A versatile wet impregnation method was employed to conveniently and controllably deposit Fe_2O_3 nanoparticles on zeolites including commercial Y, mordenite and ZSM-5 with the similar framework Si/Al ratios and cryst...A versatile wet impregnation method was employed to conveniently and controllably deposit Fe_2O_3 nanoparticles on zeolites including commercial Y, mordenite and ZSM-5 with the similar framework Si/Al ratios and crystal sizes, respectively. The ultrafine Fe_2O_3 nanoparticles in size of 5 nm can be highly dispersed on zeolite Y matrix due to its much better wettability than ZSM-5 and mordenite. By using the obtained Fe_2O_3/zeolite composite as the heterogeneous Fenton-like catalysts, the degradation of phenol as a model reaction was systematically investigated, including the zeolite supports, particle size and dispersion of Fe_2O_3, and reaction conditions of H_2O_2 concentration, temperature, and pH value. The catalyst based on zeolite Y with Fe loading of 9% exhibited the best phenol degradation efficiency (> 90%)in neutral pH within 2 h. Its high catalytic activity in Fenton reaction can be attributed to the bifunctional properties of strong surface BrФnsted acidity and high reactivity of octahedral Fe^(3+) in the highlydispersed ultrafine Fe_2O_3 nanoparticles in size of 5 nm, which were the primary active centers to quickly decompose H_2O_2 into hydroxyl radicals. Since phenol degradation can be performed under mild conditions of ambient temperature (283-323 K) and a wide pH range (4.0-7.0), the catalysts can be easily recovered for recyclable use with stable degradation activity, which own the immense potential in deep treatment of organic pollutants in industrial wastewater.展开更多
Mesoporous superacids S2O82–-Fe2O3/SBA-15(SFS)with active nanoparticles are prepared by ultrasonic adsorption method.This method is adopted to ensure a homo-dispersed nanoparticle active phase,large specific surface ...Mesoporous superacids S2O82–-Fe2O3/SBA-15(SFS)with active nanoparticles are prepared by ultrasonic adsorption method.This method is adopted to ensure a homo-dispersed nanoparticle active phase,large specific surface area and many acidic sites.Compared with bulk S2O82–-Fe2O3,Br?nsted acid catalysts and other reported catalysts,SFS with an Fe2O3 loading of 30%(SFS-30)exhibits an outstanding activity in the probe reaction of alcoholysis of styrene oxide by methanol with 100%yield.Moreover,SFS-30 also shows a more excellent catalytic performance than bulk S2O82–-Fe2O3 towards the alcoholysis of other ROHs(R=C2H5-C4H9).Lewis and Bronsted acid sites on the SFS-30 surfaces are confirmed by pyridine adsorbed infrared spectra.The highly efficient catalytic activity of SFS-30 may be attributed to the synergistic effect from the nano-effect of S2O82–-Fe2O3 nanoparticles and the mesostructure of SBA-15.Finally,SFS-30 shows a good catalytic reusability,providing an 84.1%yield after seven catalytic cycles.展开更多
A magnetic sensor for detection of Pb^2＋ has been developed based on Fe/Fe3O4 nanoparticles modified by3-（3,4-dihydroxyphenyl）propionic acid（DHCA）. The carboxyl groups of DHCA have a strong affinity to coordinati...A magnetic sensor for detection of Pb^2＋ has been developed based on Fe/Fe3O4 nanoparticles modified by3-（3,4-dihydroxyphenyl）propionic acid（DHCA）. The carboxyl groups of DHCA have a strong affinity to coordination behavior of Pb^2＋ thus inducing the transformation of Fe/Fe3O4 nanoparticles from a dispersed to an aggregated state with a corresponding decrease, then increase in transverse relaxation time（T2） of the surrounding water protons. Upon addition of the different concentrations of Pb^2＋ to an aq. solution of DHCA functionalized Fe/Fe3O4 nanoparticles（DHCA-Fe/Fe3O4 NPs）（[Fe] = 90 mmol/L）, the change of T2 values display a good linear relationship with the concentration of Pb^2＋ from 40 μmol/L to 100 μmol/L and from 130 μmol/L to 200 μmol/L, respectively. Owing to the especially strong interaction between DHCA and Pb^2＋, DHCA-Fe/Fe3O4 NPs exhibited a high selectivity over other metal ions.展开更多
Ultrafine Y（OH）3 nanoparticles were successfully deposited from an additive-free 0.005 mol/L YCl3 low-temperature bath on the steel cathode at the current density of 0.5 mA/cm2 and bath temperature of 10 oC. Heat tr...Ultrafine Y（OH）3 nanoparticles were successfully deposited from an additive-free 0.005 mol/L YCl3 low-temperature bath on the steel cathode at the current density of 0.5 mA/cm2 and bath temperature of 10 oC. Heat treatment of the prepared Y（OH）3 nanoparticles at 600 oC in air led to the formation of Y2O3 nanoparticles. Thermal behavior and phase transformation during the heat treatment of Y（OH）3 were investigated by differential scanning calorimetry （DSC） and thermogramimetric analysis （TGA）. The morphologies, crystal structures and compositions of the prepared materials were examined by means of scanning and transmission electron microscopy （SEM and TEM） as well as X-ray diffraction （XRD） and FT-IR spectroscopy. The results showed that the prepared Y（OH）3 nanoparticles was essentially amorphous and composed of well dispersed ultrafine particles with size of 4 nm. After heat treatment, the obtained oxide product was well crystallized cubic phase of Y2O3 nanoparticles with the grain size of around 5 nm. It was concluded that low-temperature cathodic electrodeposition offered a facile and feasible way for preparation of ultrafine Y（OH）3 and Y2O3 nanoparticles.展开更多
Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate （SDBS） as surfactant. Eu-doped α-Ga2O3 and β-Ga2O3 were further fabricated by annealing G...Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate （SDBS） as surfactant. Eu-doped α-Ga2O3 and β-Ga2O3 were further fabricated by annealing GaOOH：Eu and then characterized by X-ray diffraction（XRD）, transmission electron microscopy （TEM） and photoluminescence （PL）. The TEM results show that monodisperse Eu^3＋-doped GaOOH nanoparticles form and then transform into Eu^3＋-doped a-Ga2O3 and β-Ga2O3 through annealing the GaOOH：Eu nanoparticles at 600 and 900℃, respectively. PL studies indicate that GaOOH：Eu has the highest intensity at 618 nm. Luminescence quenching is observed at higher Eu3＋concentration in all samples.展开更多
Using a liquid-solid phase inversion method, a hybrid matrix poly（vinylidene fluoride）（PVDF） membrane was prepared with alumina（Al2O3） nanoparticle addition. Pd/Fe nanoparticles（NPs） were successfully immobili...Using a liquid-solid phase inversion method, a hybrid matrix poly（vinylidene fluoride）（PVDF） membrane was prepared with alumina（Al2O3） nanoparticle addition. Pd/Fe nanoparticles（NPs） were successfully immobilized on the Al2O3/PVDF membrane, which was characterized by Scanning Electron Microscopy（SEM） and Transmission Electron Microscopy（TEM）. The micrographs showed that the Pd/Fe NPs were dispersed homogeneously. Several important experimental parameters were optimized, including the mechanical properties, contact angle and surface area of Al2O3/PVDF composite membranes with different Al2O3 contents. At the same time, the ferrous ion concentration and the effect of hydrophilization were studied. The results showed that the modified Al2O3/PVDF membrane functioned well as a support. The Al2O3/PVDF membrane with immobilized Pd/Fe NPs exhibited high efficiency in terms of dichloroacetic acid（DCAA） dechlorination. Additionally, a reaction pathway for DCAA dechlorination by Pd/Fe NPs immobilized on the Al2O3/PVDF membrane system was proposed.展开更多
Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studi...Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI（OH）3 sols are produced by using 0.1 mol/L Al（NO3）3·9H2O and 0.16 mol/L （NH4）2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%（volume fraction） surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.展开更多
A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous...A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous to crystal phase was about 850 ℃. The grain size was increased with the raising of calcine temperature. The alcohol-water ratio did not affect the formation of main crystal phases, but affected the agglomeration of nanoparticles based on the results of TEM. When alcohol-water ratio was 5∶1, the dispersion of nanoparticles was good. When there was not alcohol, the dispersion of nanoparticles was poor because there was only pure co-precipitation reaction and the speed of co-precipitation reaction was too high to have enough time of PEG. dispersing particles.展开更多
Attempts had been made to synthesize Al2O3-2SiO2 nanopowders by sol-gel method with tetraethoxysilane（TEOS） and aluminum nitrate（ANN） as the starting materials.DTS,TEM,SEM and BET were employed to study the effect...Attempts had been made to synthesize Al2O3-2SiO2 nanopowders by sol-gel method with tetraethoxysilane（TEOS） and aluminum nitrate（ANN） as the starting materials.DTS,TEM,SEM and BET were employed to study the effects of process parameters on the size,specific surface area and structure（morphology） of powders.The alkali-activation reactivity of the powders was tested for manufacturing geopolymers and their hydrothermal reactions were performed for fabricating zeolites.The results show that the optimum process parameters and drying method for preparing Al2O3-2SiO2 nanopowders are as follows：the molar ratio of water and ethanol to TEOS are 0：1 and 12：1 respectively at synthetic temperature of 50 ℃ and the drying method is azeotropic distillation with microwave drying.The average particle diameters of the powders were about 70 nm and the largest BET specific surface area was up to 669 m^2·g^-1.The compressive strength of the geopolymer and the calcium exchange capacity（by CaCO3） of NaA zeolite prepared with the powders reached to 29 MPa and 366 m^2·g^-1 respectively.展开更多
基金sponsored by Shanghai Pujiang Program, China (No. 16PJ1401100)the Shanghai Committee of Science and Technology, China (No.15ZR1402000)+3 种基金Key Basic Research Program of Science and Technology Commission of Shanghai Municipality (No. 17JC1400100)the NSF of China(No. 21673048)National Youth Top Talent Support Program of National High-Level Personnel of Special Support Program (Youth Top-notch Talent Support Program)the State Key Laboratory of Transducer Technology of China (No. SKT1503)
文摘A versatile wet impregnation method was employed to conveniently and controllably deposit Fe_2O_3 nanoparticles on zeolites including commercial Y, mordenite and ZSM-5 with the similar framework Si/Al ratios and crystal sizes, respectively. The ultrafine Fe_2O_3 nanoparticles in size of 5 nm can be highly dispersed on zeolite Y matrix due to its much better wettability than ZSM-5 and mordenite. By using the obtained Fe_2O_3/zeolite composite as the heterogeneous Fenton-like catalysts, the degradation of phenol as a model reaction was systematically investigated, including the zeolite supports, particle size and dispersion of Fe_2O_3, and reaction conditions of H_2O_2 concentration, temperature, and pH value. The catalyst based on zeolite Y with Fe loading of 9% exhibited the best phenol degradation efficiency (> 90%)in neutral pH within 2 h. Its high catalytic activity in Fenton reaction can be attributed to the bifunctional properties of strong surface BrФnsted acidity and high reactivity of octahedral Fe^(3+) in the highlydispersed ultrafine Fe_2O_3 nanoparticles in size of 5 nm, which were the primary active centers to quickly decompose H_2O_2 into hydroxyl radicals. Since phenol degradation can be performed under mild conditions of ambient temperature (283-323 K) and a wide pH range (4.0-7.0), the catalysts can be easily recovered for recyclable use with stable degradation activity, which own the immense potential in deep treatment of organic pollutants in industrial wastewater.
文摘Mesoporous superacids S2O82–-Fe2O3/SBA-15(SFS)with active nanoparticles are prepared by ultrasonic adsorption method.This method is adopted to ensure a homo-dispersed nanoparticle active phase,large specific surface area and many acidic sites.Compared with bulk S2O82–-Fe2O3,Br?nsted acid catalysts and other reported catalysts,SFS with an Fe2O3 loading of 30%(SFS-30)exhibits an outstanding activity in the probe reaction of alcoholysis of styrene oxide by methanol with 100%yield.Moreover,SFS-30 also shows a more excellent catalytic performance than bulk S2O82–-Fe2O3 towards the alcoholysis of other ROHs(R=C2H5-C4H9).Lewis and Bronsted acid sites on the SFS-30 surfaces are confirmed by pyridine adsorbed infrared spectra.The highly efficient catalytic activity of SFS-30 may be attributed to the synergistic effect from the nano-effect of S2O82–-Fe2O3 nanoparticles and the mesostructure of SBA-15.Finally,SFS-30 shows a good catalytic reusability,providing an 84.1%yield after seven catalytic cycles.
基金supported by National Natural Science Foundation of China (Nos. 21271130 and 21371122)Shanghai Science and Technology Development Fund (Nos. 12ZR1421800 and 13520502800)International Joint Laboratory on Resource Chemistry (IJLRC)
文摘A magnetic sensor for detection of Pb^2＋ has been developed based on Fe/Fe3O4 nanoparticles modified by3-（3,4-dihydroxyphenyl）propionic acid（DHCA）. The carboxyl groups of DHCA have a strong affinity to coordination behavior of Pb^2＋ thus inducing the transformation of Fe/Fe3O4 nanoparticles from a dispersed to an aggregated state with a corresponding decrease, then increase in transverse relaxation time（T2） of the surrounding water protons. Upon addition of the different concentrations of Pb^2＋ to an aq. solution of DHCA functionalized Fe/Fe3O4 nanoparticles（DHCA-Fe/Fe3O4 NPs）（[Fe] = 90 mmol/L）, the change of T2 values display a good linear relationship with the concentration of Pb^2＋ from 40 μmol/L to 100 μmol/L and from 130 μmol/L to 200 μmol/L, respectively. Owing to the especially strong interaction between DHCA and Pb^2＋, DHCA-Fe/Fe3O4 NPs exhibited a high selectivity over other metal ions.
文摘Ultrafine Y（OH）3 nanoparticles were successfully deposited from an additive-free 0.005 mol/L YCl3 low-temperature bath on the steel cathode at the current density of 0.5 mA/cm2 and bath temperature of 10 oC. Heat treatment of the prepared Y（OH）3 nanoparticles at 600 oC in air led to the formation of Y2O3 nanoparticles. Thermal behavior and phase transformation during the heat treatment of Y（OH）3 were investigated by differential scanning calorimetry （DSC） and thermogramimetric analysis （TGA）. The morphologies, crystal structures and compositions of the prepared materials were examined by means of scanning and transmission electron microscopy （SEM and TEM） as well as X-ray diffraction （XRD） and FT-IR spectroscopy. The results showed that the prepared Y（OH）3 nanoparticles was essentially amorphous and composed of well dispersed ultrafine particles with size of 4 nm. After heat treatment, the obtained oxide product was well crystallized cubic phase of Y2O3 nanoparticles with the grain size of around 5 nm. It was concluded that low-temperature cathodic electrodeposition offered a facile and feasible way for preparation of ultrafine Y（OH）3 and Y2O3 nanoparticles.
基金Project(50772133) supported by the National Natural Science Foundation of ChinaProject(LA 09014) supported by Innovation Projects for Graduates of Center South University,China
文摘Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate （SDBS） as surfactant. Eu-doped α-Ga2O3 and β-Ga2O3 were further fabricated by annealing GaOOH：Eu and then characterized by X-ray diffraction（XRD）, transmission electron microscopy （TEM） and photoluminescence （PL）. The TEM results show that monodisperse Eu^3＋-doped GaOOH nanoparticles form and then transform into Eu^3＋-doped a-Ga2O3 and β-Ga2O3 through annealing the GaOOH：Eu nanoparticles at 600 and 900℃, respectively. PL studies indicate that GaOOH：Eu has the highest intensity at 618 nm. Luminescence quenching is observed at higher Eu3＋concentration in all samples.
基金supported by the Nature Science Foundation of Heilongjiang Province (No. B201410)the Postdoctoral Foundation Project of Heilongjiang Province (No. LBH-Z13128)+3 种基金the Science and Technology Research Program of Education Bureau of Heilongjiang Province (No. 12531206)the Special Scientific Research Projects of Harbin Normal University (12XQXG02)the National Nature Science Foundation of China (No. 41030743)the National Nature Science Foundation of China (No. 42171217)
文摘Using a liquid-solid phase inversion method, a hybrid matrix poly（vinylidene fluoride）（PVDF） membrane was prepared with alumina（Al2O3） nanoparticle addition. Pd/Fe nanoparticles（NPs） were successfully immobilized on the Al2O3/PVDF membrane, which was characterized by Scanning Electron Microscopy（SEM） and Transmission Electron Microscopy（TEM）. The micrographs showed that the Pd/Fe NPs were dispersed homogeneously. Several important experimental parameters were optimized, including the mechanical properties, contact angle and surface area of Al2O3/PVDF composite membranes with different Al2O3 contents. At the same time, the ferrous ion concentration and the effect of hydrophilization were studied. The results showed that the modified Al2O3/PVDF membrane functioned well as a support. The Al2O3/PVDF membrane with immobilized Pd/Fe NPs exhibited high efficiency in terms of dichloroacetic acid（DCAA） dechlorination. Additionally, a reaction pathway for DCAA dechlorination by Pd/Fe NPs immobilized on the Al2O3/PVDF membrane system was proposed.
文摘Highly pure active γ-Al2O3 nanoparticles were synthesized from aluminum nitrate and ammonium carbonate with a little surfactant by chemical precipitation method. The factors affecting the synthesis process were studied. The properties of γ-Al2O3 nanoparticles were characterized by DTA, XRD, BET, TEM, laser granularity analysis and impurity content analysis. The results show that the amorphous precursor AI（OH）3 sols are produced by using 0.1 mol/L Al（NO3）3·9H2O and 0.16 mol/L （NH4）2CO3·H2O reaction solutions, according to the volume ratio 1.33, adding 0.024%（volume fraction） surfactant PEG600, and reacting at 40℃, 1000 r/min stirring rate for 15min. Then, after stabilizing for 24 h, the precursors were extracted and filtrated by vacuum, washed thoroughly with deionized water and dehydrated ethanol, dried in vacuum at 80℃ for 8h, final calcined at 800℃ for 1h in the air, and high purity active γ-Al2O3 nanoparticles can be prepared with cubic in crystal system, OH^7-FD3M in space group, about 9 nm in crystal grain size, about 20 nm in particle size and uniform size distribution, 131.35 m^2/g in BET specific surface area, 7 - 11 nm in pore diameter, and not lower than 99.93% in purity.
基金The authors acknowledges the financial support of Tianjin University Youth FoundationTangshan Ceramics Limited
文摘A method of heating ethanol-aqueous salt solution combined with co-precipitation was used to synthesize Al2O3/ZrO2 nanoparticles. The analysis of DSC and XRD revealed that the transformation temperature from amorphous to crystal phase was about 850 ℃. The grain size was increased with the raising of calcine temperature. The alcohol-water ratio did not affect the formation of main crystal phases, but affected the agglomeration of nanoparticles based on the results of TEM. When alcohol-water ratio was 5∶1, the dispersion of nanoparticles was good. When there was not alcohol, the dispersion of nanoparticles was poor because there was only pure co-precipitation reaction and the speed of co-precipitation reaction was too high to have enough time of PEG. dispersing particles.
基金Supported by the National Natural Science Foundation of China (50962002,50602006)Opening Funds of State Key Laboratory of Chemical Resource Engineering of Beijing University of Chemical Technology (201008)
文摘Attempts had been made to synthesize Al2O3-2SiO2 nanopowders by sol-gel method with tetraethoxysilane（TEOS） and aluminum nitrate（ANN） as the starting materials.DTS,TEM,SEM and BET were employed to study the effects of process parameters on the size,specific surface area and structure（morphology） of powders.The alkali-activation reactivity of the powders was tested for manufacturing geopolymers and their hydrothermal reactions were performed for fabricating zeolites.The results show that the optimum process parameters and drying method for preparing Al2O3-2SiO2 nanopowders are as follows：the molar ratio of water and ethanol to TEOS are 0：1 and 12：1 respectively at synthetic temperature of 50 ℃ and the drying method is azeotropic distillation with microwave drying.The average particle diameters of the powders were about 70 nm and the largest BET specific surface area was up to 669 m^2·g^-1.The compressive strength of the geopolymer and the calcium exchange capacity（by CaCO3） of NaA zeolite prepared with the powders reached to 29 MPa and 366 m^2·g^-1 respectively.
