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See detailSynthesis of transition metal-doped carbon xerogels by cogelation
Job, Nathalie ULg; Pirard, René ULg; Vertruyen, Bénédicte ULg et al

in Journal of Non-Crystalline Solids (2007), 353(24-25), 2333-2345

The cogelation process, i.e. the co-polymerization of a metal complex with the gel precursors, was used for the synthesis of transition metal-doped resorcinol-formaldehyde gels. The aim of this process is ... [more ▼]

The cogelation process, i.e. the co-polymerization of a metal complex with the gel precursors, was used for the synthesis of transition metal-doped resorcinol-formaldehyde gels. The aim of this process is to anchor the metal to the polymer so that the former does not sinter during the pyrolysis step leading to porous carbon. Cu-, Ni-, Pd- or Pt-loaded gels were prepared by this technique. After drying and pyrolysis, Pd and Pt were obtained as metal nanoparticles (2-5 nm in diameter) inserted in the carbon nodules, when the complexing agent and the synthesis conditions were well chosen. These small metal particles were inaccessible to reactive gases, probably due to carbon deposit at the metal surface during pyrolysis: CO almost did not chemisorb. Oxidation of the support or pyrolysis under reductive atmosphere was applied to the metal-doped gels and carbons in order to make the surface of the metal particles accessible, but these treatments develop the macropores only. The cogelation process is then suitable to prepare metal nanoparticles protected from the outside by encapsulation in the carbon matrix. (C) 2007 Elsevier B.V. All rights reserved. [less ▲]

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See detailSynthesis optimization of organic xerogels produced from convective air-drying of resorcinol-formaldehyde gels
Job, Nathalie ULg; Panariello, Fabian; Marien, José ULg et al

in Journal of Non-Crystalline Solids (2006), 352(1), 24-34

Resorcinol-formaldehyde gels were produced at 50, 70 and 90 degrees C and with three different R/C ratios (500, 1000 and 2000). The effect of these variables combined with that of aging time was studied ... [more ▼]

Resorcinol-formaldehyde gels were produced at 50, 70 and 90 degrees C and with three different R/C ratios (500, 1000 and 2000). The effect of these variables combined with that of aging time was studied in order to optimize the synthesis conditions. The convective air-drying process was used, and the drying duration was studied with regard to the synthesis conditions. The aging time has no effect on the pore texture after 24 h at 90 degrees C or 48 h at 70 C, whatever the R/C value. The synthesis-aging step can be shortened by increasing the temperature. Nevertheless, the pore size tends then to decrease, especially when R/C is high, but this can be counterbalanced by increasing R/C. Moreover, bubbles often appear in the gel at high synthesis temperature, which limits the temperature to about 70 degrees C in the case of monolithic parts. At 70 degrees C and with an air velocity of 2 m/s, the elimination of 90% of the solvent requires 1 h drying when the pore size reaches 400-600 nm, 2.5 h for 50 nm wide pores and 3 h when the pore size decreases to 15-20 nm. The drying duration does not exceed 8 h in all cases and could be shortened by increasing the temperature at the end of the process. (c) 2005 Elsevier B.V. All rights reserved. [less ▲]

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See detailMetal catalysts suppported on texture-tailored carbon xerogels
Job, Nathalie ULg; Léonard, Angélique ULg; Colomer, Jean-François et al

in Studies in Surface Science and Catalysis (2006), 162

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See detailHighly dispersed platinum catalysts prepared by impregnation of texture-tailored carbon xerogels
Job, Nathalie ULg; Ribeiro Pereira, Manuel Fernando; Lambert, Stéphanie ULg et al

in Journal of Catalysis (2006), 240(2), 160-171

Pt/C catalysts were prepared by impregnation of carbon xerogels with H2PtCl6 aqueous solutions. Three supports with various pore textures were used: two micro-mesoporous (maximum pore size = 10 and 40 nm ... [more ▼]

Pt/C catalysts were prepared by impregnation of carbon xerogels with H2PtCl6 aqueous solutions. Three supports with various pore textures were used: two micro-mesoporous (maximum pore size = 10 and 40 nm, respectively) and one micro-macroporous (maximum pore size = 70 nm). After impregnation, drying and reduction, the metal particles were at most 1-1.5 nm in diameter. The Pt dispersion was close to 100% in the case of the xerogel with large mesopores. For the two other supports, a small fraction of Pt was trapped in blocked micropores. The specific catalytic activity obtained for benzene hydrogenation was 4-10 times higher than that obtained with active charcoal-supported catalysts prepared by a similar method. The high dispersion of Pt was attributed to the presence in the xerogel of large mesopore or macropore volumes, which facilitates impregnation, and a low amount of oxygenated surface groups. (c) 2006 Elsevier Inc. All rights reserved. [less ▲]

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See detailCarbon xerogels as catalyst supports: study of mass transfer
Job, Nathalie ULg; Heinrichs, Benoît ULg; Lambert, Stéphanie ULg et al

in AIChE Journal (2006), 52

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See detailHydrodechlorination of 1,2-dichloroethane on Pd-Ag catalysts supported on tailored texture carbon xerogels
Job, Nathalie ULg; Heinrichs, Benoît ULg; Ferauche, Fabrice et al

in Catalysis Today (2005), 102

Porous carbon xerogels synthesized in a previous study were investigated as catalysts supports. The support chosen was a micro-mesoporous carbon xerogel obtained from the pyrolysis of a resorcinol ... [more ▼]

Porous carbon xerogels synthesized in a previous study were investigated as catalysts supports. The support chosen was a micro-mesoporous carbon xerogel obtained from the pyrolysis of a resorcinol-formaldehyde resin whose synthesis variables were fixed at suitable values. Palladium and silver were deposited on this tailored texture carbon by co-impregnation using a solution of palladium and silver nitrates in nitric acid and water. Several catalysts were prepared with various Pd and Ag global contents, the latters being measured experimentally. Alloy particles, detected in all bimetallic samples, were studied by a combination of various techniques that enabled us to obtain their size as well as their bulk and surface composition. When present, the fraction of unalloyed silver was also calculated. The characterization data were related to the results of catalytic tests obtained for selective hydrodechlorination of 1,2-dichloroethane into ethylene. Results show that when the Ag content is too high, pure Ag particles are formed and the alloy composition remains constant. As a consequence, the surface composition of the alloy is constant as well and the catalytic tests lead to similar results. (c) 2005 Elsevier B.V. All rights reserved. [less ▲]

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See detailCarbon aerogels, cryogels and xerogels: Influence of the drying method on the textural properties of porous carbon materials
Job, Nathalie ULg; Thery, Alexandre; Pirard, René ULg et al

in Carbon (2005), 43(12), 2481-2494

Carbon materials with tailored texture can be obtained from drying and pyrolysis of resorcinol-formaldehyde gels. The pore texture of both dried and pyrolyzed material depends on the drying process ... [more ▼]

Carbon materials with tailored texture can be obtained from drying and pyrolysis of resorcinol-formaldehyde gels. The pore texture of both dried and pyrolyzed material depends on the drying process. Several more or less expensive methods (supercritical drying, freeze-drying, evaporative drying) were tested in order to determine which process is the most suitable for the synthesis of a porous carbon with a definite texture. Supercritical drying leads to the highest pore volume and the widest texture range, but residual surface tensions and shrinkage are not avoided when the pore size is small or when the material density is low; this hampers to fix both the pore volume and the pore size easily. Monoliths are very difficult to obtain by freeze-drying, and the appearance of huge channels due to ice crystal growth at high dilution ratio hinders the fabrication of low density materials. Moreover, gels with small pores do not remain frozen throughout drying, which leads to surface tensions and shrinkage. Although generally replaced by more complicated techniques, evaporative drying is suitable when dense carbons are needed or when the only selection criterion is the pore size: all pore sizes are reachable, but this parameter is in this case strongly correlated to the pore volume. (C) 2005 Elsevier Ltd. All rights reserved. [less ▲]

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See detailElaboration of new formulations to remove micropollutants in MSWI flue gas
Brasseur, Alain; Gambin, Amandine; Laudet, Alain et al

in Chemosphere (2004), 56(8), 745-756

This study consists in identifying and testing potential inorganic substitutes to carbon based materials commonly used as adsorbents for the removal of organic pollutants such as dioxins and furans ... [more ▼]

This study consists in identifying and testing potential inorganic substitutes to carbon based materials commonly used as adsorbents for the removal of organic pollutants such as dioxins and furans released from Municipal Solid Waste Incinerators (MSWI). Although carbon materials enable to reach the current regulation in terms of dioxins and furans emissions, they exhibit a potential auto ignition risk when present in hot flue gases. Here, the adsorption potential of carbon based products is compared to the one of some inorganic materials. Chlorobenzene was chosen as a reference molecule to compare the removal performance of the different adsorbents. This comparison was based on the determination of the adsorption energies derived from temperature programmed desorption (TPD) experiments. In the first part of this study, five inorganic materials were selected according to their chlorobenzene adsorption performance compared to those of carbon based products currently used to remove micropollutants from MSWI flue gases. In the second part of the study, the influence of the inlet concentration of adsorbate on the adsorption potential of sorbents is investigated. Actually, the organic compound concentration was decreased in order to be closer to those met in MSWI. Furthermore, the adsorption experiments were performed with other adsorbates whose molecular mass or chlorine content are higher. Thanks to these adsorption results a new organic free formulation has been proposed for the removal of micropollutants. Tests carried out on an industrial scale, demonstrated that this product enables to reach the current norm concerning dioxins and furans emissions. (C) 2004 Elsevier Ltd. All rights reserved. [less ▲]

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See detailPorous carbon xerogels with texture tailored by pH control during sol-gel process
Job, Nathalie ULg; Pirard, René ULg; Marien, José ULg et al

in Carbon (2004), 42(3), 619-628

Despite commonly accepted ideas, evaporative drying does not always completely destroy the pore texture of phenolic gel. This work shows that very porous carbon materials can be synthesized by evaporative ... [more ▼]

Despite commonly accepted ideas, evaporative drying does not always completely destroy the pore texture of phenolic gel. This work shows that very porous carbon materials can be synthesized by evaporative drying and pyrolysis of aqueous resorcinol-formaldehyde gels provided that the operating variables are correctly chosen. Moreover, in this manner monoliths can be easily produced. The pore texture of the materials was studied before and after pyrolysis in order to determine which synthesis and/or pyrolysis variables have an influence on the final texture of the carbon. Results show that it is possible to tailor the morphology of these materials by varying the initial pH of the precursors solution in a narrow range. Micro-macroporous, micro-mesoporous, microporous or totally non-porous carbon materials were obtained. The specific surface area is independent from the initial pH whereas the total void volume varies from 0.4 to 1.4 cm(3)/g when the initial pH decreases from 6.25 to 5.45. These materials can be used as catalysts supports or for electrochemical applications, the texture control being an interesting advantage. (C) 2004 Elsevier Ltd. All rights reserved. [less ▲]

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See detailSynthesis of transition metal-doped carbon xerogels by solubilization of metal salts in resorcinol-formaldehyde aqueous solution
Job, Nathalie ULg; Pirard, René ULg; Marien, José ULg et al

in Carbon (2004), 42(15), 3217-3227

The pore texture of carbon materials obtained from evaporative drying and pyrolysis of resorcinol-formaldehyde aqueous gels is controlled by the initial pH of the precursors solution. In order to produce ... [more ▼]

The pore texture of carbon materials obtained from evaporative drying and pyrolysis of resorcinol-formaldehyde aqueous gels is controlled by the initial pH of the precursors solution. In order to produce transition metal-containing carbons with tailored texture, various metallic salts were dissolved in the precursors solution. When necessary, a complexing agent (HEDTA or DTPA) was added to render the metal ions soluble. Ni, Fe and I'd loaded carbon xerogels were synthesized and their pore texture was studied after evaporative drying and after pyrolysis. The carbon texture was also studied with regard to the nature of the metal and the amount of complexing agent. The solubilization of transition metal salts in the resorcinol-formaldehyde aqueous solution does not prevent the texture regulation, even though this texture control is influenced: the limits of the pH interval leading to micro mesoporous carbon materials can slightly differ when a metal salt and/or a complexing agent are added. The pH range shift depends mainly on the amount and nature of the complexing agent, but also slightly on the nature of the metal ion. Nevertheless, the metal particles obtained are rather big (diameter > 15 nm). For catalytic applications, the metal dispersion must be enhanced, especially in the case of expensive metals. (C) 2004 Elsevier Ltd. All rights reserved. [less ▲]

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See detailElectrochemistry of lanthanum and uranium chlorides in organic media: Deposition of lanthanum and uranium
Martinot, Lucien; Lopes, L.; Marien, José ULg et al

in Journal of Radioanalytical & Nuclear Chemistry (2002), 253(3), 407-412

Molten salts have been widely used for the electrochemical preparation of lanthanum and uranium metals at high temperature. In this paper we demonstrate the feasibility of a similar process in ... [more ▼]

Molten salts have been widely used for the electrochemical preparation of lanthanum and uranium metals at high temperature. In this paper we demonstrate the feasibility of a similar process in dimethylformamide (DMF) and in the mixture gamma-butyrolactone/tetrahydrofuran (gamma-BL/THF) The best conditions for the preparation were deduced from preliminary transient electrochemistry experiments and from secondary ions mass spectrometry (SIMS) measurements involving SIMS mappings and SIMS depth profile analyses. [less ▲]

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