CHARACTERIZATION OF A POTASSIUM-PROMOTED COBALT MOLYBDENUM ALUMINA WATER-GAS SHIFT CATALYST

A series of potassium-promoted CoMo/Al2O3 has been investigated by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and temperature-programmed reduction (TPR). CoMoO4 was found in the CoMo/Al2O3 catalyst by XRD and is destroyed by the presence of potassium. The reducibility of molybdenum is enhanced by potassium in the CoMoK/Al2O3 catalyst and is easier to reduce to Mo(IV) during sulfidation. In the oxidic state catalyst cobalt is increased on the surface by the addition of potassium. After sulfidation this phenomena disappeared, the distribution of cobalt remains at a constant level and is unaffected by the potassium content. The addition of potassium leads to a monotonical decrease of the molybdenum dispersion with the impregnating amount of potassium in the oxidic state catalyst but is more complicated after sulfidation. Potassium is well dispersed on the surface in both the oxidic and sulfided state. The activity in the water-gas shift reaction was correlated with the potassium content of CoMoK/Al2O3.

A GLASSY-CARBON ELECTRODE MODIFIED BY DISPERSED ALPHA-ALUMINA AS AN ENHANCED ELECTROCHEMICAL DETECTOR IN LIQUID-CHROMATOGRAPHY FOR CYSTEINE AND GLUTATHIONE

The dispersion of alumina particles on a glassy-carbon surface serving as a modified electrode significantly enhances the amperometric detection of cysteine and glutathione following liquid chromatography. With an applied potential of 0.8 V vs. SCE, the detection limits were 1.2 ng for cysteine and 8 ng for glutathione and the electrode response was linear up to 600 ng for cysteine and 1.8-mu-g for glutathione. The modified electrode displayed high sensitivity and stability and was easy and inexpensive to prepare.

Thioreduction of cyclopentanone and hydrodesulfurization of dibenzothiophene over sulfided nickel or cobalt-promoted molybdenum on alumina catalysts

Two series of sulfided Ni or Co promoted Mo/alumina catalysts, having different Ni or Co loadings, were characterized by their activities for the transformation of cyclopentanone into cyclopentanethiol (flow reactor, 220 degrees C, atmospheric pressure) and for the hydrodesulfurization of dibenzothiophene (flow reactor, 340 degrees C, 3 MPa hydrogen pressure). The addition of the promoter increased significantly the activity of the Mo/alumina catalyst for both reactions, up to a maximum obtained with the catalysts having a (promoter)/(promoter+Mo) molar ratio equal to 0.3-0.4. This increase in activity was due in part to an increase in the hydrogenating properties of the Mo/alumina catalyst. However, an additional modification of the catalyst (basic and nucleophilic properties) must be considered to account for the spectacular effect of the promoter on the rate of the dibenzothiophene direct desulfurization reaction. (C) 1999 Elsevier Science B.V. All rights reserved.

A novel method to synthesize amorphous silica-alumina materials with mesoporous distribution without using templates and pore-regulating agents

In this study, a novel sol-gel method is used to synthesize amorphous silica-alumina materials with a narrow mesoporous distribution and various Si/Al molar ratios without using any templates and pore-regulating agents. During the preparation procedure, only inexpensive inorganic salts were used as raw materials, instead of expensive and harmful alkoxides. The precursor sol was dried at room temperature in a vacuum box kept at 60 mmHg until it began to form the gel. The results of a nitrogen sorption experiment indicate that the synthesized materials with different Si/Al molar ratios have similar mesoporous distributions (within 2-12 nm). Moreover, it was found that the material's pore size distribution remains at a similar value during the heat treatment from room temperature to 550 degreesC. On the basis of the nitrogen sorption, TEM, and AFM characterization results, a formation mechanism of mesopores which accounts for the experimental data is also suggested. This suggested mechanism involves rearrangement of the primary particles during the drying process to form the precursors of the similarly sized mesopores. The synthesized materials were characterized by XRD, thermal analysis (TG/DTA), Al-27 and Si-29 MAS NMR spectroscopy, SEM, TEM, and AFM. The results of Al-27 and 29Si MAS NMR indicate that the distribution of silicon and aluminum in the synthesized materials is more uniform and homogeneous than that in the mixed oxides prepared via the traditional sol-gel method even at high alumina contents. The type and density of the acid sites were studied using pyridine adsorption-desorption FTIR spectroscopy. It was shown that the acidity of the synthesized materials is higher than that of the silica-alumina materials prepared by conventional methods.

Ultrasonic synthesis of silica-alumina nanomaterials with controlled mesopore distribution without using surfactants

A novel sol-gel process has been developed for the synthesis of amorphous silica-aluminas with controlled mesopore distribution without the use of organic templating agents, e.g., surfactant molecules. Ultrasonic treatment during the synthesis enables production of precursor sols with narrow particle size distribution. Atomic force microscopy analysis shows that these sol particles are spherical in shape with a narrow size distribution (i.e., 13-25 nm) and their aggregation during the gelation creates clusters containing similar sized interparticle mesopores. A nitrogen physiadsorption study indicates that the mesoporous materials containing different Si/Al ratios prepared by the new synthesis method has a large specific surface area (i.e., 587-692 m(2)/g) and similar pore sizes of 2-11 nm. Solid-state Al-27 magic angle spinning (MAS) NMR shows that most of the aluminum is located in the tetrahedral position. A transmission electron microscopy (TEM) image shows that the mesoporous silica-alumina consists of 12-25 nm spheres. Additionally, high-resolution TEM and electron diffraction indicate that some nanoparticles are characteristic of a crystal, although X-ray diffraction and Si-29 MAS NMR analysis show an amorphous material.