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Synthesis and characterization of zirconium-doped mesoporous nano-crystalline TiO<sub>2</sub>
Bineesh, Kanattukara Vijayan,Kim, Dong-Kyu,Park, Dae-Won Royal Society of Chemistry 2010 Nanoscale Vol.2 No.7
<P>A series of zirconium-doped nano-titania (Zr/TiO<SUB>2</SUB>) with various amounts of Zr were prepared by sol–gel method using titanium(<SMALL>IV</SMALL>) isopropoxide and zirconium nitrate as precursors. Zr/TiO<SUB>2</SUB> samples were characterized using X-ray diffraction (XRD), surface area–pore volume measurements, infrared (FTIR) spectroscopy, UV–vis-diffuse reflectance spectroscopy (UV–vis-DRS), X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, thermogravimetric (TG) analysis, and transmission electron microscopy (TEM) techniques. XRD data and Raman spectra indicated that even after 5 mol% doping of zirconium in the crystal lattice of TiO<SUB>2</SUB>, the samples were phase pure with the anatase structure. The crystalline size of the anatase decreased with increasing Zr content. An increase in the BET surface area was also observed after doping of zirconium on nano-titania.</P> <P>Graphic Abstract</P><P>Highly dispersed zirconium-doped nano-TiO<SUB>2</SUB> materials were synthesized by sol–gel method and its physico-chemical properties were studied using characterization techniques. <IMG SRC='http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/image/GA?id=c0nr00108b'> </P>
Bineesh, Kanattukara Vijayan,Kim, Dong-Kyu,Kim, Dong-Woo,Cho, Han-Jun,Park, Dae-Won Royal Society of Chemistry 2010 ENERGY AND ENVIRONMENTAL SCIENCE Vol.3 No.3
<P>The performance of vanadia-doped zirconia-pillared clay (V/Zr-PILC) for the selective catalytic oxidation of H<SUB>2</SUB>S was investigated in this study. A series of vanadia-doped zirconia pillared clays (V/Zr-PILCs) with various amounts of vanadia were prepared and characterized using X-ray diffraction (XRD), surface area-pore volume measurements, chemical analysis, infrared (FTIR) spectroscopy, UV–vis-diffuse reflectance spectroscopy (UV–vis-DRS), X-ray photoelectron spectroscopy (XPS), and thermogravimetric (TG) analysis. V/Zr-PILCs showed better catalytic performance than Zr-PILC at temperatures ranging from 220–300 °C without any considerable SO<SUB>2</SUB> emission. The H<SUB>2</SUB>S conversion over V/Zr-PILCs increased with increasing vanadia content up to 6 wt%. However, it decreased at higher vanadia loadings due to the decrease of surface area and to the formation of the crystalline V<SUB>2</SUB>O<SUB>5</SUB> phase. The results of a regeneration experiment using 6 wt% V/Zr-PILC catalyst showed good reproducibility in its catalytic activity, even through five successive sulfidation-regeneration cycles at 280 °C.</P> <P>Graphic Abstract</P><P>Vanadia-doped zirconia-pillared clays (V/Zr-PILCs) were synthesized and used as catalysts for the selective catalytic oxidation of H<SUB>2</SUB>S. <IMG SRC='http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/image/GA?id=b921937d'> </P>
Bineesh, K.V.,Kim, S.Y.,Jermy, B.R.,Park, D.W. Korean Society of Industrial and Engineering Chemi 2009 Journal of industrial and engineering chemistry Vol.15 No.2
A series of vanadia-doped titania pillared clay (V/Ti-PILC) with various amounts of vanadia were prepared and their performance for the selective catalytic oxidation of H<SUB>2</SUB>S was investigated in this study. V/Ti-PILCs were characterized using X-ray diffraction (XRD), BET apparatus, and X-ray photoelectron spectroscopy (XPS). V/Ti-PILCs showed better catalytic performance than as such Ti-PILC at temperatures ranging from 220 to 300<SUP>o</SUP>C without any considerable SO<SUB>2</SUB> emission. The H<SUB>2</SUB>S conversion over V/Ti-PILC increased with increasing vanadia content up to 5wt.%. This superior catalytic performance might be related to the uniform dispersion of vanadia in the form of monomeric and polymeric species. However, it decreased at 10wt.% vanadia loading due to the decrease of surface area and to the formation of crystalline V<SUB>2</SUB>O<SUB>5</SUB> phase. The presence of water vapor in the reactant mixture resulted in the decrease of the H<SUB>2</SUB>S conversion.
Bineesh, K.V.,Kim, D.K.,Cho, H.J.,Park, D.W. Korean Society of Industrial and Engineering Chemi 2010 Journal of industrial and engineering chemistry Vol.16 No.4
In the present work, titania-pillared clay (Ti-PILC) and zirconia-pillared clay (Zr-PILC) were synthesized, and their catalytic performance was studied for the selective oxidation of H<SUB>2</SUB>S to elemental sulfur. The obtained pillared clays (PILCs) were characterized by X-ray fluorescence spectroscopy (XRF), infrared (FTIR) spectroscopy, BET surface area measurements, X-ray photoelectron spectroscopy (XPS), UV-vis-diffuse reflectance spectroscopy (UV-vis-DRS), temperature-programmed desorption of ammonia (NH<SUB>3</SUB>-TPD), and thermogravimetric (TG) analysis. The reaction tests were carried out in a continuous flow fixed-bed reactor at temperature ranging from 220 to 300<SUP>o</SUP>C. The conversion of H<SUB>2</SUB>S increased with increasing temperature for all PILCs while the selectivity to SO<SUB>2</SUB> remained almost constant. The good catalytic performance of the metal-oxide pillared clays may be due to the high surface area and the presence of Bronsted and Lewis acid sites.
Bineesh, Kanattukara Vijayan,Kim, Dong-Kyu,Kim, Moon-IL,Selvaraj, Manickam,Park, Dae-Won Royal Society of Chemistry 2011 Dalton transactions Vol.40 No.15
<P>A series of vanadia-doped iron-oxide-pillared clays (V/Fe-PILCs) with various amounts of vanadia were prepared and their performance for the selective catalytic oxidation of H<SUB>2</SUB>S was investigated. V/Fe-PILCs were characterized using X-ray diffraction (XRD), surface area- and pore volume measurements, chemical analysis, Fourier-transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and temperature-programmed reduction by H<SUB>2</SUB> (H<SUB>2</SUB>-TPR). V/Fe-PILCs showed better catalytic performance than Fe-PILC without any significant SO<SUB>2</SUB> emissions. The H<SUB>2</SUB>S conversion over V/Fe-PILCs increased with increasing vanadia content up to 7 wt.%. However, it decreased at higher vanadia loading due to the decrease in surface area and the formation of the crystalline V<SUB>2</SUB>O<SUB>5</SUB> phase. The presence of water vapor in the reactant mixture resulted in a decrease of H<SUB>2</SUB>S conversion.</P> <P>Graphic Abstract</P><P>Vanadia-doped iron-oxide-pillared clays (V/Fe-PILCs) were synthesized and used as efficient heterogeneous catalysts for the selective catalytic oxidation of H<SUB>2</SUB>S. <IMG SRC='http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/image/GA?id=c0dt01144d'> </P>
Bineesh, K.V.,Kim, M.i.,Lee, G.H.,Selvaraj, M.,Hyun, K.,Park, D.W. Korean Society of Industrial and Engineering Chemi 2012 Journal of industrial and engineering chemistry Vol.18 No.5
The catalytic oxidation of hydrogen sulfide in the presence of water and ammonia was studied over V<SUB>2</SUB>O<SUB>5</SUB> supported on Zr-pillared clay catalysts (V/Zr-PILCs). The synthesized catalysts were examined using a variety of characterization techniques. A catalytic performance study using V/Zr-PILC catalysts showed that H<SUB>2</SUB>S was successfully converted to elemental sulfur and ammonium thiosulfate (ATS) without considerable emission of sulfur dioxide. The H<SUB>2</SUB>S conversion over V/Zr-PILCs increased with increasing the content of vanadia up to 6wt.%. This superior catalytic performance might be related to the uniform dispersion of vanadia species on the Zr-PILC support.
Kanattukara Vijayan Bineesh,,Balasamy Rabindran Jermy,Sang-Yun Kim,박대원 한국공업화학회 2009 Journal of Industrial and Engineering Chemistry Vol.15 No.2
A series of vanadia-doped titania pillared clay (V/Ti-PILC) with various amounts of vanadia were prepared and their performance for the selective catalytic oxidation of H2S was investigated in this study. V/Ti-PILCs were characterized using X-ray diffraction (XRD), BET apparatus, and X-ray photoelectron spectroscopy (XPS). V/Ti-PILCs showed better catalytic performance than as such Ti-PILC at temperatures ranging from 220 to 300 ℃ without any considerable SO2 emission. The H2S conversion over V/Ti-PILC increased with increasing vanadia content up to 5 wt.%. This superior catalytic performance might be related to the uniform dispersion of vanadia in the formof monomeric and polymeric species. However, it decreased at 10 wt.% vanadia loading due to the decrease of surface area and to the formation of crystalline V2O5 phase. The presence ofwater vapor in the reactantmixture resulted in the decrease of the H2S conversion. 2009 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.
Kanattukara Vijayan Bineesh,Moon-il Kim,Goo-Hwa Lee,셀바라지,현규,박대원 한국공업화학회 2012 Journal of Industrial and Engineering Chemistry Vol.18 No.5
The catalytic oxidation of hydrogen sulfide in the presence of water and ammonia was studied over V2O5supported on Zr-pillared clay catalysts (V/Zr-PILCs). The synthesized catalysts were examined using a variety of characterization techniques. A catalytic performance study using V/Zr-PILC catalysts showed that H2S was successfully converted to elemental sulfur and ammonium thiosulfate (ATS) without considerable emission of sulfur dioxide. The H2S conversion over V/Zr-PILCs increased with increasing the content of vanadia up to 6 wt.%. This superior catalytic performance might be related to the uniform dispersion of vanadia species on the Zr-PILC support.
Synthesis of metal-oxide pillared montmorillonite clay for the selective catalytic oxidation of H2S
Kanattukara Vijayan Bineesh,,Dong-Kyu Kim,Han-Jun Cho,박대원 한국공업화학회 2010 Journal of Industrial and Engineering Chemistry Vol.16 No.4
In the present work, titania-pillared clay (Ti-PILC) and zirconia-pillared clay (Zr-PILC) were synthesized,and their catalytic performance was studied for the selective oxidation of H2S to elemental sulfur. The obtained pillared clays (PILCs) were characterized by X-ray fluorescence spectroscopy (XRF), infrared (FTIR) spectroscopy, BET surface area measurements, X-ray photoelectron spectroscopy (XPS), UV–visdiffuse reflectance spectroscopy (UV–vis-DRS), temperature-programmed desorption of ammonia (NH3-TPD), and thermogravimetric (TG) analysis. The reaction tests were carried out in a continuous flow fixed-bed reactor at temperature ranging from 220 to 300 8C. The conversion of H2S increased with increasing temperature for all PILCs while the selectivity to SO2 remained almost constant. The good catalytic performance of the metal-oxide pillared clays may be due to the high surface area and the presence of Bro¨nsted and Lewis acid sites.
Balasamy Rabindran Jermy,Sang-Yun Kim,Kanattukara Vijayan Bineesh,셀바라지,Seung-Kug Song,Jong-Woo Ryu,박대원 한국화학공학회 2009 Korean Journal of Chemical Engineering Vol.26 No.5
The direct incorporation of vanadium into the three-dimensional (3-D) cubic Ia3d mesostructure designated as V-KIT-6 was prepared, and the material obtained therein showed a very high specific surface area of ~1,000㎡/g with tunable pore diameters in a narrow distribution of sizes, ~5.7 to 6.0 nm. The coordination and nature of the V sites in V-KIT-6 were characterized by 51V-spin-echo NMR analysis. It shows that after calcination, the V4+ species are totally oxidized to the V5+ state with 4- and 6-coordinated V-O environments in a highly dispersed state with much less crystalline V2O5 formation. The calcined V-KIT-6 materials showed excellent catalytic activity in the direct oxidation of styrene using tert-butyl hydroperoxide (TBHP) as an oxidant.