Nikola S. Vukelić

Effect of the support and the reduction temperature on the formation of metallic nickel phase in Ni/silica gel precursors of vegetable oil hydrogenation catalysts

Ni/SiO2 materials with identical composition (SiO2/Ni = 1.0) have been synthesized by precipitation of Ni(NO3)2 · 6H2O solution with Na2CO3 solution on the silica gel, obtained at three different pH values. The present investigation was undertaken in an endeavor to study the effects of the silica gel support type and the reduction temperature on the formation and dispersion of the metallic nickel phase in the reduced Ni/SiO2 precursors of the vegetable oil hydrogenation catalyst. The physicochemical characterization of the unreduced and reduced precursors has been accomplished appropriately by powder X-ray diffraction, infrared spectroscopy, temperature programmed reduction and H2-chemisorption techniques. It can be stated that the texture peculiarities of the silica gels used as supports influence on the crystalline state and distribution of the deposited Ni-containing phases during the preparation of the precursors, on the reduction temperature of the investigated solids as well as on the bulk size and surface dispersion of the arising metallic nickel particles. It was shown that two types of Ni2+-species are formed during the synthesis procedure, namely basic nickel carbonate-like and Ni-phyllosilicate with different extent of presence, location and strength of interaction. The different location of these species is supposed to result in various strength of Ni-O and Ni-O-Si interaction, thus determining the overall reducibility of the precursors. It was specified that the Ni2+-species are strongly bonded to the surface of the silica gel obtained at neutral pH value and weakly bonded to the surface of those prepared in acidic and alkaline conditions. It was established that the precursor, derivates from the silica gel obtained at alkaline conditions, demonstrates both significant reduction of the Ni2+ ions at 430°C and finely dispersed metallic nickel particles on its surface. High dispersion of the metallic nickel might be the crucial reason for achieving of high activity in the vegetable oil hydrogenation.

Effect of experimental variables onto Co(2+) and Sr(2+) sorption behavior in red mud-water suspensions.

ABSTRACT The prospects of rinsed red mud (alumina production residue) utilization for liquid radioactive waste treatment have been investigated, with Co2+ and Sr2+ as model cations of radioactive elements. To evaluate the sorption effectiveness and corresponding binding mechanisms, the process was analyzed in batch conditions, by varying experimental conditions (pH, Co2+ and Sr2+ concentrations in single solutions and binary mixtures, contact time, and the concentration of competing cations and ligands common in liquid radioactive waste). Comparison of the Co2+ and Sr2+ sorption pH edges with the red mud isoelectric point has revealed that Co2+ removal took place at both positive and negative red mud surface, while Sr2+ sorption abruptly increased when the surface became negatively charged. The increase of initial cation content and pH resulted in increased equilibrium times and sorption capacity and decreased rate constants. From single metal solutions and various binary mixtures, Co2+ was sorbed more efficiently and selectively than Sr2+. While Sr2+ sorption was reduced by coexisting cations in the order Al3+ ≥ Ca2+ >Na+ ≥Cs+, removal of Co2+ was affected by Al3+ species and complexing agents (EDTA and citrate). Desorption of Co2+ was negligible in Ca2+ and Sr2+ containing media and in solutions with initial pH 4–7. Sr2+ desorption was generally more pronounced, especially at low pH and in the presence of Co2+. Collected macroscopic data signify that Co2+ sorption by red mud minerals occurred via strong chemical bonds, while Sr2+ was retained mainly by weaker ion-exchange or electrostatic interactions. Results indicate that the rinsed red mud represent an efficient, low-cost sorbent for Co2+ and Sr2+ immobilization.

Concurrent Co2+ and Sr2+ sorption from binary mixtures using aluminum industry waste: Kinetic study

Multi-component sorption studies are essential to identify the applicability of red mud as a lowcost sorbent for the simultaneous removal of metal ions from wastewaters. Sorption kinetics of Co2+ and Sr2+ ions was investigated, at different total concentrations of mixtures and different molar ratios of two cations. Kinetics of metal sorption from binary systems was found to be well described by pseudo-second order rate model. Equilibrium sorbed amounts and equilibrium times for Co2+ sorption increased with the increase of its total concentration in the mixture, whereas pseudo-second order rate constants exhibited the opposite trend. Sr2+ sorption was strongly suppressed in the presence of Co2+ ions, and the removal efficiency decreased with increasing concentration and mole fraction of Co2+. Red mud can be used for simultaneous Co2+ and Sr2+ removal from mixtures of lower initial concentration, otherwise Co2+ sorption is dominant.

Methanol electrooxidation in alkaline solutions on platinum-based electrodes: Classical and dynamical approach

The electrochemical oxidation of methanol has been carefully studied due to its application in fuel cells. In this work electrooxidation of methanol was investigated on bare platinum electrode, the platinum electrode covered with Nafion and platinum supported on zeolite 13X. Along with classical electrochemical methods, attractor reconstruction was used to make rough distinction among possible reaction mechanisms on different forms of Pt. The obtained transient voltammogram records were used to calculate apparent rate constants for methanol oxidation limiting steps in transient period. All samples contributed to methanol oxidation by basically same reaction mechanism, but with significantly different apparent rate constants.

Perlite as a potential support for nickel catalyst in the process of sunflower oil hydrogenation

Investigation was conducted in order to elucidate the possibility of using perlite as support for preparation of nickel based precursor catalyst, potentially applicable in vegetable oil hydrogenation process. On three differently prepared expanded perlite, nickel catalyst precursors with identical Ni/SiO2 = 1.1 and Ni/Mg = 10/1 ratios were synthesized by precipitation-deposition method. Different techniques, SEM micrography, He-pycnometry, calcimetry, Hg-porosimetry, N2-physisorption, H2-chemisorption and temperature programmed reduction, were used for characterization of obtained samples. Determining the precursor texture, morphology and reducibility shows a successfully deposited nickel phase on perlite support with promising properties for vegetable oil hydrogenation. Chosen precursor was reduced and passivated in paraffin oil and the obtained catalyst showed significant catalytic activity in the test of sunflower oil hydrogenation.

Adsorption of Methylene Blue from Aqueous Solution onto Bentonite

Technological development brought a number of advantages and conveniences to the modern life, but also brought many problems, environment pollution above all. Although a number of methods for water refining are already developed, there is still a demand to find a more efficient, cheaper and ecologically more acceptable sorbents. Possibility of using bentonite as naturally occurring material for methylene blue (MB) removal from its aqueous solutions was investigated in this paper. Characterization of starting material has been conducted by chemical analysis, XRD, particle size analysis, and N2 physisorption at –196°C. The influence of the acidity of the initial MB solution on bentonite sorption characteristic was examined. Equilibrium sorption isotherms were determined. It was shown that with increase of pH and temperature the amount of sorbed MB increases.

Nickel/Silica Precursor from Sodium Silicate Solution - Synthesis and Characterization

The aim of this paper was the investigation of the influence of synthesis parameters, as well as the order of synthesis steps, in procedure of chemical precipitation, on the properties of synthesized nickel precursor. The starting materials were always the same aqueous solutions of Ni(NO3)2×6H2O and Mg(NO3)2×6H2O of constant molar ratio, 2% solution of SiO2 in the form of sodium silicate solution (module SiO2/Na2O = 3.0) and 10% solution of Na2CO3, while synthesis steps and addition modes were varied. Complete pH and temperature monitoring was performed during entire synthesis at 90°C. The formed precipitate aged 30 minutes at synthesis temperature. By changing the order and conditions of adding SiO2 and Na2CO3 solutions and keeping the treatment of precipitates the same (rinsing with hot distilled water followed by drying at 110°C for 24 hours) six different precursors were obtained. Samples characterizations were performed using different experimental techniques: XRD analysis, IR spectroscopy, reflection spectroscopy, TG analysis, N2 physisorption. The relation between synthesis procedure and precursor properties was established.

The influence of chemical oxidation and polishing on the surface and characteristics of a glassy carbon electrode

Abstract The effects of chemical oxidation and polishing on the condition of a glassy carbon surface have been investigated. The electrochemical characteristics of the laboratory-made glassy carbon electrode were examined and found to be satisfactory. Chemical oxidation with chromic acid led to a considerable decrease in the difference between the anodic and cathodic current-potential peaks (ΔEp), indicating increased reversibility of the electrode processes. Glassy carbon samples were treated in the same manner as the electrode by polishing and/or chemical oxidation with chromic acid, and the topography of the treated surfaces was examined by SEM. It was found that mechanical damage caused by abrasives plays a significant role in surface destruction by chromic acid.