benzoic acid. (C) 2000 Elsevier Science Ltd. All rights reserved.

Effect of Nanostructuring and Ex situ Amorphous Carbon Coverage on the Lithium Storage and Insertion Kinetics in Anatase Titania

Implications of nanostructuring and conductive carbon interface on lithium insertion/removal capacity and insertion kinetics innanoparticles of anatase polymorph of titania is discussed here.Sol-gel synthesized nanoparticles of titania (particle size similar to 6 nm) were hydrothermally coated ex situ with a thin layer of amorphous carbon (layer thickness: 2-5 nm) and calcined at a temperature much higher than the sol-gel synthesis temperature. The carbon-titania composite particles (resulting size similar to 10 nm) displayed immensely superior cyclability and rate capability (higher current rates similar to 4 g(-1)) compared to unmodified calcined anatase titania. The conductive carbon interface around titania nanocrystal enhances the electronic conductivity and inhibits crystallite growth during electrochemical insertion/removal thus preventing detrimental kinetic effects observed in case of unmodified anatase titania. The carbon coating of the nanoparticles also stabilized the titania crystallographic structure via reduction in the accessibility of lithium ions to the trapping sites. This resulted in a decrease in the irreversible capacity observed in the case of nanoparticles without any carbon coating.

Quinone studies. Part III. Metal ion-catalysed oxidation of halophenols and halonaphthols by peroxidisulphate

Oxidation of representative halophenols and halonaphthols by peroxidisulphate has been examined. The influence of metallic ions, viz. Cu2+, Fe3+, Ag+, on the above reaction has been studied. Cu2+ ion-catalyzed oxidation gives halo-1, 4-quinones in excellent yield. Potassium bis(biureto)cuprate(III) complex also oxidises halophenols to halo-1, 4-quinones.

Oxide-based bifunctional oxygen electrode for rechargeable metal/air batteries

Statistical methods for optimizing the morphology of oxide-based, bifunctional oxygen electrodes for use in rechargeable metal/air batteries are examined with regard to binder composition, compaction time, and compaction load. Results show that LaNiO3 with PTFE binder in a nickel mesh envelope provides a satisfactory electrode.

Attaching chelating ligands to polybenzimidazole via epoxidation to obtain metal selective sorbents

Microporous polybenzimidazole of 250–500 μm spherical bead size from Celanese has been reacted with epichlorohydrin and sodium hydroxide and the resulting product with pendant epoxy groups has been reacted with various chelating ligands in order to augment the metal sorption capacity and selectivity of the resin. The chelating ligands used include ethylenediamine, diethylenetriamine, diethanolamine, dimethylglyoxime, L-cysteine, thiourea, dithiooxamide, glyoxal-bis-2-hydroxyanil, salicylaldehyde-ethylenediimine, and glyoxal-bis-2-mercaptoanil. The aminolysis of the pendant epoxy groups with the oligoamines has been performed in pyridine under reflux conditions, while the addition reactions with the other ligands which are alkali soluble have been carried out at room temperature in a mixture of dioxane and aqueous KOH using tetra-n-butylammonium iodide as the phase transfer catalyst. The products are found to possess high capacity and selectivity in metal sorption depending on the ligand attached.

Crystal structure of 2-thiophene-2-yl-3(thiophene-2-carboxylideneamino)-1,2-dihydroquinazolin-4(3H)-one and the synthesis, spectral and thermal studies of its transition metal(II) complexes

The synthesis of manganese(II), cobalt(II), nickel(II), copper(II), zinc(II) and cadmium(II) complexes of a new ligand 2-thiophene-2-yl-3(thiophene-2-carboxylidene-amino)-1,2-dihydroquinazolin-4(3H)-one (TTCADQ) is described. The ligand and metal complexes were characterized by elemental analysis, conductivity measurements, spectral (u.v.-vis., i.r., 1D n.m.r., 2D hetcor and e.p.r.) and thermal studies. The formation of 1,2-dihydroquinazolin-4(3H)-one rather than hydrazone, in the reaction of aromatic aldehyde and o-aminobenzoylhydrazide is proved by single crystal X-ray diffraction and 2D hetcor n.m.r. studies. On the basis of elemental analysis, u.v.-vis.spectroscopy and magnetic moment studies, six coordinate geometry for all the complexes was proposed. The i.r. spectral studies reveal the bidentate behaviour of the ligand.

Towards a green synthesis of LAB's: Effect of rare earth metal ions on the benzene alkylation with 1-dodecene over NaFAU-Y zeolites

Chemically modified microporous materials can be prepared as robust catalysts suitable for application in vapor phase processes such as Friedel-Crafts alkylation. In the present paper we have investigated the use of rare earth metal (Ce3+, La3+, RE3+, and Sm3+) exchanged Na-Y zeolites as catalysts for the alkylation of benzene with long chain linear 1-olefin; 1-dodecene. Thermodesorption studies of 2,6-dimethylpyridine adsorbed catalysts (in the temperature range 573 to 873 K) show that the rare earth zeolites are highly Bronsted acidic in nature. A perfect correlation between catalyst selectivity towards the desired product (2-phenyldodecane) and Bronsted acid sites amount has been observed. (c) 2006 Springer Science + Business Media, Inc.

Studies on removal of metal ions and sulphate reduction using rice husk and Desulfotomaculum nigrificans with reference to remediation of acid mine drainage

The utility of rice husk as an adsorbent for metal ions such as iron, zinc and copper from acid mine water was assessed. The adsorption isotherms exhibited Langmuirian behavior and were endothermic in nature. The free energy values for adsorption of the chosen metal ions onto rice husk were found to be highly negative attesting to favorable interaction. Over 99% Fe3+, 98% of Fe2+ and Zn2+ and 95% Cu2+ uptake was achieved from acid mine water, with a concomitant increase in the pH value by two units using rice husk. The remediation studies carried out on acid mine water and simulated acid mine water pretreated with rice husk indicated successful growth of Desulfotomaculum nigrificans (D. nigrificans). The amount of sulphate bioreduction in acid mine water at an initial pH of 5.3 was enhanced by D. nigrificans from 21% to 40% in the presence of rice husk filtrate supplemented with carbon and nitrogen. In simulated acid mine water with fortified husk filtrate, the sulphate reduction was even more extensive, with an enhancement to 73%. Concurrently, almost 90% Fe2+, 89% Zn2+ and 75% Cu2+ bioremoval was attained from simulated acid mine water. Metal adsorption by rice husk was confirmed in desorption experiments in which almost complete removal of metal ions from the rice husk was achieved after two elutions using 1 M HCl. The possible mechanisms of metal ion adsorption onto rice husk and sulphate reduction using D. nigrificans are discussed.

A building-up process in open-framework metal carboxylates that involves a progressive increase in dimensionality

Extensive research work has been carried out in the last few years on the synthesis and characterization of several families of open-framework materials, including aluminosilicates,[1] phosphates,[2] and carboxylates.[3] These studies have shown the occurrence of a variety of three dimensional (3D) architectures containing channels and other features.

A Novel Synthetic Route For The Preparation Of Ammonium And Alkali-Metal Tetrafluoroborates And Alkyl Substituted Ammonium Tetrafluoroborates Using Pyridinium Tetrafluoroborate As The Precursor

Ammonium and alkali metal tetrafluoroborates have been prepared by the cation exchange reaction of pyridinium tetrafluoroborate with the corresponding hydroxides/halides. The reaction of pyridinium tetrafluoroborate with primary, secondary and tertiary alkyl amines at room temperature gives rise to mono-, di- and tri-alkylammonium tetrafluoroborates, respectively. The yields are good and the samples are of high purity. The products have been characterised by elemental analysis, IR and PMR spectroscopy. The spectral data for most of the compounds are reported for the first time.