Image analysis, impedance spectroscopy and mercury porosimetry characterisation of freeze-drying porous materials

in Colloids and Surfaces A : Physicochemical and Engineering Aspects (2001), 187-188

Image analysis and impedance spectroscopy have been used as potential tools for the characterization of the texture of ultramacroporous PLA foams prepared by freeze-drying. It has been shown that these ... [more ▼]

Image analysis and impedance spectroscopy have been used as potential tools for the characterization of the texture of ultramacroporous PLA foams prepared by freeze-drying. It has been shown that these two techniques actually provide valuable information on the structure of this material. They are complementary to mercury porosimetry, which does not allow morphological details to be distinguished. Image analysis of SEM micrographs of transverse cross-sections at two different magnifications gave information on both the macroporosity (1 μm < width < 10 μm) and ultramacroporosity (width > 10 μm). Impedance spectroscopy was used to investigate the transport properties of the three-dimensional porous matrices by measurement of ionic conduction [less ▲]

Mass transfer in low-density xerogel catalysts

in AIChE Journal (2001), 47(8), 1866-1873

Texture and morphology of a Pd-Ag/SiO2 hydrodechlorination low-density xerogel catalyst prepared by a cogelation sot-gel process were characterized in detail to examine mass transfer in such catalysts ... [more ▼]

Texture and morphology of a Pd-Ag/SiO2 hydrodechlorination low-density xerogel catalyst prepared by a cogelation sot-gel process were characterized in detail to examine mass transfer in such catalysts. The catalyst consists of active Pd-Ag nanocrystallites trapped inside elementary 20 nm microporous silica particles arranged in larger aggregates, which constitute the macroscopic pellet. To reach active sites, reactants must first diffuse through large pores located between aggregates of SiO2 Particles and then through smaller pores located between those elementary particles inside the aggregates. Finally, they, diffuse through micropores located inside silica particles. Diffusion in such a "funnel" structure cannot be described assimilating the pellet to a pseudo-continuum. Diffusion should be examined carefully at three levels of decreasing size: the macroscopic pellet, the aggregate of silica particles, and the elementary silica particle. This approach shows that cogelled xerogel catalysts have remarkable mass-transfer properties. [less ▲]

Palladium-silver sol-gel catalysts for selective hydrodechlorination of 1,2-dichloroethane into ethylene III. Kinetics and reaction mechanism

in Journal of Catalysis (2001), 200(2), 309-320

The kinetics of selective hydrodechlorination of 1,2-dichloro-ethane into ethylene over a Pd-Ag/SiO2 catalyst is studied. Kinetic data at 573, 596, and 647 K have been obtained by means of experimental ... [more ▼]

The kinetics of selective hydrodechlorination of 1,2-dichloro-ethane into ethylene over a Pd-Ag/SiO2 catalyst is studied. Kinetic data at 573, 596, and 647 K have been obtained by means of experimental designs in the space of the partial pressures of the four components influencing kinetics, that is, 1,2-dichloroethane, hydrogen, ethylene, and hydrogen chloride. One model among the numerous ones examined allows us to represent correctly the experimental data. Ii: corresponds to the following mechanism: dechlorination of 1,2-dichloroethane into ethylene occurs on silver through dissociative adsorption with successive breaking of the two C-Cl bonds and desorption of C2H4. Thanks to its activation power of hydrogen by dissociative chemisorption, palladium present at the surface of the alloy supplies hydrogen atoms for regeneration of the chlorinated silver surface into metallic silver. The presence of hydrogen adsorbed on Pd also causes the undesired ethylene hydrogenation leading to a loss of olefin selectivity. (C) 2001 Academic Press. [less ▲]

Preparation of low-density xerogels by incorporation of additives during synthesis

in Journal of Non-Crystalline Solids (2001), 289(1-3), 88-96

Low-density xerogels were prepared by incorporation of an additive to alcogels prior to gelation. The additives studied are 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS), 3 ... [more ▼]

Low-density xerogels were prepared by incorporation of an additive to alcogels prior to gelation. The additives studied are 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS), 3-aminopropyltrimethoxysilane (AMS), propyltrimethoxysilane (PMS), tetramethylorthosilicate (TMOS) and 3-aminopropyltriethoxysilane (AES) using tetraethylorthosilicate (TEOS) as main silica precursor. Samples were also prepared with EDAS as additive and TMOS as main silica reagent. When the additive contains methoxy groups, it reacts first, forms nuclei on which the main reagent TEOS reacts to form the silica particles. The nucleation mechanism by the additive occurs only in case of a difference of reactivity between additive and main silica precursor. The other group of the additive (amine, alkyl group, ...) influences only the gelation time. In case of ethoxy groups (series AES/TEOS) or methoxy groups (series EDAS/TMOS) for both additive and main reagent, there is no nucleation by the additive. (C) 2001 Elsevier Science B.V. All rights reserved. [less ▲]

Characterization of porous polylactide foams by image analysis and impedance spectroscopy

in Langmuir (2000), 16(26), 10463-10470

The texture of highly porous polylactide foams prepared by freeze-drying of poly-L-lactide (L-PLA) and poly-DL-lactide (DL-PLA) solutions of various concentrations was investigated by two novel ... [more ▼]

The texture of highly porous polylactide foams prepared by freeze-drying of poly-L-lactide (L-PLA) and poly-DL-lactide (DL-PLA) solutions of various concentrations was investigated by two novel methodologies, image analysis and impedance spectroscopy. Image analysis of scanning electron micrographs of transverse cross-sections at two different magnifications gave information on both the macroporosity (1 mum < width 10 <mu>m) and ultramacroporosity (width > 10 mum). Impedance spectroscopy was used to investigate the transport properties of the three-dimensional porous matrices by measurement of ionic conduction. Image analysis showed that: (a) the macroporosity, which mainly contributes to porosity, is independent of the sample composition; (b) when the concentration of the polymer solution is increased, the density of the ultramacropores decreases and their average diameter increases; (c) the distribution of the ultramacropores is more homogeneous in the semicrystalline L-PLA. foams than in the amorphous DL-PLA counterparts, in which the ultramacropores tend to make clusters. The dielectric properties changed at low frequency, in relation to modifications in the ultramacroporosity. Ultramacropores of the L-PLA foams were found to be more open and more sensitive to the concentration of the polymer solutions compared with DL-PLA. Expectedly, the mechanical properties of the PLA foams changed with the structure of the ultramacroporous network. These results encourage further investigations on the texture of porous supports, to collect pertinent information on the physical macro- and ultramacroenvironment in which cells will reside. [less ▲]

Process for the preparation of a catalyst and its use for the conversion of chloroalkanes into alkenes containing less chlorine

Patent (2000)

Process for the preparation of a catalyst including a metal of group VIII and a metal of group Ib, according to which the mixture including the alkoxide precursor of an inorganic oxide and complexes ... [more ▼]

Process for the preparation of a catalyst including a metal of group VIII and a metal of group Ib, according to which the mixture including the alkoxide precursor of an inorganic oxide and complexes including the metals of group VIII and Ib and difunctional complexing compounds including an electron-donor group and a hydrolysable group is hydrolysed in order to form a gel. Process for the conversion of chloroalkanes into alkenes containing less chlorine by means of hydrogen, using such a catalyst. [less ▲]

Micropore size distributions of activated carbons

in Langmuir (2000), 16(16), 6754-6756

Dispersed Pd-Ag alloys for selective production of olefins from chlorinated alkanes

in Studies in Surface Science and Catalysis (2000), 130

Characterization of porous polylactide foams by image analysis and impedance spectroscopy

in Langmuir (2000), 16(26), 10463-10470

Dispersed Pd-Ag alloys for selective production of olefins from chlorinated alkanes

Poster (2000)