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See detailUnpredictable photocatalytic ability of H2-reduced rutile-TiO2 xerogel in the degradation of dye-pollutants under UV and visible light irradiation
Páez Martínez, Carlos ULg; Lambert, Stéphanie ULg; Poelman, Dirk et al

Poster (2011)

Photocatalytic degradation of organic and inorganic pollutants on the TiO2 semiconductor has been extensively studied as a way to solve environmental problems relating to wastewater and polluted air ... [more ▼]

Photocatalytic degradation of organic and inorganic pollutants on the TiO2 semiconductor has been extensively studied as a way to solve environmental problems relating to wastewater and polluted air. Anatase and rutile are the most commonly used crystalline structures of TiO2, with anatase showing a higher photocatalytic activity attributed to its higher specific surface area and its favourable band gap energy (Eg). However, its high band gap (Eg = 3.2 eV) implies the use of UV light (lambda ≤ 380 nm) to inject electrons into the conduction band (TiO2(e-CB)) and to leave holes in the valence band (TiO2(h+VB)). Although the low band gap energy of rutile-TiO2 (Eg = 3.02 eV) allows rutile to potentially absorb more solar energy than anatase, the anatase-to-rutile phase transition leads to the collapse of the TiO2 specific surface area, which may result in a decrease in the photocatalytic activity of rutile. Low specific surface area and therefore poor absorption properties lead to strong limitations in exploring the photo-efficiency of rutile. Nevertheless, rutile has been proved to be comparable to anatase in its photoelectrochemical properties when used in dye-sensitized solar cells. In the present study, a new process for the reduction of rutile-TiO2 xerogel under hydrogen flow was developed to enhance the photocatalytic activity of TiO2 materials synthesized by the sol-gel process. So a series of H2-reduced TiO2 xerogels of low specific surface area was prepared by hydrolysis and condensation of tetraisopropoxy titanium(IV) in 2-methoxyethanol. The gels were dried under vacuum, calcined in air at different temperatures (400°C, 500°C and 700°C) and finally reduced in H2 at 400 °C. The materials were characterized by X-ray diffraction, transmission electron microscopy (TEM), FT-IR spectroscopy and UV/Visible diffuse reflectance spectroscopy. The texture was determined by nitrogen adsorption-desorption measurements. The effects of the calcination/reduction treatments on the adsorption of methylene blue (MB) in aqueous solution and on the photocatalytic degradation of MB and crystal violet (CV) under UV and visible light irradiation were also evaluated. Results showed predictable modifications in the physico-chemical properties caused by the annealing of TiO2 xerogel at high calcination temperature (700 °C), such as a total anatase-to-rutile phase transition and a considerable loss of specific surface area from 260 to 2 m2 g-1. However, the higher degree of reduction exhibited by the rutile-TiO2 lattice led to unpredictable photocatalytic activity for the dye conversion under UV and visible light irradiation: the loss of specific surface area of the rutile-TiO2 sample was compensated by the increase in the affinity of this sample for the dye. Under UV light irradiation, the rutile-TiO2 xerogel obtained after a calcination at 700 °C showed a similar level of photoactivity as the one obtained with anatase-TiO2 xerogels obtained by calcination at 400 °C and 500 °C. Under visible light, unlike anatase-TiO2 xerogels, the rutile-TiO2 xerogel showed a higher dye photoconversion rate per external surface area (40 times higher) than the commercial TiO2 Degussa P25. [less ▲]

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See detailRelationships between the structure of P-doped TiO2 xerogels and their photocatalytic properties
Bodson, Céline ULg; Cattoën, Xavier; Bied, Catherine et al

Conference (2011)

TiO2 heterogeneous photocatalysis has been the subject of numerous recent investigations as it is an attractive technique for the complete destruction of undesirable contaminants both in aqueous and ... [more ▼]

TiO2 heterogeneous photocatalysis has been the subject of numerous recent investigations as it is an attractive technique for the complete destruction of undesirable contaminants both in aqueous and gaseous phase by using solar or artificial light illumination. However, TiO2-based materials present a large band gap and therefore only a small fraction of solar light, in the UV region, can be utilized. Furthermore, anatase-TiO2 transforms to the rutile structure at temperatures relatively lower, which greatly reduces surface areas of the particles resulting in the decrease in photocatalytic ability of TiO2. To counter both disadvantages, several studies have been conducted by doping non-metallic elements, such as phosphor, into the Ti-O framework to form TiO2 solutions. In the present study, a sol-gel method is developed to synthesize P-doped TiO2 xerogels by a cogelation method based on the hydrolysis and the condensation of Ti(OC3H7)4 with functionalized P alkoxides: NH2-(CH2)2-NH-(CH2)2-P(O)-(OC2H5)2, or (C2H5O)2-P(O)-(CH2)7-CH3, in various alcohols. These xerogels are dried at 150°C under vacuum for 24 h, and calcined under air for 6 h at 350°C, 450°C, 550°C and 650°C. The resulting materials were characterized by TG-ATD, TEM, XRD, nitrogen adsorption-desorption isotherms, FT-IR and diffuse reflectance measurements in the UV/Vis region. It was found that the phosphor-doped species could significantly increase the surface area of the materials. Moreover, the phosphor-doping improved the thermal stability of titania and decreased the phase transformation of anatase to rutile. Diffuse reflectance measurements proved that the modification by phosphor shifted the absorption edge of titania to the visible region, making it an effective photocatalyst in visible light. This is shown by the degradation of p-nitrophenol under visible light irradiation. The excellent photocatalytic activity of P-doped TiO2 xerogels compared to pure TiO2 could be explained by its high surface area and small crystallite size. [less ▲]

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See detailRelations entre la structure et la texture poreuse de xérogels de TiO2 dopés au phosphore et leurs propriétés photocatalytiques
Bodson, Céline ULg; Cattoën, Xavier; Bied, Catherine et al

in Récents Progrès en Génie des Procédés, Lavoisier Technique et Documentation, Volume 101, 6 p. (CD-ROM) (2011)

The sol-gel process is used to prepare phosphorus (P)-doped TiO2 xerogels by cogelation of Ti(O-iPr)4 with a functionalized P-based alkoxide : NH2-(CH2)2-NH-(CH2)2-P(O)-(OEt)2, in various alcohols. These ... [more ▼]

The sol-gel process is used to prepare phosphorus (P)-doped TiO2 xerogels by cogelation of Ti(O-iPr)4 with a functionalized P-based alkoxide : NH2-(CH2)2-NH-(CH2)2-P(O)-(OEt)2, in various alcohols. These xerogels were dried under vacuum at 150°C during 12 h, and calcined under air for 5 h at 350 °C, 450 °C, 550 °C and 650 °C. The samples obtained were characterized by X-ray diffraction, nitrogen adsorption-desorption isotherms and diffuse reflectance spectroscopy in UV/Vis region. The presence of phosphorus in the samples leads to a significant increase of their specific surface area, proportionally to the amount of phosphorus in the sample. Furthermore, the doping of the TiO2 by a phosphonate compound increases the thermal stability of the TiO2 and delays the phase transformation from amorphous to anatase. The diffuse reflectance measurements clearly show the translation of absorption peak of TiO2 towards the visible region when the content in phosphorus increases. Indeed, it is observed a degradation of the p-nitrophenol under visible light by using these P-doped TiO2 xerogels, which means that the P-doping enhances the photocatalytic activity in the visible region. [less ▲]

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See detailExperimental procedure and statistical data treatment for the kinetic study of selective hydrodechlorination of 1,2-dichloroethane into ethylene over a Pd-Ag sol–gel catalyst
Pirard, Sophie ULg; Pirard, Jean-Paul ULg; Heyen, Georges ULg et al

in Chemical Engineering Journal (2011), 173(3), 801-812

The kinetics of selective hydrodechlorination of 1,2-dichloroethane into ethylene over a Pd- Ag/SiO2 catalyst was studied using an a priori experimental design with five independent variables—temperature ... [more ▼]

The kinetics of selective hydrodechlorination of 1,2-dichloroethane into ethylene over a Pd- Ag/SiO2 catalyst was studied using an a priori experimental design with five independent variables—temperature and partial pressures of 1,2-dichloroethane, hydrogen, ethylene and hydrogen chloride. A Langmuir–Hinshelwood model including two types of active site and the 1,2-dichloroethane adsorption as the rate-determining step was found to fit correctly with experimental data, according to the analysis of variance and the analysis of pondered residuals. The study allowed for catalytic deactivation. The rigorous experimental and statistical approach followed to carry out such a kinetic study is explained in detail. [less ▲]

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See detailStudy of photocatalytic decomposition of hydrogen peroxide over ramsdellite-MnO2 by O2-pressure monitoring
Páez Martínez, Carlos ULg; Liquet, Dimitri ULg; Calberg, Cédric ULg et al

in Catalysis Communications (2011), 15

The catalytic and photocatalytic activities of ramsdellite type manganese oxide, R-MnO2 were studied from the initial rate of decomposition of H2O2 in aqueous solution. The kinetic study was followed by ... [more ▼]

The catalytic and photocatalytic activities of ramsdellite type manganese oxide, R-MnO2 were studied from the initial rate of decomposition of H2O2 in aqueous solution. The kinetic study was followed by the production of O2 via gas pressure monitoring (O2-monitored method), in the dark and under visible light irradiation (λ≥400 nm), at 20 °C. Experimental data showed that the rate of H2O2 decomposition, under visible light irradiation and in the dark, obeys the first order kinetic law.While in the dark the H2O2 decomposition rate bymass unit was around 6.88 mmol g−1 s−1, under visible light irradiation theH2O2 decomposition rate achieved a maximal value of 15.13 mmol g−1 s−1. The increase in the H2O2 decomposition, by effect of the visible light, was observed in ranges of catalyst concentrations from 16 to 374 mg L−1. These results reflect the potential of R-MnO2 as a photoactive catalyst, being a consequence of presumed photoreduction of Mn4+centers. [less ▲]

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See detailImprovement in the methylene blue adsorption capacity and photocatalytic activity of H2-reduced rutile-TiO2 caused by Ni(II)porphyrin preadsorption
Páez Martínez, Carlos ULg; Lambert, Stéphanie ULg; Poelman, Dirk et al

in Applied Catalysis B : Environmental (2011), 106

H2-reduced rutile-TiO2 xerogel (Ti-700), obtained via the sol–gel process, was found to strongly adsorb the Ni(II)-5,10,15,20-tetrakis(4-carboxyphenyl)-porphyrin (NiTCPP) from a methanolic solution ... [more ▼]

H2-reduced rutile-TiO2 xerogel (Ti-700), obtained via the sol–gel process, was found to strongly adsorb the Ni(II)-5,10,15,20-tetrakis(4-carboxyphenyl)-porphyrin (NiTCPP) from a methanolic solution, despite its very low specific surface area (SBET ≈ 2 m2 g−1). UV/vis spectroscopy analysis showed that after calcination at 700 ◦C and reduction under H2 flow at 400 ◦C, the TiO2-xerogel increased its NiTCPP-adsorption capacity by surface area unit by up to 120 times. The effect of the porphyrin presence in the catalytic performances of TiO2-xerogels was studied through three kinetics models: (i) the pseudo-first-order kinetic model; (ii) the pseudo-second-order kinetic model, which are used to describe the adsorption rate based on the adsorption capacity of the catalysts; and (iii) the Langmuir–Hinshelwood kinetic model which is used to describe the photocatalytic degradation rate of methylene blue (MB). A significant improvement in the efficiency of Ti-700 was observed after the porphyrin-adsorption process (NiTCPP/Ti-700): MB-adsorption capacity at equilibrium and the apparent MB-photoconversion constant, kapp, of NiTCPP/Ti-700 were both up to 2 times higher than those observed for the Ti-700. [less ▲]

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See detailEffects of additives and solvents on the gel formation rate and on the texture of P- and Si-doped TiO2 materials
Bodson, Céline ULg; Lambert, Stéphanie ULg; Alié, Christelle ULg et al

in Microporous and Mesoporous Materials (2010), 134

Organic/inorganic hybrid TiO2 xerogels have been synthesized from titanium tetraisopropoxide and an organosilylated or organophosphorylated additive either in 2-methoxyethanol or isopropanol. The ... [more ▼]

Organic/inorganic hybrid TiO2 xerogels have been synthesized from titanium tetraisopropoxide and an organosilylated or organophosphorylated additive either in 2-methoxyethanol or isopropanol. The mechanisms of formation of the gels have been studied before gelation by liquid NMR spectroscopy and connected to their structure after drying analyzed by Raman spectroscopy, solid state NMR and N2 adsorption/desorption. The effects of the additives and solvents on the gel formation rate and on the texture of the xerogel have been addressed. [less ▲]

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See detailAn in-situ NMR analysis of the formation of P- and SiO2-doped TiO2 xerogels
Bodson, Céline ULg; Lambert, Stéphanie ULg; Cattoën, Xavier et al

Poster (2010, July)

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See detailActivated-carbon-xerogel/TiO2-P25 composite photocatalysts with high activity for the degradation of p-nitrophenol
Páez Martínez, Carlos ULg; Contreras, María; Olivera-Fuentes, Claudio et al

Poster (2010, July)

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See detailCours de base et applications - Une approche pédagogique
Heinrichs, Benoît ULg

Speech/Talk (2010)

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See detailChimie (3e partie)
Heinrichs, Benoît ULg

Learning material (2010)

Detailed reference viewed: 52 (23 ULg)
See detailChimie (2e partie)
Heinrichs, Benoît ULg

Learning material (2010)

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See detailSynthesis of very highly dispersed platinum catalysts supported on carbon xerogels by the strong electrostatic adsorption method
Lambert, Stéphanie ULg; Job, Nathalie ULg; D'Souza, Lawrence et al

in Journal of Catalysis (2009), 261

Highly dispersed Pt/carbon xerogel catalysts are obtained by applying the “Strong Electrostatic Adsorption” (SEA) of hexachloroplatinic acid to carbon xerogels (PZC = 9.4) and platinum tetraammine ... [more ▼]

Highly dispersed Pt/carbon xerogel catalysts are obtained by applying the “Strong Electrostatic Adsorption” (SEA) of hexachloroplatinic acid to carbon xerogels (PZC = 9.4) and platinum tetraammine chloride to oxidized carbon xerogels (PZC = 2.4). After the reduction step, all these Pt/carbon xerogel catalysts display a very high level of metal dispersion: very small platinum particles (1.1-1.3 nm) are observed by TEM. Pt particle sizes obtained by CO chemisorption are in good agreement with TEM micrographs, which shows that the metal is accessible to reactants. These Pt/carbon xerogel catalysts are very active for the hydrogenation of benzene into cyclohexane. [less ▲]

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