Sequentially Compressive and Intrusive Mechanisms in Mercury Porosimetry of Carbon BlacksPirard, René ; ; Blacher, Silvia et alin Journal of Colloid & Interface Science (1999), 217(1), 216-217 The mechanism of mercury penetration in two different commercial carbon blacks is studied. We show that the volume variation measured by mercury porosimetry in these systems is due to three successive ... [more ▼] The mechanism of mercury penetration in two different commercial carbon blacks is studied. We show that the volume variation measured by mercury porosimetry in these systems is due to three successive mechanisms, which occur as the pressure increases: (1) mercury invasion of voids between macroscopic grains, (2) compaction and elastic compression of macroscopic grains, (3) intrusion in the voids of aggregates formed by primary particles. The cumulative surface calculated by the Rootare-Prenzlow equation (S(RP)) in the intrusion part and the BET surface area measured by nitrogen adsorption (S(BET)) are compared. Copyright 1999 Academic Press. [less ▲] Detailed reference viewed: 10 (2 ULg) Deactivation mechanisms and regeneration of a bimetallic hydrodechlorination catalystHeinrichs, Benoît ; Noville, Francis ; et alin Studies in Surface Science and Catalysis (1999), 126 The temporal evolution of the activity and selectivity of a 1.9%Pd-3.7%Ag/SiO2 catalyst during selective hydrodechlorination of 1,2-dichloroethane into ethylene is examined. A comparison between the ... [more ▼] The temporal evolution of the activity and selectivity of a 1.9%Pd-3.7%Ag/SiO2 catalyst during selective hydrodechlorination of 1,2-dichloroethane into ethylene is examined. A comparison between the physico-chemical properties of the fresh catalyst and of the deactivated one suggests a deactivation mechanism by poisoning or coking of Ag sites at the surface of the active Pd-Ag particles. A regeneration treatment is proposed which allows to restore the initial properties of the fresh catalyst. [less ▲] Detailed reference viewed: 22 (6 ULg) Deactivation mechanisms and regeneration of a bimetallic hydrodechlorination catalystHeinrichs, Benoît ; Noville, Francis ; et alPoster (1999) Detailed reference viewed: 7 (0 ULg) Preparation of low-density xerogels through additives to TEOS-based alcogelsAlié, Christelle ; Pirard, René ; et alin Journal of Non-Crystalline Solids (1999), 246(3), 216-228 A new process for preparing silica xerogels with similar textural properties to silica aerogels by drying under vacuum has been studied. The xerogels are produced by adding, before gelation, 3-(2 ... [more ▼] A new process for preparing silica xerogels with similar textural properties to silica aerogels by drying under vacuum has been studied. The xerogels are produced by adding, before gelation, 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS) to tetraethylorthosilicate (TEOS)-based alcogels, synthesised in a single base-catalysed (NH3) step. It is hypothesized that EDAS acts as a nucleation agent leading to silica particles with a hydrolysed EDAS core and a shell principally made of hydrolysed TEOS. The EDAS concentration and the basicity of the aqueous NH3 solution are important parameters influencing the resistance of the gel to drying stress. A decreasing EDAS/TEOS ratio or an increasing concentration of NH3 at constant EDAS content leads to less shrinkage during drying and so the final pore volume is larger. Gels prepared with a low EDAS/TEOS ratio (about 0.03) contain large particles (similar to 20 nm) due to the nucleation process by EDAS, thus the pores between those particles are also large and the drying stress is reduced. (C) 1999 Published by Elsevier Science B.V. All rights reserved. [less ▲] Detailed reference viewed: 14 (1 ULg) Sequentially compressive and intrusive mechanisms in mercury porosimetry of carbon blacksPirard, René ; ; Blacher, Silvia et alin Journal of Colloid & Interface Science (1999), 217(1), 216-217 The mechanism of mercury penetration in two different commercial carbon blacks is studied. We show that the volume variation measured by mercury porosimetry in these systems is due to three successive ... [more ▼] The mechanism of mercury penetration in two different commercial carbon blacks is studied. We show that the volume variation measured by mercury porosimetry in these systems is due to three successive mechanisms, which occur as the pressure increases: (1) mercury invasion of voids between macroscopic grains, (2) compaction and elastic compression of macroscopic grains, (3) intrusion in the voids of aggregates formed by primary particles. The cumulative surface calculated by the Rootare-Prenzlow equation (S-RP) in the intrusion part and the BET surface area measured by nitrogen adsorption (S-BET) are compared. (C) 1999 Academic Press. [less ▲] Detailed reference viewed: 8 (0 ULg) Biodegradable and biocompatible inorganic-organic hybrid materials. 3. A valuable route to the control of the silica porosity; Blacher, Silvia ; Pirard, Jean-Paul et alin Langmuir (1998), 14(7), 1905-1910 Porous silica has been successfully prepared from poly(epsilon-caprolactone)-silica hybrid materials on the basis of the template approach. The final texture of the porous silica has been analyzed by the ... [more ▼] Porous silica has been successfully prepared from poly(epsilon-caprolactone)-silica hybrid materials on the basis of the template approach. The final texture of the porous silica has been analyzed by the nitrogen adsorption-desorption technique and by small-angle X-ray scattering (SAXS). The porosity of silica can be tailored by the poly(epsilon-caprolactone) (PCL) template, particularly molecular weight, molecular weight distribution, content, and type and number of reactive groups per chain. Increasing the molecular weight, content, and chain polydispersity of the PCL template and decreasing the reactivity and number of reactive groups per PCL chain result in a more heterogeneous microporosity and, as a rule, in larger pores, a broader pore size distribution, a larger specific surface area, and a larger total and microporous volume. [less ▲] Detailed reference viewed: 20 (9 ULg) Mercury porosimetry applied to low density xerogels; relation between structure and mechanical propertiesPirard, René ; Heinrichs, Benoît ; et alin Journal of Sol-Gel Science and Technology (1998), 13(1-3), 335-339 Samples of low density xerogels were submitted to mercury porosimetry at pressures up to 200 MPa. These samples show an unusual behavior: they are first crushed by the isostatic mercury pressure without ... [more ▼] Samples of low density xerogels were submitted to mercury porosimetry at pressures up to 200 MPa. These samples show an unusual behavior: they are first crushed by the isostatic mercury pressure without mercury intrusion and are then intruded by the mercury above a certain pressure. This transition allows the easy determination of the one constant found in the buckling model that is used to interpret the crushing part of the mercury porosimetry experiment. The relation between this constant and the structure of the xerogels determined by TEM and nitrogen adsorption is discussed. [less ▲] Detailed reference viewed: 13 (2 ULg) High temperature catalysts through sol-gel synthesis; Pirard, Jean-Paul ![]() in Journal of Non-Crystalline Solids (1998), 225 Detailed reference viewed: 6 (1 ULg) Texture control of freeze-dried resorcinol-formaldehyde gels; ; Blacher, Silvia et alin Journal of Non-Crystalline Solids (1998), 225 Detailed reference viewed: 44 (3 ULg) Porous silica obtained from biodegradable and biocompatible inorganic-organic hybrid materials; Blacher, Silvia ; Dubois, Philippe et alin Journal of Sol-Gel Science and Technology (1998), 13(1-3), 415-419 Porous silicas have been successfully prepared from poly(ε -caprolactone) (PCL)-silica hybrid materials based on the template approach. The final texture of the porous silica can be tailored by the PCL ... [more ▼] Porous silicas have been successfully prepared from poly(ε -caprolactone) (PCL)-silica hybrid materials based on the template approach. The final texture of the porous silica can be tailored by the PCL template, i.e., molecular weight and molecular weight distribution, content, type and number of reactive end-groups per chain. Porosity has been investigated by nitrogen adsorption-desorption technique and small angle X-ray scattering (SAXS). [less ▲] Detailed reference viewed: 24 (6 ULg) Pd-Ag/SiO2 sol-gel catalysts designed for selective conversion of chlorinated alkanes into alkenesHeinrichs, Benoît ; ; et alin Studies in Surface Science and Catalysis (1998), 118 Detailed reference viewed: 9 (2 ULg) Pd-Ag/SiO2 sol-gel catalysts designed for selective conversion of chlorinated alkanes into alkenesHeinrichs, Benoît ; ; et alConference (1998) Detailed reference viewed: 4 (0 ULg) Hydrodéchloration sélective du 1,2-dichloroéthane en éthylène sur un catalyseur xérogel Pd-Ag/SiO2Heinrichs, Benoît ; ; Pirard, Jean-Paul et alin Récents Progrès en Génie des procédés (1997, September 24) Detailed reference viewed: 16 (7 ULg) Kinetic study of 1,2-dichloroethane hydrodechlorination with a Pd-Ag/SiO2 sol-gel catalystHeinrichs, Benoît ; ; et alin 1st European Congress on Chemical Engineering, ECCE1 (Vol. 4, pp. 2919-2922) (1997, May 04) Detailed reference viewed: 10 (2 ULg) Pd/SiO2-cogelled aerogel catalysts and impregnated aerogel and xerogel catalysts: Synthesis and characterizationHeinrichs, Benoît ; Noville, Francis ; Pirard, Jean-Paul ![]() in Journal of Catalysis (1997), 170(2), 366-376 Pd/SiO2 aerogel catalysts have been synthesized by cogelation of tetraethoxysilane with complex Pd2+[NH2-CH2-CH2-NH-(CH2)(3)-Si(OCH3)(3)](2) containing a hydrolysable silyl group. Pd catalysts have also ... [more ▼] Pd/SiO2 aerogel catalysts have been synthesized by cogelation of tetraethoxysilane with complex Pd2+[NH2-CH2-CH2-NH-(CH2)(3)-Si(OCH3)(3)](2) containing a hydrolysable silyl group. Pd catalysts have also been prepared by impregnation of silica aerogels and xerogels with solutions of this complex or Pd2+(NH3)(4) followed by drying under hypercritical conditions or under vacuum. It appears that, in cogelled samples, the Pd2+ complex acts as a nucleation agent in the formation of silica particles. The resulting catalysts are then composed of completely accessible palladium crystallites with a diameter of about 2.3 nm located inside silica particles with a monodisperse microporous distribution centered on a hydraulic radius of 0.43 nm. The continuous meso- and macropore distribution is located in voids between particles and between aggregates constituted of those particles. In impregnated samples, it appears that Pd particles are located outside SiO2 particles. The relation between the texture of cogelled and impregnated catalysts and their behavior toward sintering has been studied in detail. In cogelled samples, it has been shown that Pd crystallites cannot migrate because they are trapped in the pores of SiO2 particles. These catalysts are sinterproof during hypercritical drying, When Pd crystallites are not trapped inside SiO2 particles, hypercritical drying leads to an extensive sintering of metal particles. During calcination of impregnated catalysts dried under vacuum, sintering occurs to a various extent depending on the support texture. The Pd crystallites size decreases when the pore size distribution is shifted toward the small sizes. (C) 1997 Academic Press. [less ▲] Detailed reference viewed: 41 (15 ULg) Palladium-silver sol-gel catalysts for selective hydrodechlorination of 1,2-dichloroethane into ethylene - I. Synthesis and characterizationHeinrichs, Benoît ; ; et alin Journal of Catalysis (1997), 172(2), 322-335 Low-density xerogel Pd-Ag/SiO2 catalysts were prepared by a cogelation of tetraethoxysilane with organically substituted alkoxides capable of forming chelates with palladium and silver ions, followed by a ... [more ▼] Low-density xerogel Pd-Ag/SiO2 catalysts were prepared by a cogelation of tetraethoxysilane with organically substituted alkoxides capable of forming chelates with palladium and silver ions, followed by a drying under vacuum, a calcination, and a reduction. The resulting Pd-Ag alloy particles have diameters of about 2-3 nm and are dispersed inside the silica particles which exhibit a monodisperse micropore size distribution centered at 0.8 nm. At low silver loading, the composition of the bimetallic particles is almost identical to the overall composition, but when this loading is increased, the percentage of silver in the alloy particles is appreciably lower than the overall percentage, In all bimetallic samples, a few large pure silver particles are observed. When dried under vacuum, the xerogels exhibit a texture similar to that of aerogels dried under supercritical conditions with pore volumes in the range 2-6 cm(3)/g and pores ranging from micro- to macropores of several hundred nanometers. When the silver loading is increased, xerogels containing palladium show aggregates of increasingly interpenetrated silica particles. This is explained bq an aggregation, during the gelation reaction, of colliding SiO2 particles which is limited by an increasingly slow sticking reaction due to the growing basicity in the precursor solution when the concentrations of Ag and associated compounds are increased. During thermal treatments, the Pd-Ag alloy seems to form by the migration, through the porous network, of silver which finally alloys with Pd crystallites trapped inside SiO2 particles. Whereas ethane is the main product when hydrodechlorination of 1,2-dichloroethane is performed over pure palladium, the dilution of this active metal by silver leads to a strong increase in ethylene selectivity. (C) 1997 Academic Press. [less ▲] Detailed reference viewed: 24 (6 ULg) Mercury porosimetry applied to low density xerogelsPirard, René ; Heinrichs, Benoît ; Pirard, Jean-Paul ![]() in Characterization of Porous Solids IV (1997) Detailed reference viewed: 12 (6 ULg) Rheological characterization on the BaTiO3 sol-gel transition; ; et al in Faraday Discussions (1997), 101 Detailed reference viewed: 20 (3 ULg) On the texture characterization of mixed SiO2-ZrO2 aerogels using the nitrogen adsorption-desorption isotherms. Classical and fractal methodsBlacher, Silvia ; Pirard, René ; Pirard, Jean-Paul et alin Langmuir (1997), 13 Detailed reference viewed: 13 (1 ULg) Textural properties and thermal stability of silica-zirconia aerogelsPirard, René ; ; et alin Journal of Sol-Gel Science and Technology (1997), 8 Detailed reference viewed: 33 (8 ULg) |
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