CN101746825B - Organic solvent-water heating method for preparing football-shaped mesoporous BiVO4 - Google Patents

Organic solvent-water heating method for preparing football-shaped mesoporous BiVO4 Download PDF

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CN101746825B
CN101746825B CN2009102436461A CN200910243646A CN101746825B CN 101746825 B CN101746825 B CN 101746825B CN 2009102436461 A CN2009102436461 A CN 2009102436461A CN 200910243646 A CN200910243646 A CN 200910243646A CN 101746825 B CN101746825 B CN 101746825B
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organic solvent
mixed solution
ethanol
ethylene glycol
bivo
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CN101746825A (en
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戴洪兴
孟雪
张磊
蒋海燕
高京杰
张凯
何洪
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Beijing University of Technology
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Beijing University of Technology
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Abstract

The invention discloses an organic solvent-water heating method for preparing football-shaped mesoporous BiVO4, comprising the following experimental steps: under the condition of stirring, bismuth nitrate and ammonium metavanadate are dissolved in a mixed solution of ethanol, ethylene glycol, nitric acid and laurylamine (oleylamine or mixed liquid of oleylamine and oleic acid); a sodium hydroxide (2mol / L) alcohol solution of ethanol and ethylene glycol with the volume ratio of 1 to 1 is used to regulate the pH of the solution to be equal to 1.5-3; the mixed solution is transferred in a stainless steel self-pressing vessel (the volume filling degree is about 70%) with a Teflon inner liner and is put in an incubator to carry out organic solvent - water heating treatment for 12h in constant temperature of 100 DEG C; and the mixed solution is naturally cooled to room temperature after taking out. The obtained product after the organic solvent - water heating treatment is filtered, is washed with deionized water and absolute ethanol and is dried for 12h at the temperature of 60 DEG C, and then football-shaped mesoporous BiVO4 micron particles with a monoclinic scheelite structure is obtained. The porous bismuth vanadate obtained by the method has good application prospects in the fields of photocatalysis, electrode materials, pigments, ion conductive ceramic, and the like.

Description

Mesoporous BiVO＜the sub of a kind of preparation American football shape〉4＜/sub organic solvent-hydrothermal method
Technical field
The present invention relates to a kind of specific morphology porous BiVO 4The preparation method of micron particle relates in particular to the mesoporous BiVO of American football shape of monocline scheelite-type structure 4Organic solvent-the hydrothermal method of micron particle.
Background technology
Pucherite is a kind of novel semiconductor material with visible light-responded ability, can be used as photocatalyst, ferroelasticity material, nontoxic yellow ultramarine, reversible thermochromic materials, electrode materials, ionic conductor material etc.In three kinds of crystalline structure of pucherite, the monocline scheelite-type structure demonstrates best photocatalysis performance.At present, can adopt solid phase method, sonochemical method, microwave method, hydrothermal method, the precipitator method to wait and prepare BiVO 4Studies show that BiVO 4Crystalline structure and particle morphology and pore structure its photocatalysis performance is had material impact.Therefore, the research and development preparation has the BiVO of monocline scheelite-type structure, specific morphology and vesicular structure 4Micron-particle is significant.
In recent years, people have explored some preparation BiVO 4Method.For example: with hexadecyl trimethylammonium bromide (CTAB) is template Bi 2O 3And NH 4VO 3For raw material can be prepared four directions bulk, sheet, flower-shaped BiVO under hydrothermal condition 4, its under radiation of visible light to catalytic activity of methyl orange degradation reaction be better than P25 (HB Li, et al.Mater.Chem.Phys., 2009,115:9-13).With Bi (NO 3) 35H 2O and NH 4VO 3Be presoma, pass through NaHCO 3Regulate the pH value, can obtain three-dimensional flower-shaped BiVO at 80 ℃ of hydro-thermal 30h 4(L Zhou, et al.Crystal Growth Design, 2008,8:728-733).With Bi (NO 3) 3And Na 3VO 4Be raw material, hydro-thermal makes the dendroid BiVO of monocline under acidic conditions 4, behind the radiation of visible light 45min, to the degradation rate of rhodamine B be higher than 90% (Y Zhao, et al.Chem.Eur.J., 2008,14:1601-1606).Be source metal, be the order mesoporous BiVO that hard template can be synthesized the monocline scheelite-type structure with Bismuth trinitrate and ammonium meta-vanadate with mesoporous silicon KIT-6 4, and adopt hydrothermal method can prepare the BiVO of monocline scheelite-type structure 4, the result shows that both all are higher than P25 to the degradation rate of methylene blue under radiation of visible light, and the degradation rate of order mesoporous methylene blue exceeds by hydrothermal method and makes BiVO 4On one times (G Li, et al.Chem.Mater., 2008,20:3983-3992).
In addition, manganese acetate can synthesize sheet, spherical and wire Mn with the mixed solution of being made up of oleyl amine, water and dimethylbenzene 90 ℃ of following reactions 3O 4(T Yu, et al.Chem.Mater., 2009,21:2272-2279).Under oleic acid or oleyl amine effect, can synthesize cubic and bar-shaped rare-earth oxide (T D Nguyen, et al.J.Phys.Chem.C, 2009,113:11204-11214).
Up to now, utilize amino dodecane, oleic acid or oleyl amine to synthesize BiVO 4Work do not appear in the newspapers as yet, also not having document and patent report to cross with amino dodecane, oleic acid and oleyl amine and ethanol and ethylene glycol mixing organism is the organic solvent-Hydrothermal Preparation specific morphology porous BiVO of solvent 4
Summary of the invention
The object of the present invention is to provide a kind of American football shape porous BiVO for preparing the monocline scheelite-type structure 4Organic solvent hydro-thermal method.
Under agitation condition, to volume ratio 5: 5: 1 ethanol: ethylene glycol: dense HNO 3In the mixed solution of (concentration is 67%), add amino dodecane or oleyl amine or oleyl amine and oleic mixed solution, to be mixed evenly after, add Bi (NO again 3) 35H 2O powder and NH 4VO 3Powder, wherein amino dodecane (or oleyl amine): Bi (NO 3) 3: NH 4VO 3: the mol ratio of nitric acid is 3: 1: 1: 8 or oleyl amine: oleic acid: Bi (NO 3) 3: NH 4VO 3: the nitric acid mol ratio is 15: 3: 5: continue stir after again with volume ratio be the pH=1.5-3 of 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution at 5: 40.With above-mentioned mixed solution be transferred to liner be the stainless steel of tetrafluoroethylene from pressing (the volume compactedness is 70%) in the still, and place thermostat container in 100 ℃ of organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief.The product that obtains is filtered, deionized water wash and absolute ethanol washing each 3 times, in 60 ℃ of dry 12h, in air atmosphere, rise to 400 ℃ of calcination 4h with the temperature rise rate of 1 ℃/min after, promptly obtain the American football shape porous BiVO of monocline scheelite-type structure 4Micron particle.
Characteristics such as the present invention has that raw material is cheap, technology is simple, target product particle morphology and crystal phase structure are controlled.
The present invention adopts with amino dodecane, oleic acid and oleyl amine and ethanol and ethylene glycol and is mixed solvent, is that source metal is carried out organic solvent-hydrothermal treatment consists under the highly basic condition with Bismuth trinitrate and ammonium meta-vanadate, the mesoporous BiVO of preparation American football shape 4Micron particle.Organic solvent amino dodecane, oleic acid and oleyl amine are forming the mesoporous BiVO of above specific morphology 4Micron particle plays an important role.
The mesoporous pucherite of the specific morphology that the present invention obtained has good application prospect in fields such as photochemical catalysis, electrode materials, pigment and ionic conductivity ceramics.
Utilize X-ray diffraction (XRD, D8 Advance), high resolution scanning electron microscope (HRSEM, Zeiss Supra 55) and ultraviolet-visible spectrum (UV-Vis, shimadzuUV2450) etc. technology is measured crystalline structure, surface topography and the photo absorption performance of gained target product respectively.The result shows, according to the mesoporous BiVO of the prepared American football shape of the inventive method 4Micron particle (long is 0.2-2 μ m, and wide is 0.1-1 μ m, and mean pore size is 20-50nm) has monocline scheelite-type structure and good visible light-responded ability.
Description of drawings
In order further to understand the present invention, elaborate with embodiment below, and provide accompanying drawing and describe monocline scheelite-type structure and the mesoporous BiVO of American football shape that the present invention obtains 4, wherein:
Fig. 1 is obtained BiVO 4The XRD spectra of sample, wherein curve (a) and (b), (c), (d), (e) and (f) be respectively the XRD spectra of embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 and embodiment 6 samples.
Fig. 2 is obtained BiVO 4The HRSEM photo of sample, wherein Fig. 2 (a), 2 (b), 2 (c), 2 (d), 2 (e) and 2 (f) are respectively the HRSEM photo of embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5 and embodiment 6 samples.
Fig. 3 (A) is obtained BiVO 4The UV-Vis spectrogram of sample, wherein curve (a) and (b), (c), (d), (e) and (f) be respectively the UV-Vis spectrogram of embodiment 1, embodiment 2, embodiment 3, embodiment 5, embodiment 6 and embodiment 4 samples, Fig. 3 (B) is the partial enlarged drawing of Fig. 3 (A).
Embodiment
Embodiment 1: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3(cumulative volume is 55mL) adds the 30mmol amino dodecane in the mixed solution of (concentration is 67wt%), to be mixed evenly after, add 10mmol Bi (NO again 3) 35H 2O powder and 10mmolNH 4VO 3Powder, with volume ratio is that 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution pH are 1.5, it is that the stainless steel of tetrafluoroethylene is from pressing (the volume compactedness is 70%) in the still that above-mentioned mixed solution is transferred to the 100mL liner, and place thermostat container in 100 ℃ of constant temperature organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains after organic solvent-hydrothermal treatment consists is filtered, use deionized water wash 3 times and absolute ethanol washing 3 times respectively, in 60 ℃ of dry 12h, speed with 1 ℃/min is warming up to 400 ℃, roasting 4h obtains the mesoporous BiVO of American football shape of monocline scheelite-type structure to remove template 4Micron particle (long is 0.5-2 μ m, and wide is 0.2-1 μ m, and mean pore size is 20-50nm), its absorbing boundary is 522nm.Its XRD spectra is seen Fig. 1 (a), and the HRSEM photo is seen Fig. 2 (a), and the UV-Vis spectrogram is seen Fig. 3 (a).
Embodiment 2: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3(cumulative volume is 55mL) adds the 30mmol amino dodecane in the mixed solution of (concentration is 67%), to be mixed evenly after, add 10mmol Bi (NO again 3) 35H 2O powder and 10mmolNH 4VO 3Powder, with volume ratio is that 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution pH are 3, it is that the stainless steel of tetrafluoroethylene is from pressing (the volume compactedness is about 70%) in the still that above-mentioned mixed solution is transferred to the 100mL liner, and place thermostat container in 100 ℃ of constant temperature organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains after organic solvent-hydrothermal treatment consists is filtered, use deionized water wash 3 times and absolute ethanol washing 3 times respectively, in 60 ℃ of dry 12h, speed with 1 ℃/min is warming up to 400 ℃, roasting 4h obtains the mesoporous BiVO of American football shape of monocline scheelite-type structure to remove template 4Micron particle (long is 0.2-1 μ m, and wide is 0.1-1 μ m, and mean pore size is 20-40nm), its absorbing boundary is 525nm.Its XRD spectra is seen Fig. 1 (b), and the HRSEM photo is seen Fig. 2 (b), and the UV-Vis spectrogram is seen Fig. 3 (b)
Embodiment 3: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3(cumulative volume is 55mL) adds the 30mmol oleyl amine in the mixed solution of (concentration is 67%), to be mixed evenly after, add 10mmol Bi (NO again 3) 35H 2O powder and 10mmolNH 4VO 3Powder, with volume ratio is that 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution pH are 1.5, it is that the stainless steel of tetrafluoroethylene is from pressing (the volume compactedness is about 70%) in the still that above-mentioned mixed solution is transferred to the 100mL liner, and place thermostat container in 100 ℃ of constant temperature organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains after organic solvent-hydrothermal treatment consists is filtered, use deionized water wash 3 times and absolute ethanol washing 3 times respectively, in 60 ℃ of dry 12h, speed with 1 ℃/min is warming up to 400 ℃, roasting 4h obtains the mesoporous BiVO of American football shape of monocline scheelite-type structure to remove template 4Micron particle (long is 0.2-1 μ m, and wide is 0.1-1 μ m, and mean pore size is 20-50nm), its absorbing boundary is 526nm.Its XRD spectra is seen Fig. 1 (c), and the HRSEM photo is seen Fig. 2 (c), and the UV-Vis spectrogram is seen Fig. 3 (c).
Embodiment 4: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3(cumulative volume is 55mL) adds the 30mmol oleyl amine in the mixed solution of (concentration is 67%), to be mixed evenly after, add 10mmol Bi (NO again 3) 35H 2O powder and 10mmolNH 4VO 3Powder, with volume ratio is that 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution pH are 3, it is that the stainless steel of tetrafluoroethylene is from pressing (the volume compactedness is about 70%) in the still that above-mentioned mixed solution is transferred to the 100mL liner, and place thermostat container in 100 ℃ of constant temperature organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains after organic solvent-hydrothermal treatment consists is filtered, use deionized water wash 3 times and absolute ethanol washing 3 times respectively, in 60 ℃ of dry 12h, speed with 1 ℃/min is warming up to 400 ℃, roasting 4h obtains the mesoporous BiVO of American football shape of monocline scheelite-type structure to remove template 4Micron particle (long is 0.1-0.5 μ m, and wide is 0.05-0.2 μ m, and mean pore size is 20-50nm), its absorbing boundary is 511nm.Its XRD spectra is seen Fig. 1 (d), and the HRSEM photo is seen Fig. 2 (d), and the UV-Vis spectrogram is seen Fig. 3 (f)
Embodiment 5: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3(cumulative volume is 55mL) adds 30mmol oleyl amine and 6mmol oleic acid in the mixed solution of (concentration is 67%), to be mixed evenly after, add 10mmol Bi (NO again 3) 35H 2O powder and 10mmol NH 4VO 3Powder, with volume ratio is that 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution pH are 1.5, it is that the stainless steel of tetrafluoroethylene is from pressing (the volume compactedness is about 60%) in the still that above-mentioned mixed solution is transferred to the 100mL liner, and place thermostat container in 100 ℃ of constant temperature organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains after organic solvent-hydrothermal treatment consists is filtered, use deionized water wash 3 times and absolute ethanol washing 3 times respectively, in 60 ℃ of dry 12h, speed with 1 ℃/min is warming up to 400 ℃, roasting 4h obtains the mesoporous BiVO of American football shape of monocline scheelite-type structure to remove template 4Micron particle (long is 0.2-1 μ m, and wide is 0.1-0.5 μ m, and mean pore size is 20-50nm), its absorbing boundary is 519nm.Its XRD spectra is seen Fig. 1 (e), and the HRSEM photo is seen Fig. 2 (e), and the UV-Vis spectrogram is seen Fig. 3 (d)
Embodiment 6: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3(cumulative volume is 55mL) adds 30mmol oleyl amine and 6mmol oleic acid in the mixed solution of (concentration is 67%), to be mixed evenly after, add 10mmol Bi (NO again 3) 35H 2O powder and 10mmol NH 4VO 3Powder, with volume ratio is that 1: 1 ethanol and the sodium hydroxide of ethylene glycol (2mol/L) alcoholic solution regulator solution pH are 3, it is that the stainless steel of tetrafluoroethylene is from pressing (the volume compactedness is about 70%) in the still that above-mentioned mixed solution is transferred to the 100mL liner, and place thermostat container in 100 ℃ of constant temperature organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains after organic solvent-hydrothermal treatment consists is filtered, use deionized water wash 3 times and absolute ethanol washing 3 times respectively, in 60 ℃ of dry 12h, speed with 1 ℃/min is warming up to 400 ℃, roasting 4h obtains the mesoporous BiVO of American football shape of monocline scheelite-type structure to remove template 4Micron particle (long is 0.2-0.4 μ m, and wide is 0.05-0.2 μ m, and mean pore size is 20-50nm), its absorbing boundary is 513nm.Its XRD spectra is seen Fig. 1 (f), and the HRSEM photo is seen Fig. 2 (f), and the UV-Vis spectrogram is seen Fig. 3 (e).

Claims (1)

1. one kind prepares the mesoporous BiVO of American football shape 4Organic solvent-hydrothermal method, it is characterized in that, may further comprise the steps: under agitation condition, be 5: 5: 1 ethanol to volume ratio: ethylene glycol: dense HNO 3Mixed solution in add amino dodecane or oleyl amine or oleyl amine and oleic mixed solution, dense HNO 3Concentration is 67%, to be mixed evenly after, add Bi (NO again 3) 35H 2O powder and NH 4VO 3Powder, wherein amino dodecane or oleyl amine: Bi (NO 3) 3: NH 4VO 3: the mol ratio of nitric acid is 3: 1: 1: 8 or oleyl amine: oleic acid: Bi (NO 3) 3: NH 4VO 3: the nitric acid mol ratio is 15: 3: 5: continue stir after again with volume ratio be the pH=1.5-3 of the sodium hydroxide alcoholic solution regulator solution of 1: 1 ethanol and ethylene glycol at 5: 40, and sodium hydroxide alcoholic solution concentration is 2mol/L; It is that the stainless steel of tetrafluoroethylene is from pressing in the still that above-mentioned mixed solution is transferred to liner, from pressing the long-pending compactedness of kettle is 70%, and place thermostat container in 100 ℃ of organic solvent-hydrothermal treatment consists 12h, it naturally cools to room temperature to take out relief, the product that obtains is filtered, and deionized water wash and absolute ethanol washing each 3 times are in 60 ℃ of dry 12h, after in air atmosphere, rising to 400 ℃ of calcination 4h, promptly obtain the American football shape porous BiVO of monocline scheelite-type structure with the temperature rise rate of 1 ℃/min 4Micron particle.
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