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See detailPhotocatalytic degradation of water pollutants with visible light-sensitized TiO2 xerogels
Tasseroul, Ludivine ULg; Pirard, Sophie ULg; Lambert, Stéphanie ULg et al

in Récents Progrès en Génie des Procédés (2014), 106

To extend its photocatalytic activity to visible light, TiO2 has been doped in situ through the cogelation sol-gel proces with two dyes : free metal tetra(4-carboxyphenyl)porphyrin and nickel tetra(4 ... [more ▼]

To extend its photocatalytic activity to visible light, TiO2 has been doped in situ through the cogelation sol-gel proces with two dyes : free metal tetra(4-carboxyphenyl)porphyrin and nickel tetra(4-carboxyphenyl)porphyrin. DR and FT-IR spectroscopies have been performed to determine the interaction between porphyrins and TiO2. Cristallinity and specific surface area have been measured by XRD and N2 adsorption. The photoactivity of the doped TiO2 xerogels has been evaluated for p-nitrophenol (a model water pollutant) degradation under visible light and a kinetic study has been performed. The samples allow the degradation of 40% of p-nitrophenol in 6 h which makes them very promising for water decontamination under natural light. A kinetic study of p-nitrophenol degradation with the Ni-doped catalyst has shown that the best kinetic model involves one type of active site corresponding to the hole h+ of electron-hole pairs created at the TiO2 surface by light. The rate determining step consists of the surface reaction between adsorbed p-nitrophenol and adsorbed OH• radicals. [less ▲]

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See detailSol-gel preparation and characterisation of SnO2 powders employed as catalyst for phenol photodegradation
Benhebal, Hadj; Chaib, Messaoud; Léonard, Angélique ULg et al

in Scientia Iranica (2013), 20(6), 1891-1898

Crystallized pure SnO2 powders were prepared by the sol-gel process and were used as photocatalyst for the degradation of phenol under UV light at pH 6.5 and a temperature of 20°C. The physical properties ... [more ▼]

Crystallized pure SnO2 powders were prepared by the sol-gel process and were used as photocatalyst for the degradation of phenol under UV light at pH 6.5 and a temperature of 20°C. The physical properties of photocatalyst were characterized by X-ray diffraction, Scanning Electron Microscopy, nitrogen adsorption-desorption and Ultraviolet-visible diffuse reflectance spectroscopy. The influences of different operating variables such as the pH, the photocatalyst loading, the initial concentration of phenol, were studied to improve the efficiency of phenol degradation. [less ▲]

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See detailAdsorption du bleu de méthylène sur des xérogels de carbone activés
Páez Martínez, Carlos ULg; Contreras, Soledad; Léonard, Angélique ULg et al

Poster (2012, October)

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See detailEffect of CO2 activation of carbon xerogels on the adsorption of methylene blue
Páez Martínez, Carlos ULg; Contreras, M. S.; Léonard, Angélique ULg et al

in Adsorption (2012), 18(3-4), 199-211

The effect of physical activation with CO2 of carbon xerogels, synthesized by pyrolysis of a resorcinolformaldehyde aqueous gel, on the adsorption capacities of Methylene Blue (MB) was studied. The ... [more ▼]

The effect of physical activation with CO2 of carbon xerogels, synthesized by pyrolysis of a resorcinolformaldehyde aqueous gel, on the adsorption capacities of Methylene Blue (MB) was studied. The activation with CO2 lead to carbon materials with micropore volumes ranging from 0.28 to 0.98 cm³/g -1 C. MB-adsorption isotherm studies showed that the increase of micropore volume and corresponding surface area led to: (i) a significant improvement in the capacity of MB-adsorption at monolayer coverage, from 212 to 714 mgg -1 C, and (ii) an increase of the binding energy related to Langmuir isotherm constant up to 45 times greater than those of commercial microporous activated carbons used as reference (NORIT R2030, CALGON BPL and CALGON NC35). It is proposed that the increase of the binding energy results from chemical cleaning of the O-groups onto carbon surface as a consequence of CO2-activation, increasing the π-π interaction between MB and graphene layers of the carbon xerogels. Finally, a series of batch kinetics were performed to investigate the effect of CO2-activation conditions on the mechanism of MB-adsorption. Experimental data were fitted using pseudo-first-order, pseudo-second-order and intraparticle diffusion kinetic models. From pseudo-second-order kinetic model, one observes an increase in the initial rate of MB-adsorption from 0.019 to 0.0565 min -1, by increasing the specific surface area from 630 to 2180 m²/g -1 C via CO2-activation. Depending on the activation degree of the carbons, two different mechanisms control the MB-adsorption rate: (i) at low activation degree, the intraparticle diffusion is the rate-limiting phenomenon, whereas (ii) at high activation degree, the reactions occurring at the solid/liquid interface are the rate-limiting steps. © 2012 Springer Science+Business Media, LLC. [less ▲]

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See detailKinetic study of p-nitrophenol photodegradation with modified TiO2 xerogels
Tasseroul, Ludivine ULg; Pirard, Sophie ULg; Lambert, Stéphanie ULg et al

in Chemical Engineering Journal (2012), 191

TiO2 xerogels were sensitized in one step by the in situ introduction of nickel (II) tetra(4-carboxyphenyl)porphyrin (TCPPNi) into the TiO2 matrix during sol–gel synthesis. Crystalline photoactive phase ... [more ▼]

TiO2 xerogels were sensitized in one step by the in situ introduction of nickel (II) tetra(4-carboxyphenyl)porphyrin (TCPPNi) into the TiO2 matrix during sol–gel synthesis. Crystalline photoactive phase TiO2-anatase was obtained without high thermal treatments and was determined by X-ray diffraction. The presence of TCPPNi in TiO2 xerogels was established by DR-UV/Vis and FT-IR spectroscopy. The introduction of porphyrin led to a diminution of the specific surface area of TiO2 xerogels, and this diminution was analyzed by nitrogen adsorption–desorption. The particle size was estimated by SEM. The xerogel surface charge state, which influences the interactions between pollutant and TiO2, was determined by measurement of the point of zero charge. The photoactivity of xerogels was evaluated for p-nitrophenol degradation in aqueous medium at 20 ◦C. Results showed that porphyrin doped TiO2 degraded more than 40% of the p-nitrophenol whereas non doped TiO2 xerogel degraded only 10% of the compound. Moreover, porphyrin was found to improve the photoactivity of TiO2 xerogels in a similar way to UV-A pretreatment. A kinetic study of p-nitrophenol degradation was then performed. Results showed that one type of active site corresponding to the hole of electron–hole pairs was created at the TiO2 surface by light and that the rate determining step was the reaction between the adsorbed p-nitrophenol molecule and the adsorbed OH• radical. The apparent activation energy was found to be equal to 12 kJ mol−1. [less ▲]

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See detailAdsorption of methylene blue on activated carbon xerogels
Páez Martínez, Carlos ULg; Contreras, Maria Soledad; Léonard, Angélique ULg et al

Poster (2011, November 30)

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See detailSynthesis by the sol-gel process of visible light sensitive-TiO2 for the degradation of pollutants and microorganisms
Tasseroul, Ludivine ULg; Lambert, Stéphanie ULg; Páez Martínez, Carlos ULg et al

in Récents Progrès en Génie des Procédés, Lavoisier Technique et Documentation, Volume 101, 6 p. (CD-ROM) (2011, November 29)

To stabilize the TiO2-dye interaction, free metal tetra(4-carboxyphenyl)porphyrin and nickel tetra(4-carboxyphenyl)porphyrin were introduced into the TiO2 matrix by cogelation rather than by grafting. DR ... [more ▼]

To stabilize the TiO2-dye interaction, free metal tetra(4-carboxyphenyl)porphyrin and nickel tetra(4-carboxyphenyl)porphyrin were introduced into the TiO2 matrix by cogelation rather than by grafting. DR and FT-IR spectroscopies were performed to establish the interaction between porphyrins and TiO2. Cristallinity and specific surface area were performed by XRD and nitrogen adsorption-desorption measurements. The photoactivity of doped-TiO2 xerogels was evaluated for p-nitrophenol and Escherichia coli degradation. Under visible light, the samples allowed the degradation of 40% of p-nitrophenol in 6 h and the elimination of 108 CFU/mL of E. coli in 48 h. [less ▲]

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See detailHighly efficient organic/inorganic titania xerogels for photocatalysis applications
Bodson, Céline ULg; Bied, Catherine; Páez Martínez, Carlos ULg et al

Poster (2011)

TiO2 heterogeneous photocatalysis is an attractive technique for the complete destruction of undesirable contaminants either in aqueous or gaseous phase by using solar or artificial light illumination ... [more ▼]

TiO2 heterogeneous photocatalysis is an attractive technique for the complete destruction of undesirable contaminants either in aqueous or gaseous phase by using solar or artificial light illumination. The main drawback of TiO2 is that it can be activated only by UV light because of its large band gap (3.20 eV for anatase). Thus, it would be interesting to sensitize TiO2 to the whole visible region by doping with non-metal atoms such as phosphorus. Furthermore, it was found that the P-doped species could significantly increase the specific surface area of the materials, which consequently exhibit a higher content of surface hydroxyl groups. Upon band gap excitation of TiO2, the photoinduced electrons and positively charged holes can reduce and oxidize the species adsorbed on the TiO2 particles. The high degree of recombination between photogenerated electrons and holes is a major rate-limiting factor controlling the photocatalytic efficiency. Attempts to increase the titania efficiency have been made by doping P-doped TiO2 with metals, such as Ag. In the present study, a sol-gel method is developed to synthesize P-doped TiO2 and P/Ag-codoped xerogels by a cogelation method [1] based on the hydrolysis and the condensation of Ti(OC3H7)4 in the presence of a phosphoryled compound able to complex silver: NH2-(CH2)2-NH-(CH2)2-P(O)-(OC2H5)2, EDAP), in various alcohols. These xerogels are dried at 150°C under vacuum for 24 h, and calcined under air for 5 h at 350°C, 450°C, 550°C and 650°C. The resulting materials were characterized by ICP-AES, TG-DSC, TEM, XRD, nitrogen adsorption-desorption isotherms, FT-IR and diffuse reflectance measurements in the UV/Vis region. To measure the photoactivity of these new hybrid organic/inorganic titania xerogels, all these samples were tested for the degradation of p-nitrophenol under visible light. The titanium, phosphorus and silver contents in xerogels were confirmed by ICP-AES. As expected, theoretical and actual Ti/P molar ratio and Ag contents in xerogels are similar and then after washing with THF for 48 h. These results allow to conclude that EDAP and Ag are well incorporated within the TiO2 matrix: EDAP is anchored in the titania matrix by complexation and cogelation with TTIP [2], whereas silver, first incorporated by complexation through the ethylenediamine fragment of EDAP, is present in the xerogels in the form of nanoparticles. It was found that the phosphor-doped species could significantly increase the surface area of the materials. [2] It is noteworthy that the porosity of these materials is not affected by the addition of silver acetate during the synthesis, a very slight decrease of the specific surface area being observed in all cases. The organic/inorganic hybrid titania materials display very high photocatalytic efficiencies in the degradation of p-nitrophenol compared to pure titania. Deeper investigations concerning the structure of these materials should enable a better understanding of the photocatalytic mechanisms involved with these hybrids and will soon be reported. 1. S. Lambert, K. Y. Tran, G. Arrachart, F. Noville, C. Henrist, C. Bied, J. J. E. Moreau, M. Wong Chi Man, B. Heinrichs, Micropor. Mesopor. Mater. 2008, 115, 609. 2. C.J.Bodson1, S.D. Lambert1, C. Alié1, X. Cattoën2, J-P. Pirard1, C. Bied2, M.Wong Chi Man2, B. Heinrichs1 ,Micropor. Mesopor. Mater. 2010, 134,157 [less ▲]

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See detailSynthesis by sol-gel process of visible light sensitive-TiO2 for the degradation of pollutants and microorganisms
Tasseroul, Ludivine ULg; Lambert, Stéphanie ULg; Páez Martínez, Carlos ULg et al

Poster (2011)

Since the discovery of photocatalytic decomposition of water on TiO2 electrodes by Fujishima and Honda [1], heterogenous photocatalysis has been widely studied for environmental applications ... [more ▼]

Since the discovery of photocatalytic decomposition of water on TiO2 electrodes by Fujishima and Honda [1], heterogenous photocatalysis has been widely studied for environmental applications. Photocatalytic processes are new technologies for waste water treatment because new compounds (alkanes, pesticides, dyes, etc.) in effluents are not readily degraded by the conventional treatments [2]. Oxidative processes can completely destroy organic pollutants [3] or microorganisms (bacteria, viruses, fungi, etc.) [4,5]. At this moment, the commercial Degussa P25 is the mostly used photocatalyst. Nevertheless, it requires UV light to be activated, that is why scientists try to activate TiO2 under visible light. The aim of this study is to synthesize photocatalysts activated by visible light and to evaluate their activity for the degradation of pollutants and microorganisms. The sol-gel process allows the direct introduction of visible light sensitive species like porphyrins inside the TiO2 matrix during the synthesis [6]. Two tetracarboxyphenyl porphyrins are synthesized for the sensitization of TiO2 to visible light : the metal free tetracarboxyphenyl porphyrin and the nickel tetracarboxyphenyl porphyrin. These porphyrins are characterized by 1H NMR, FT-IR and UV/Vis spectroscopies. They are introduced during the sol-gel synthesis of TiO2 matrix. Diffuse reflectance and FT-IR spectroscopies are used to ensure that porphyrins are incorporated inside the matrix of TiO2. Indeed, characteristic porphyrins peaks appear on spectra. The cristallinity and specific surfaces of catalysts are also determined by XRD and nitrogen adsorption-desorption measurements respectively. The depolluting efficiency of photocatalysts is evaluated for the degradation in water of p-nitrophenol, which is listed as one of the 114 organic pollutants by the Environmental Protection Agency in the US. After 6 h under visible light, 40 % of p-nitrophenol are degraded with some catalysts. The activity is influenced by i) the presence of porphyrins : the photoactivity increases with the amount of porphyrins ; ii) the nature of porphyrins : nickel porphyrins are more active than free metal porphyrins ; and iii) the crystallinity of catalysts : amorphous catalysts are less active than crystallized samples. The photocatalysts with the highest degradation rating of dyes will be selected for the degradation in water of Escherichia coli and Lactobacillus acidophilus. [1] A. Fujishima, K. Honda, Nature 238, 37-38 (1972) [2] P. Gogate, A. Pandit, Advances in Environmental Research 8, 501-551 (2004). [3] D. Chen, A. Ray, Water Research 32, 3223-3234 (1998) [4] R. Watts, S. Kong, M. Orr, G. Miller, B. Henry, Water Research 29, 95-100 (1995). [5] J. Hong, M. Otaki, Journal of Bioscience and Bioengineering 101, 185-189 (2006). [6] C. Wang, J. Li, G. Mele, G.M. Yang, F.-X. Zhang, L. Palmisano, G. Vasapollo, Applied catalysis 78, 218-226 (2007). [less ▲]

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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 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 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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