References of "Heinrichs, Benoît"
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See detailAqueous sol-gel synthesis and film deposition methods for the large-scale manufacture of coated steel with self-cleaning properties
Mahy, Julien ULg; Léonard, Géraldine ULg; Pirard, Sophie ULg et al

in Journal of Sol-Gel Science and Technology (in press)

A process has been developed to enable the large scale production of pure TiO2 films deposited on 316L stainless steel in order to get an easy-to-clean surface. This large scale process requires an easy ... [more ▼]

A process has been developed to enable the large scale production of pure TiO2 films deposited on 316L stainless steel in order to get an easy-to-clean surface. This large scale process requires an easy aqueous sol-gel procedure for the synthesis of the TiO2 sol. This synthesis has been simplified to facilitate the extrapolation towards an industrial scale. Results of TEM, photocatalytic properties, film hydrophilicity, and texture obtained with the simplified aqueous sol-gel synthesis (IsoP-TiO2 synthesis) show similar properties to those obtained with the standard aqueous sol-gel synthesis of TiO2 (HAc-TiO2 synthesis) developed previously. Only X-Ray Diffraction patterns showed differences, with the presence of anatase-brookite phases in IsoP-TiO2 synthesis while anatase phase only was observed in HAc-TiO2 synthesis. Both the aqueous sol-gel synthesis of pure TiO2 and the film deposition on steel by roll-coating have been successfully extrapolated to a larger scale. The photocatalytic activity and the hydrophilicity of the film were found to be unchanged when compared to films produced at a laboratory scale, thus validating the production of an efficient easy-to-clean material. Although some problems are still to be solved, this study is a hopeful first step in the development of a large scale process for self-cleaning steel production. [less ▲]

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See detailNon-isocyanate polyurethanes from carbonated soybean oil Using monomeric or oligomeric diamines To achieve thermosets or thermoplastics
Poussard, Loïc; Mariage, J.; Grignard, Bruno ULg et al

in Macromolecules (2016), 49(6), 2162-2171

Fully bio- and CO2-sourced non-isocyanate polyurethanes (NIPUs) were synthesized by reaction of carbonated soybean oil (CSBO) either with biobased short diamines or amino-telechelic oligoamides derived ... [more ▼]

Fully bio- and CO2-sourced non-isocyanate polyurethanes (NIPUs) were synthesized by reaction of carbonated soybean oil (CSBO) either with biobased short diamines or amino-telechelic oligoamides derived from fatty acids to achieve respectively thermoset or thermoplastic NIPUs. Biobased carbonated vegetable oils were first obtained by metal-free coupling reactions of CO2 with epoxidized soybean oils under supercritical conditions (120 °C, 100 bar) before complete characterization by FTIR, 1H NMR, and electrospray ionization mass spectroscopy (ESI-MS). In a second step, biobased NIPUs were produced by melt-blending of the so-produced cyclocarbonated oil with the biobased aminated derivatives. The thermal and mechanical properties of resulting polymers were found to be depending on the cyclocarbonated vegetable oil/amine ratio. More precisely, short diamines and CSBO led to the formation of cross-linked NIPUs, and the resulting tensile and thermal properties were poor. In contrast, elastomeric NIPUs derived from oligoamides and CSBO exhibited a better rigidity, an improved elongation at break (εr up to 400%), and a higher thermal stability (T95 wt% > 350 °C) than those of starting oligoamides. These results are impressive and highlight the potentiality of this environmental friendly approach to prepare renewable NIPU materials of high performances. [less ▲]

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See detailDoping TiO2 films with carbon nanotubes to simultaneously optimise antistatic, photocatalytic and superhydrophilic properties
Léonard, Géraldine ULg; Remy, Simon; Heinrichs, Benoît ULg

in Journal of Sol-Gel Science and Technology (2016)

Pure and multiwall carbon nanotube (MWCNT)- doped titanium dioxide (TiO2) films, synthesised from two sol–gel routes (alcoholic and aqueous) and deposited by dipcoating on glass, have been developed as ... [more ▼]

Pure and multiwall carbon nanotube (MWCNT)- doped titanium dioxide (TiO2) films, synthesised from two sol–gel routes (alcoholic and aqueous) and deposited by dipcoating on glass, have been developed as conductive, photocatalytic and superhydrophilic materials. While already crystallised in anatase structure at low temperature when synthesised in water, samples prepared in alcohol are amorphous. Their crystallisation in air has been studied at increasing temperatures. Effective incorporation of functionalised MWCNTs is confirmed in both aqueous and alcoholic samples with a closer interaction with TiO2 particles in the case of aqueous synthesis. In alcoholic samples, 400 C seems to be an optimised calcination temperature since 300 C does not allow crystallisation into anatase and 500 C removes MWCNTs through burning. The purpose of MWCNT doping is to obtain coatings that exhibit easy-toclean or self-cleaning properties. This can be achieved through an optimised combination of electrical conductivity (for antistatic property), photoactivity and superhydrophilicity. These three properties require the crystallisation of TiO2 into anatase. MWCNT doping dramatically increases both conductivity and photocatalytic activity, especially in alcoholic samples for the former and in aqueous samples for the latter. On the other hand, MWCNT introduction does not significantly affect the (super)hydrophilicity of films, which depends solely on the crystallinity of TiO2. [less ▲]

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See detailOverview of Superhydrophilic, Photocatalytic and Anticorrosive Properties of TiO2 Thin Films Doped with Multi-walled Carbon Nanotubes and Deposited on 316L Stainless Steel
Léonard, Géraldine ULg; Remy, Simon; Heinrichs, Benoît ULg

in Materials Today: Proceedings (2016, February), 3(2), 434-438

TiO2 films with MWCNTs are produced for anticorrosive applications to increase the lifetime of steel materials. TiO2 has two additional properties, photoactivity and superhydrophilicity. Two TiO2 samples ... [more ▼]

TiO2 films with MWCNTs are produced for anticorrosive applications to increase the lifetime of steel materials. TiO2 has two additional properties, photoactivity and superhydrophilicity. Two TiO2 samples, synthesized in aqueous or alcoholic media, have been doped with MWCNTs. The material which best combines anticorrosive, superhydrophilic and photocatalytic properties, is the one produced in aqueous medium (Aq-TiO2-CNT). Doping with MWCNTs increases the photodegradation of p-nitrophenol from 18% to 50%. MWCNTs allow to reduce the corrosion current and the corrosion potential. The good superhydrophilicity of TiO2 is kept on stainless steel with a contact angle after illumination around 5°. [less ▲]

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See detailDoped sol–gel films vs. powders TiO2: On the positive effect induced by the presence of a substrate
Léonard, Géraldine ULg; Malengreaux, Charline; Melotte, Quentin et al

in Journal of Environmental Chemical Engineering (2016), 4

SiO2 and Ag–SiO2 doped TiO2 films and powders have been produced using a controlled sol–gel process. The dopant has been introduced using an alkoxysilane-functionalized ligand, with or without complexed ... [more ▼]

SiO2 and Ag–SiO2 doped TiO2 films and powders have been produced using a controlled sol–gel process. The dopant has been introduced using an alkoxysilane-functionalized ligand, with or without complexed silver ions. The influence of dopants on physico-chemical properties of the catalysts is studied by XRD, TEM–EDX, DRUV–vis analyses in the case of powders, while GIXRD, XPS, profilometry, UV–vis absorption analyses have been used for thin films. The photocatalytic activity has been evaluated from the degradation of methylene blue under UV-A light in the presence of the different catalysts over a period of 24 h. The detailed comparison between powders and films highlights a surprising positive effect in the case of films due to the presence of the substrate. In the case of photocatalytic powders, the presence of SiO2 or Ag–SiO2 into the TiO2 matrix has a detrimental effect on the photocatalytic activity while the opposite tendency is observed in the case of films, with best activities obtained with Ag–SiO2 doping. Different factors, in particular crystallinity modification between powders and films, have been studied to explain these opposite behaviors. In the case of powders, crystallization is hindered by SiO2 and Ag particles incorporation into the TiO2 matrix, leading to a decrease of the photocatalytic activity. In the case of thin films, probably because of the presence of a substrate, crystallization is not influenced by the presence of SiO2 and Ag particles. Therefore, the latter ones can fully play their role of electron traps leading to an enhanced photocatalytic activity. [less ▲]

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See detailPhotocatalytic decomposition of hydrogen peroxide over nanoparticles of TiO2 and Ni(II)-porphyrin doped TiO2: a relationship between activity and porphyrin anchoring mode
Tasseroul, Ludivine ULg; Pàez Martinez, Carlos ULg; Lambert, Stéphanie ULg et al

in Applied Catalysis B : Environmental (2016), 182

The nickel tetra(4-carboxyphenyl)porphyrin (TCPPNi) was chimisorbed on Degussa P25 TiO2 at different concentrations. Diffuse reflectance spectroscopy in the UV/vis region, Fourier transform infrared ... [more ▼]

The nickel tetra(4-carboxyphenyl)porphyrin (TCPPNi) was chimisorbed on Degussa P25 TiO2 at different concentrations. Diffuse reflectance spectroscopy in the UV/vis region, Fourier transform infrared spectroscopy and thermal gravimetry combined with differential scanning calorimetry measurements allowed the determination of the TCPPNi anchoring mode. At low TCPPNi concentrations, this anchoring on Degussa P25 TiO2 took place through all four carboxylic groups, while at higher concentrations the anchoring occurred through one or two carboxylic groups. For the firsttime,the effect of UV/vis light irradiation on the H2O2-degradation activity of TiO2 and TCPPNi-doped TiO2 was studied using the method of following the production of O2 by gas pressure monitoring. The activity of seven different catalysts was related to the TCPPNi anchoring mode and the percentage of TiO2 Degussa P25 coverage. An optimum degradation of H2O2 was observed for 0.0115 mol TCPPNi × g−1 P25. In that case, the TCPPNi was anchored through the four carboxylic groups, corresponding to a strong interaction with Degussa P25 TiO2. Moreover, the TCPPNi did not cover the surface completely, therefore allowing the light to reach and activate the TiO2. [less ▲]

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See detailProtoporphyrin IX Functionalised AgSiO2 Core-shell Nanoparticle: Plasmonic Enhancement of Fluorescence and Singlet Oxygen Production
Lismont, Marjorie ULg; Dreesen, Laurent ULg; Heinrichs, Benoît ULg et al

in Photochemistry & Photobiology (2016), 92

Metal-enhanced processes arising from the coupling of a dye with metallic nanoparticles (NPs) have been widely reported. However, few studies have simultaneously investigated these mechanisms from the ... [more ▼]

Metal-enhanced processes arising from the coupling of a dye with metallic nanoparticles (NPs) have been widely reported. However, few studies have simultaneously investigated these mechanisms from the viewpoint of dye fluorescence and photoactivity. Herein, protoporphyrin IX (PpIX) is grafted onto the surface of silver core silica shell NPs in order to investigate the effect of silver (Ag) localized surface plasmon resonance (LSPR) on PpIX fluorescence and PpIX singlet oxygen (1O2) production. Using two Ag core sizes, we report a systematic study of these photophysical processes as a function of silica (SiO2) spacer thickness, LSPR band position and excitation wavelength. The excitation of Ag NP LSPR, which overlaps the PpIX absorption band, leads to the concomitant enhancement of PpIX fluorescence and 1O2 production independently of the Ag core size, but in a more pronounced way for larger Ag cores. These enhancements result from the increase in the PpIX excitation rate through the LSPR excitation and decrease when the distance between PpIX and Ag NPs increases. A maximum fluorescence enhancement of up to 14-fold, together with an increase in photogenerated 1O2 production of up to five times are obtained using 100 nm Ag cores coated with a 5 nm thick silica coating. [less ▲]

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See detailDegradation of p-nitrophenol and bacteria with TiO2 xerogels sensitized in situ with tetra(4-carboxyphenyl)porphyrins
Tasseroul, Ludivine ULg; Lambert, Stéphanie ULg; Eskenazi, David et al

Poster (2015, September 10)

Heterogeneous photocatalysis is widely studied for environmental applications as oxidative processes can completely destroy organic pollutants such as alkanes, pesticides, dyes, etc. and microorganisms ... [more ▼]

Heterogeneous photocatalysis is widely studied for environmental applications as oxidative processes can completely destroy organic pollutants such as alkanes, pesticides, dyes, etc. and microorganisms. The most used photocatalyst is the commercial TiO2 Degussa P25, which is composed of 80% anatase and 20% rutile and which is active when TiO2 is exposed to UV light ( < 380 nm). Recently, several studies have been performed to extend the light absorption range of TiO2 towards the visible range. In this study, TiO2-based materials doped with porphyrins, a widely used dye for the photosensibilization of TiO2, have been prepared using a sol-gel process. To stabilize the TiO2-dye interactions, free metal tetra(4-carboxyphenyl)porphyrin and nickel tetra(4-carboxyphenyl)porphyrin were introduced in situ into the TiO2 matrix during the sol-gel process rather than by grafting. Samples were thoroughly characterized by TEM, X-ray diffraction, FT-IR, DR-UV/Vis and their texture has been examined by nitrogen adsorption–desorption at 77 K. The photocatalytic activity for the degradation of p-nitrophenol and Escherichia coli and Lactobacillus rhamnosus bacteria cells in aqueous medium, under halogen lamp light have been evaluated in relation with the physico-chemical modifications induced by the doping. The low temperature vacuum drying protocol (150°C) used in the present study enabled to obtain porphyrin doped TiO2 xerogels with a high specific surface area, and containing nanoparticles composed of amorphous- and anatase-TiO2. Diffuse reflectance spectroscopy attest the presence of TCPPH2 and TCPPNi within the TiO2 matrix. In a first step, the photoactivity of the xerogels is tested for p-nitrophenol degradation. Results show that crystallinity and nature and concentration of porphyrin introduced in situ have major impact on the degradation performances. In a second step, the best xerogel for p-nitrophenol degradation has been used to degrade bacteria. This xerogel degrades E. coli and L. rhamnosus bacteria cells in less than 48 and 24 h respectively. The photocatalytic degradation of a pollutant is thus correlated to the degradation of bacteria since a xerogel doped with the TCPPNi degrades both p-nitrophenol, E. coli and L. rhamnosus. [less ▲]

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See detailPhotocatalytic Oxidative Treatment of Waste Water contamined with Pharmaceutical Products
Vreuls, Christelle; Wilmot, Annick; Cludts, Marc et al

Poster (2015, July)

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See detailDevelopment by the sol–gel process of highly dispersed Ni–Cu/SiO2 xerogel catalysts for selective 1,2-dichloroethane hydrodechlorination into ethylene
Pirard, Sophie ULg; Mahy, Julien ULg; Pirard, Jean-Paul ULg et al

in Microporous and Mesoporous Materials (2015), 209

Ni–Cu/SiO2 xerogel catalysts have been synthesized by cogelation of industrial tetraethoxysilane (Dynasil) and chelates of Ni and Cu with industrial 3-(2-aminoethylamino)propyltrimethoxysilane (Dynasylan ... [more ▼]

Ni–Cu/SiO2 xerogel catalysts have been synthesized by cogelation of industrial tetraethoxysilane (Dynasil) and chelates of Ni and Cu with industrial 3-(2-aminoethylamino)propyltrimethoxysilane (Dynasylan DAMO) in industrial ethanol denatured with diethyl phthalate. Despite the use of industrial grade reagents, highly dispersed bimetallic Ni–Cu/SiO2 xerogel catalysts were obtained. These samples are composed of completely accessible Ni–Cu alloy crystallites with sizes of 1.6–3.4 nm located inside silica particles exhibiting a monodisperse microporous distribution. It appears that the bimetallic complex acts as a nucleation agent in the formation of silica particles. The combination of results obtained from the calculation of the metal ratio in catalysts, H2 chemisorption and transmission electron microscopy allowed calculating the surface composition of the nickel–copper particles in Ni–Cu/SiO2 cogelled xerogel catalysts. Values obtained indicate a very pronounced surface enrichment with copper. While 1,2-dichloroethane hydrodechlorination over pure nickel mainly produces ethane, increasing copper content in bimetallic catalysts results in an increase in ethylene selectivity. The specific consumption rate of 1,2-dichloroethane decreases when copper loading increases. The turnover frequency, that is, the number of catalytic cycle per active site (nickel atom and its surrounding copper atoms) and per second, seems to be independent of surface composition of alloy particles. [less ▲]

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See detailCatalytic epuration of biogaz
Claude, Vincent ULg; Toye, Dominique ULg; Heinrichs, Benoît ULg et al

Poster (2015, May 08)

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See detailWet method for the production of thin films (2)
Liquet, Dimitri ULg; Calberg, Cédric ULg; Eskenazi, David et al

Patent (2015)

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See detailWet method for the production of thin films (1)
Liquet, Dimitri ULg; Calberg, Cédric ULg; Eskenazi, David et al

Patent (2015)

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See detailEffect of iron nanoparticles synthesized by a sol-gel process on Rhodococcus erythropolis T902.1 for biphenyl degradation
Wannoussa, Wissal ULg; Masy, Thibaut ULg; Lambert, Stéphanie ULg et al

in Journal of Water Resource and Protection (2015), 7

Nanoparticles (NPS) are considered as a new generation of compounds to improve environmental remediation and biological processes. The aim of this study is to investigate the effect of iron NPS ... [more ▼]

Nanoparticles (NPS) are considered as a new generation of compounds to improve environmental remediation and biological processes. The aim of this study is to investigate the effect of iron NPS encapsulated in porous silica (SiO2) on the biphenyl biodegradation by Rhodococcus erythropolis T902.1 (RT902.1). The iron NPS (major iron oxide FexOy form) were dispersed in the porosity of a SiO2 support synthesized by sol-gel process. These Fe/SiO2 NPS offer a stimulating effect on the biodegradation rate of biphenyl, an organic pollutant that is very stable and water-insoluble. This positive impact of NPS on the microbial biodegradation was found to be dependent on the NPS concentration ranging from 10−6 M to 10−4 M. After 18 days of incubation the cultures containing NPS at a concentration of 10−4 M of iron improved RT902.1 growth and degraded 35% more biphenyl than those without NPS (positive control) or with the sole SiO2 particles. Though the microorganism could not interact directly with the insoluble iron NPS, the results show that about 10% and 35% of the initial 10−4 M iron NPS encapsulated in the SiO2 matrix would be incorporated inside or adsorbed on the cell surface respectively and 35% would be released in the supernatant. These results suggest that RT902.1 would produce siderophore-like molecules to attract iron from the porous silica matrix. [less ▲]

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See detailEffect of metal ions and metal nanoparticles encapsulated in porous silica on biphenyl biodegradation by Rhodococcus erythropolis T902.1
Wannoussa, Wissal ULg; Hiligsmann, Serge ULg; Tasseroul, Ludivine ULg et al

in Journal of Sol-Gel Science and Technology (2015), 75

Biodegradation of biphenyl was carried out by Rhodococcus erythropolis T902.1 in presence ofnanometer-sized metallic (Co, Pd, Ag and Cu) nanoparticles (NPS) synthesized by the sol-gel process. In order to ... [more ▼]

Biodegradation of biphenyl was carried out by Rhodococcus erythropolis T902.1 in presence ofnanometer-sized metallic (Co, Pd, Ag and Cu) nanoparticles (NPS) synthesized by the sol-gel process. In order to <br />prevent their agglomeration, the metallic NPs (1-2 nm diameter) were anchored inside microporous silica crystallites and named Co/SiO2, Pd/SiO2, Ag/SiO2 and Cu/SiO2 samples respectively. They were added at low concentrations of 10-6 M, 10-5 M and 10-4 M of metal in the culture medium and their impact was compared with that of the simple metal ions added as cobalt, palladium, silver or copper salts. The cultures containing Pd/SiO2 or Co/SiO2 samples at 10-4 M of metal achieved a 50% higher biphenyl degradation yield after 18 days of incubation and improved Rhodococcus erythropolis T902.1 growth compared with those without (positive control) or with silica particles only. The highest biodegradation performance, i.e. 107 ±3 ppm/day, which was about 85% higher than in control conditions without NPs, was recorded in 250 ml baffled flasks stirred at 150 rpm with Co/SiO2 sample at 10-4 M Co. Furthermore, the stimulating effect of NPs on biphenyl biodegradation seems to also depend on the thermal treatment conditions applied to NPs since the experimental results indicated that, after calcination, the cobalt oxide NPs at a concentration of 10-4 M were more effective than the reduced cobalt NPs with a degradation yield of 81 ±1% and 77 ±2% respectively after 18 days. On the other hand, the results showed that the addition of 10-4 M of Cu2+ or Ag+ ions or the addition of Cu/SiO2 or Ag/SiO2 samples at 10-4 M of metal have an inhibitory effect on biphenyl biodegradation. However, Cu2+ and Ag+ ions were more toxic to the Rhodococcus erythropolis T902.1 bacteria than the respective Cu or Ag NPS anchored inside silica particles. Moreover, this work showed that in these <br />conditions, the activity of catechol 1, 2-dioxygenase (a critical enzyme in aromatic biodegradation pathway) was severely inhibited, whereas the presence of 10-4 M of Co2+ ions or Co/SiO2 sample stimulated the enzyme activity compared to the conditions without NPs. [less ▲]

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See detailAmélioration de la biodégradation du biphényle par Rhodococcus erythropolis t902.1 en présence de Fe2O3 et de nanoparticules de fer encapsulées dans un xérogel de silice
Wannoussa, Wissal ULg; Hiligsmann, Serge ULg; Tasseroul, Ludivine ULg et al

in Déchets Sciences et Techniques (2015), 69

In this work, the effect of iron oxide particles Fe2O3 and iron nanoparticles encapsulated in a porous silica matrix (xerogel Fe/SiO2) was investigated on biphenyl biodegradation by the strain Rhodococcus ... [more ▼]

In this work, the effect of iron oxide particles Fe2O3 and iron nanoparticles encapsulated in a porous silica matrix (xerogel Fe/SiO2) was investigated on biphenyl biodegradation by the strain Rhodococcus erythropolis T902.1. After 18 days of incubation biodegradation yields of 75% and 85% were achieved respectively in presence of non-autoclaved or autoclaved xerogel Fe/SiO2 at 10-5 M iron. These results are 42 and 60 % higher than in standard conditions without nanoparticles. They suggest that the autoclave procedure lead to the release of some iron less anchored in the silica matrix. This study highlights that siderophore production by Rhodococcus erythropolis T902.1 would be related to the presence of iron nanoparticles in the culture. It suggests that the production of these strong chelating compounds decreases with increase of iron release from xerogel Fe/SiO2. Moreover, most of the surfactants synthesized by Rhodococcus erythropolis T902.1 which are glycolipids containing trehalose (hexose), would be linked to cell surface and not excreted in the culture medium; the biomass hexose content also increased by 85% in presence of iron nanoparticles. [less ▲]

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See detailHighly dispersed iron xerogel catalysts for p-nitrophenol degradation by photo-Fenton effects
Mahy, Julien ULg; Tasseroul, Ludivine ULg; Zubiaur, Anthony ULg et al

in Microporous and Mesoporous Materials (2014), 197

Several iron xerogel catalysts were synthesized by hydrolysis and condensation of tetraethoxysilane (TEOS) and 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS) which is able to form a chelate with iron ... [more ▼]

Several iron xerogel catalysts were synthesized by hydrolysis and condensation of tetraethoxysilane (TEOS) and 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS) which is able to form a chelate with iron ions. The EDAS/TEOS ratio strongly influences the texture of xerogel catalysts. The specific surface area and the micro- and mesoporous volume increase with this ratio. It seems that EDAS plays a nucleating agent role for silica particles and allows to anchor Fe-based moieties inside the silica network. Iron oxide nanoparticles of diameter 1-1.5 nm and Fe3+ ions result, encapsulated in silica particles with sizes of about 10-30 nm in diameter. The iron species was determined by Mössbauer spectroscopy and magnetometry measurements and only Fe3+ species were observed in xerogel catalysts. The Fenton and photo-Fenton effect of these catalysts were evaluated on the degradation of p-nitrophenol in aqueous media under different conditions. Results show that in the presence of H2O2, iron xerogel catalysts present a photo-Fenton effect, reaching 99 % of degradation after 24 h. [less ▲]

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