Silica gel and MCM-41 synthesized mesoporous materials were treated with either oxygen(O_2),hexamethyldisiloxane(HMDSO) and organic vapors like ethanol(Et OH),and acrylonitrile(AN)inductive plasma.The radiofre...Silica gel and MCM-41 synthesized mesoporous materials were treated with either oxygen(O_2),hexamethyldisiloxane(HMDSO) and organic vapors like ethanol(Et OH),and acrylonitrile(AN)inductive plasma.The radiofrequency power for the modification was fixed to 120 W and30 min,assuring a high degree of organic ionization energy in the plasma.The surface properties were studied by infrared spectroscopy(FTIR),scanning electron microscopy,x-ray photoelectron spectroscopy and dynamic light scattering technique was used for characterizing size distributions.When the silica and MCM-41 particles were modified by AN and HMDSO plasma gases,the surface morphology of the particles was changed,presenting another color,size or shape.In contrast,the treatments of oxygen and Et OH did not affect the surface morphology of both particles,but increased the oxygen content at the surface bigger than the AN and HMDSO plasma treatments.In this study,we investigated the influence of different plasma treatments on changes in morphology and the chemical composition of the modified particles which render them a possible new adsorbent for utilization in sorptive extraction techniques for polar compounds.展开更多
TiO2 grafted silica MCM-41 catalyst with and without sulfate treatment were prepared. The structural and acid properties of these materials were investigated by XRD, N2 adsorption-desorption, element analysis, thermal...TiO2 grafted silica MCM-41 catalyst with and without sulfate treatment were prepared. The structural and acid properties of these materials were investigated by XRD, N2 adsorption-desorption, element analysis, thermal analysis, Raman and FTIR measurements. Their acid-catalytic activities were evaluated using the cyclization reaction of pseudoionone. It was found that the obtained materials possess well-ordered mesostructure, and the grafted TiO2 components were in highly dispersed amorphous form. T/MCM41 without sulfation contained only Lewis acid sites, while Brφnsted and Lewis acidities were remarkably improved for the sulfated materials ST/MCM41 and d-ST/MCM41. T/MCM-41 was not active for the cyclization reaction of pseudoionone, but ST/MCM-41 and d-ST/MCM-41 possessed favorable catalytic activities. The catalytic performance of ST/MCM-41 was comparable with that of the commercial solid acid catalyst of Amberlyst-15, and better than that of d-ST/MCM-41, although the latter underwent a second TiO2 grafting process and accordingly had higher Ti and S content. The specific surface structure of Si-O-Ti-O-S=O in ST/MCM-41 and the bilateral induction effect of Si and S=O on Si-O-Ti bonds were speculated to account for its higher acid catalytic activity.展开更多
Silica sources influence different aspects of Al-MCM-41 product. The crystallinity of nanosized Al-MCM-41 zeolites prepared crystallization and lead to change in the properties of the final from precursors mixtures co...Silica sources influence different aspects of Al-MCM-41 product. The crystallinity of nanosized Al-MCM-41 zeolites prepared crystallization and lead to change in the properties of the final from precursors mixtures containing different silica sources, e.g. tetraethylorthosilicate (TEOS), colloidal silica (CS), silicic acid (SA) and fumed silica (FS) have been studied. The produced samples are investigated using XRD, SEM, FT-IR, pyridine adsorption and N2 physisorption. XRD results show that the products obtained from different silica sources are in Al-MCM-41 phase. SEM results show that silica sources influence the produced Al-MCM-41 shape. Using silicic acid leads to formation of spherical crystals, TEOS gives cubical crystals, colloidal silica forms spherical crystals with smaller aggregated, and fumed silica gives rounded crystals. N2 physisorption results show that silica sources influence pore-diameter and pore-volume of the produced Al-MCM-41 ; the pore diameter of the produced Al-MCM-41 in case of colloidal silica, TEOS, fumed silica, and silicic acid are 12, 20, 15, and 17A respectively. Also, the pore volume of the produced AI-MCM-41 in case of colloidal silica, TEOS, fumed silica and silicic acid are 0.78, 0.71, 0.76, and 0.8 cm^3/gm, respectively.展开更多
A convenient and economic method for preparing highly ordered MCM 41 was studied in an open vessel by using waterglass as the silicon source. XRD, nitrogen adsorption and TEM show that the product has a highly ordered...A convenient and economic method for preparing highly ordered MCM 41 was studied in an open vessel by using waterglass as the silicon source. XRD, nitrogen adsorption and TEM show that the product has a highly ordered structure and the hexagonal arrangements of uniformly size pores distribution.展开更多
It was proved by ICP, fluorescence spectra and N 2 adsorption that the rare earth complex [C 5H 5NC 16H 33] [Eu(TTA) 4] is in the channel of Si-MCM-41 in the course of assembly. The rare earth complex of 67.9% is in t...It was proved by ICP, fluorescence spectra and N 2 adsorption that the rare earth complex [C 5H 5NC 16H 33] [Eu(TTA) 4] is in the channel of Si-MCM-41 in the course of assembly. The rare earth complex of 67.9% is in the channel, suggesting that the assembly of the complex molecular on the mesoporous MCM-41 was carried out mainly in the channel.展开更多
基金supported by CONACYT Ciencia Básica project 176544SEM and XPS measurements were performed at LANNBIO Cinvestav Mérida,under support from projects FOMIX-Yucatán 2008-108160,CONACYT LAB2009-01 No.123913
文摘Silica gel and MCM-41 synthesized mesoporous materials were treated with either oxygen(O_2),hexamethyldisiloxane(HMDSO) and organic vapors like ethanol(Et OH),and acrylonitrile(AN)inductive plasma.The radiofrequency power for the modification was fixed to 120 W and30 min,assuring a high degree of organic ionization energy in the plasma.The surface properties were studied by infrared spectroscopy(FTIR),scanning electron microscopy,x-ray photoelectron spectroscopy and dynamic light scattering technique was used for characterizing size distributions.When the silica and MCM-41 particles were modified by AN and HMDSO plasma gases,the surface morphology of the particles was changed,presenting another color,size or shape.In contrast,the treatments of oxygen and Et OH did not affect the surface morphology of both particles,but increased the oxygen content at the surface bigger than the AN and HMDSO plasma treatments.In this study,we investigated the influence of different plasma treatments on changes in morphology and the chemical composition of the modified particles which render them a possible new adsorbent for utilization in sorptive extraction techniques for polar compounds.
文摘TiO2 grafted silica MCM-41 catalyst with and without sulfate treatment were prepared. The structural and acid properties of these materials were investigated by XRD, N2 adsorption-desorption, element analysis, thermal analysis, Raman and FTIR measurements. Their acid-catalytic activities were evaluated using the cyclization reaction of pseudoionone. It was found that the obtained materials possess well-ordered mesostructure, and the grafted TiO2 components were in highly dispersed amorphous form. T/MCM41 without sulfation contained only Lewis acid sites, while Brφnsted and Lewis acidities were remarkably improved for the sulfated materials ST/MCM41 and d-ST/MCM41. T/MCM-41 was not active for the cyclization reaction of pseudoionone, but ST/MCM-41 and d-ST/MCM-41 possessed favorable catalytic activities. The catalytic performance of ST/MCM-41 was comparable with that of the commercial solid acid catalyst of Amberlyst-15, and better than that of d-ST/MCM-41, although the latter underwent a second TiO2 grafting process and accordingly had higher Ti and S content. The specific surface structure of Si-O-Ti-O-S=O in ST/MCM-41 and the bilateral induction effect of Si and S=O on Si-O-Ti bonds were speculated to account for its higher acid catalytic activity.
文摘Silica sources influence different aspects of Al-MCM-41 product. The crystallinity of nanosized Al-MCM-41 zeolites prepared crystallization and lead to change in the properties of the final from precursors mixtures containing different silica sources, e.g. tetraethylorthosilicate (TEOS), colloidal silica (CS), silicic acid (SA) and fumed silica (FS) have been studied. The produced samples are investigated using XRD, SEM, FT-IR, pyridine adsorption and N2 physisorption. XRD results show that the products obtained from different silica sources are in Al-MCM-41 phase. SEM results show that silica sources influence the produced Al-MCM-41 shape. Using silicic acid leads to formation of spherical crystals, TEOS gives cubical crystals, colloidal silica forms spherical crystals with smaller aggregated, and fumed silica gives rounded crystals. N2 physisorption results show that silica sources influence pore-diameter and pore-volume of the produced Al-MCM-41 ; the pore diameter of the produced Al-MCM-41 in case of colloidal silica, TEOS, fumed silica, and silicic acid are 12, 20, 15, and 17A respectively. Also, the pore volume of the produced AI-MCM-41 in case of colloidal silica, TEOS, fumed silica and silicic acid are 0.78, 0.71, 0.76, and 0.8 cm^3/gm, respectively.
文摘A convenient and economic method for preparing highly ordered MCM 41 was studied in an open vessel by using waterglass as the silicon source. XRD, nitrogen adsorption and TEM show that the product has a highly ordered structure and the hexagonal arrangements of uniformly size pores distribution.
文摘It was proved by ICP, fluorescence spectra and N 2 adsorption that the rare earth complex [C 5H 5NC 16H 33] [Eu(TTA) 4] is in the channel of Si-MCM-41 in the course of assembly. The rare earth complex of 67.9% is in the channel, suggesting that the assembly of the complex molecular on the mesoporous MCM-41 was carried out mainly in the channel.