A series of ZnO/SiO_(2) adsorbents were prepared by a sol-gel method using tetraethyl orthosilicate,ethylene glycol(EG)and nitrates as precursors.The effect of gel drying temperature on the structure and desulfurizati...A series of ZnO/SiO_(2) adsorbents were prepared by a sol-gel method using tetraethyl orthosilicate,ethylene glycol(EG)and nitrates as precursors.The effect of gel drying temperature on the structure and desulfurization performance of the adsorbents were investigated in detail.It is found that the low drying temperature led to a weak interaction among EG,Si AOH/H_(2)O and the nitrates in the gel system,which caused the oxidation of EG by NO3-and formed zinc glyoxylate complex during the gel calcination process,whereas this oxidation process also occurred at a high drying temperature during the gel drying process.The formed zinc glyoxylate complex promoted the generation of monodentate carbonate on the surface of Zn O,which resulted in the inferior desulfurization performance of adsorbents despite they have smaller Zn O nanoparticles.The gel dried at 120°C formed the hydrogen bonds between EG and Si AOH/H_(2)O and a strong interaction between zinc oxo-clusters and NO3-was also found in the gel system,which avoided the oxidation of EG by NO3-during the preparation process and the Zn O nanoparticles with sizes of 6 nm were formed by a combustion method.The adsorbent affords a highest sulfur capacity of 104.9 mg·g^(-1) in this case.In addition,the gel drying temperature has a significant influence on the textural properties of the adsorbents except their surface area.展开更多
Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary...Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200 ℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.展开更多
A series of TiO 2-MoO 3 nano-composite photocatalysts were prepared by supercritical fluid dry method(SCFD) and an impregnation technique with TiCl 4 and (NH 4) 6Mo 7O 24 ·4H 2O as the starting materia...A series of TiO 2-MoO 3 nano-composite photocatalysts were prepared by supercritical fluid dry method(SCFD) and an impregnation technique with TiCl 4 and (NH 4) 6Mo 7O 24 ·4H 2O as the starting materials. The catalysts were characterized by the means of XRD, TEM and UV-Vis. Methyl orange was used as model compound for the evaluation of their catalytic activities. The results indicated that the photo-catalyst prepared by SCFD had the advantages of small size(12.84 nm), narrow distribution and good dispersivity. The presence of small amount of Mo in composite catalyst gives rise to the red shift of its absorbance wavelength, decrease of its energy gap and increase of the utility of visible light. Furthermore, higher surface acidity of the photo-catalyst was obtained as the result of the addition of MoO 3. Compared with pure TiO 2, the catalytic activity of the TiO 2-MoO 3 nano-composite photo-catalyst was improved significantly. As the doping concentration of the composite catalysts was controlled at 0.6%(molar percentage), 100% degradation of methyl orange was achieved with in 1.2 h irradiation time.展开更多
Herein,N-Ti3C2@CNT microspheres are successfully synthesized by the simple spray drying method.In the preparation process,HCl-treated melamine(HTM)is selected as the sources of carbon and nitrogen.It not only realizes...Herein,N-Ti3C2@CNT microspheres are successfully synthesized by the simple spray drying method.In the preparation process,HCl-treated melamine(HTM)is selected as the sources of carbon and nitrogen.It not only realizes in situ growth of CNTs on the surface of MXene nanosheets with the catalysis of Ni,but also introduces efficient N-doping in both MXene and CNTs.Within the microsphere,MXene nanosheets interconnect with CNTs to form porous and conductive network.In addition,N-doped MXene and CNTs can provide strong chemical immobilization for polysulfides and effectively entrap them within the porous microspheres.Above-mentioned merits enable N-Ti3C2@CNT microspheres to be ideal sulfur host.When used in lithium–sulfur(Li–S)battery,the N-Ti3C2@CNT microspheres/S cathode delivers initial specific capacity of 927 mAh g−1 at 1 C and retains high capacity of 775 mAh g−1 after 1000 cycles with extremely low fading rate(FR)of 0.016%per cycle.Furthermore,the cathode still shows high cycling stability at high C-rate of 4 C(capacity of 647 mAh g−1 after 650 cycles,FR 0.027%)and high sulfur loading of 3 and 6 mg cm−2 for Li–S batteries.展开更多
A series of TiO2-SnO2 nano-sized composite photo-catalysts containing Sn (9.3%-30.1%) were prepared from TiCI4 and SnCl4·5H2O by using sol-gel, supercritical fluid dry and solid-phase reaction (SCFD) combination ...A series of TiO2-SnO2 nano-sized composite photo-catalysts containing Sn (9.3%-30.1%) were prepared from TiCI4 and SnCl4·5H2O by using sol-gel, supercritical fluid dry and solid-phase reaction (SCFD) combination technology. Characterizations with X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier Transform Infrared Spectroscopy (FTIR) showed that, in addition to anatase type TiO2, a new active phase (Ti, Sn)O2 (with particle size of 2.0-4.3 nm) formed, and there were no SnO2 crystals observed in the range of the doping concentration studied. Photo-catalytic reaction of phenol was used as a model reaction to evaluate the catalytic activities of the obtained catalysts. Compared with pure TiO2 or Ti-Sn catalyst prepared with general sol-gel method, Ti-Sn nano-composite photo-catalyst thus obtained showed significant improvement in catalytic activity. The photo-catalytic degradation rate of phenol could reach as high as 93.5% after 7 h. The preparation conditions of the new phase (Ti, Sn)O2 were investigated and its catalytic mechanism was proposed. The photo-catalytic particles prepared using SCFD combination technology exhibited small particle size, large surface area and high activity.展开更多
基金financially supported by the National Natural Science Foundation of China(22078223 and 21878209)Shanxi Province Science Foundation for Youths(20210302123065)。
文摘A series of ZnO/SiO_(2) adsorbents were prepared by a sol-gel method using tetraethyl orthosilicate,ethylene glycol(EG)and nitrates as precursors.The effect of gel drying temperature on the structure and desulfurization performance of the adsorbents were investigated in detail.It is found that the low drying temperature led to a weak interaction among EG,Si AOH/H_(2)O and the nitrates in the gel system,which caused the oxidation of EG by NO3-and formed zinc glyoxylate complex during the gel calcination process,whereas this oxidation process also occurred at a high drying temperature during the gel drying process.The formed zinc glyoxylate complex promoted the generation of monodentate carbonate on the surface of Zn O,which resulted in the inferior desulfurization performance of adsorbents despite they have smaller Zn O nanoparticles.The gel dried at 120°C formed the hydrogen bonds between EG and Si AOH/H_(2)O and a strong interaction between zinc oxo-clusters and NO3-was also found in the gel system,which avoided the oxidation of EG by NO3-during the preparation process and the Zn O nanoparticles with sizes of 6 nm were formed by a combustion method.The adsorbent affords a highest sulfur capacity of 104.9 mg·g^(-1) in this case.In addition,the gel drying temperature has a significant influence on the textural properties of the adsorbents except their surface area.
基金Project (5JJ30103) supported by the Natural Science Foundation of Hunan Province, China
文摘Ammonium aluminum carbonate hydroxide (AACH) precursor was synthesized by the precipitation reaction of aluminum sulfate and ammonium carbonate. Then the precursor was dealt with five drying methods including ordinary drying, alcohol exchange, vacuum freeze-drying, glycol distillation, n-butanol azeotropic distillation respectively and calcined at 1 200 ℃ for 2 h to get α-Al2O3. The effects of drying methods on preparation of nanometer α-Al2O3 were discussed, and the optimal drying method was confirmed. The structural properties of powders were characterized by XRD, SEM and BET measurements. The results show that vacuum freeze-drying, glycol distillation and n-butanol azeotropic distillation can prevent the powders from aggregating, and among them the n-butanol azeotropic distillation is the best method. The nanometer α-Al2O3 powder with non-aggregation can be manufactured using n-butanol azeotropic distillation and the average particle size is about 40 nm.
文摘A series of TiO 2-MoO 3 nano-composite photocatalysts were prepared by supercritical fluid dry method(SCFD) and an impregnation technique with TiCl 4 and (NH 4) 6Mo 7O 24 ·4H 2O as the starting materials. The catalysts were characterized by the means of XRD, TEM and UV-Vis. Methyl orange was used as model compound for the evaluation of their catalytic activities. The results indicated that the photo-catalyst prepared by SCFD had the advantages of small size(12.84 nm), narrow distribution and good dispersivity. The presence of small amount of Mo in composite catalyst gives rise to the red shift of its absorbance wavelength, decrease of its energy gap and increase of the utility of visible light. Furthermore, higher surface acidity of the photo-catalyst was obtained as the result of the addition of MoO 3. Compared with pure TiO 2, the catalytic activity of the TiO 2-MoO 3 nano-composite photo-catalyst was improved significantly. As the doping concentration of the composite catalysts was controlled at 0.6%(molar percentage), 100% degradation of methyl orange was achieved with in 1.2 h irradiation time.
文摘Herein,N-Ti3C2@CNT microspheres are successfully synthesized by the simple spray drying method.In the preparation process,HCl-treated melamine(HTM)is selected as the sources of carbon and nitrogen.It not only realizes in situ growth of CNTs on the surface of MXene nanosheets with the catalysis of Ni,but also introduces efficient N-doping in both MXene and CNTs.Within the microsphere,MXene nanosheets interconnect with CNTs to form porous and conductive network.In addition,N-doped MXene and CNTs can provide strong chemical immobilization for polysulfides and effectively entrap them within the porous microspheres.Above-mentioned merits enable N-Ti3C2@CNT microspheres to be ideal sulfur host.When used in lithium–sulfur(Li–S)battery,the N-Ti3C2@CNT microspheres/S cathode delivers initial specific capacity of 927 mAh g−1 at 1 C and retains high capacity of 775 mAh g−1 after 1000 cycles with extremely low fading rate(FR)of 0.016%per cycle.Furthermore,the cathode still shows high cycling stability at high C-rate of 4 C(capacity of 647 mAh g−1 after 650 cycles,FR 0.027%)and high sulfur loading of 3 and 6 mg cm−2 for Li–S batteries.
基金The authors thank the National Natural Scir nce Foun-dation of China(No.20076004)the National Development Project of High Technology(No.2001AA322030)the Doctoral Program of Higher Education(No.2000001005)for the financial support of this project.
文摘A series of TiO2-SnO2 nano-sized composite photo-catalysts containing Sn (9.3%-30.1%) were prepared from TiCI4 and SnCl4·5H2O by using sol-gel, supercritical fluid dry and solid-phase reaction (SCFD) combination technology. Characterizations with X-ray diffraction (XRD), transmission electron microscopy (TEM) and Fourier Transform Infrared Spectroscopy (FTIR) showed that, in addition to anatase type TiO2, a new active phase (Ti, Sn)O2 (with particle size of 2.0-4.3 nm) formed, and there were no SnO2 crystals observed in the range of the doping concentration studied. Photo-catalytic reaction of phenol was used as a model reaction to evaluate the catalytic activities of the obtained catalysts. Compared with pure TiO2 or Ti-Sn catalyst prepared with general sol-gel method, Ti-Sn nano-composite photo-catalyst thus obtained showed significant improvement in catalytic activity. The photo-catalytic degradation rate of phenol could reach as high as 93.5% after 7 h. The preparation conditions of the new phase (Ti, Sn)O2 were investigated and its catalytic mechanism was proposed. The photo-catalytic particles prepared using SCFD combination technology exhibited small particle size, large surface area and high activity.