CN102992406B - Preparation method of bismuth tungstate nano-sheet - Google Patents
Preparation method of bismuth tungstate nano-sheet Download PDFInfo
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- CN102992406B CN102992406B CN201110272612.2A CN201110272612A CN102992406B CN 102992406 B CN102992406 B CN 102992406B CN 201110272612 A CN201110272612 A CN 201110272612A CN 102992406 B CN102992406 B CN 102992406B
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Abstract
The invention relates to bismuth tungstate nano-sheets and a preparation method thereof. The bismuth tungstate nano-sheets are approximately square-shaped. A single sheet layer has a thickness of 10-100nm, a length of 1-20mum, and a width of 1-20mum; a plurality of bismuth tungstate nano-sheets are stacked along a same specific direction, such that a multilayer square ordered stack is formed. A specific preparation method comprises the steps that: bismuth salt which is soluble in acid is added into concentrated nitric acid; primary stirring is carried out, and deionized water is added for dissolving and diluting; tungstate is added into ammonia water, and is dissolved by stirring; the two solutions are mixed, and a hydrothermal treatment is further carried out, such that the bismuth tungstate nano-sheets are obtained. The preparation method has the advantages of simple process, wide parameter adjustable range, high repeatability, and low cost. The method has good commercial prospect. The prepared bismuth tungstate nano-sheets have high application values in fields such as pollution treatment, environment protection, novel energy preparation, and the like.
Description
Technical field
The present invention relates to a kind of nanometer sheet and preparation method thereof, particularly a kind of Bismuth tungstate nano-sheet and preparation method thereof, belong to inorganic nano material and synthesis technical field.
Background technology
In recent years, problem of environmental pollution is day by day serious, and energy scarcity problem is also extremely urgent.Under the situation facing above-mentioned two large crises, people expand the scientific research of Pollution abatement, protection of the environment.Be catalyzer with semi-conductor, utilize sunlight catalytic oxidative degradation pollution substance as the effective pollution administration method of one, become a focus of environmental protection science research.Under research background as above, various countries research worker have developed multiple semiconductor nano material, as titanium dioxide, zinc oxide, tungstic oxide etc., for the improvement of pollutent and the acquisition of new forms of energy.For titanium dioxide, although nano titanium oxide has very high stability, stronger photo-catalysis capability, the advantage that nontoxic pollution-free etc. are outstanding.But titanium dioxide energy gap is 3.2 ev, this just means the incident photon that titanium dioxide can only absorb the wavelength matched and is less than 387 nanometers, and photoabsorption is only only limitted to ultraviolet region, and the luminous energy of this wave band accounts for 5% of the sunlight being irradiated to ground.The ratio of visible light part accounts for 45% of sun power, and the actual solar radiation energy arriving earth's surface concentrates on 460 ~ 500 nanometer wavelength range.Therefore how to utilize natural light to carry out light-catalyzed reaction efficiently, exploitation can be caused the interest of people just day by day by the photocatalyst of excited by visible light.
In recent years, the focused on searching of more research worker by research has on the two-phase metal oxide of different crystal morphology, by expanding light abstraction width to visible region, with development of new photocatalyst.Nearest many researchs find, bismuth tungstate (Bi
2wO
6) be laminate structure, containing perovskite structure lamella, there is dielectric, luminescence, from the characteristic such as conductor, catalysis, be widely used in association area (Ju Wu, Fang Duan, et al, J.Phys.Chem.C 2007,111,12866-12871).Further, the most key, bismuth tungstate has visible light photocatalysis performance, can be used for photocatalytic water and degradable organic pollutant under visible light.(Dekun?Ma，Shaoming?Huang，et?al，J.Phys.Chem.C?2009，113，4369-4374)
Li Guishengs etc. have synthesized by Bismuth tungstate nano-sheet along stacking microballoon (the Guisheng Li of any direction, Dieqing Zhang, et al, Environ.Sci.Technol.2010,44,4276-4281), but, the nanometer sheet forming this microballoon grows together completely, cannot separate, and centre of sphere place is entity structure.But the Bismuth tungstate nano-sheet stacking along same specific direction has no report.
Summary of the invention
The object of the present invention is to provide a kind of Bismuth tungstate nano-sheet and preparation method thereof.
The invention provides a kind of Bismuth tungstate nano-sheet, it is characterized in that: Bismuth tungstate nano-sheet is closely square, monolithic lamellar spacing is 10 ~ 100 nanometers, and long and wide is 1 ~ 20 micron; Multi-disc Bismuth tungstate nano-sheet is stacked along same specific direction, forms a kind of multilayer, square ordered stacks body.
The invention provides a kind of preparation method of Bismuth tungstate nano-sheet, it is characterized in that comprising the steps:
(1) acid-soluble bismuth salt is joined in concentrated nitric acid, add deionized water after preliminary stirring and carry out dissolved dilution; In addition tungstate is joined stirring and dissolving in the ammoniacal liquor of 10wt% ~ 28wt%; Being added drop-wise to by the salpeter solution being dissolved with bismuth salt is dissolved with in the ammonia soln of tungstate, and dropping limit, limit is stirred, and forms uniform suspension;
(2) then hydro-thermal reaction process will be carried out at the temperature of suspension 373 ~ 473K in autoclave 6 ~ 72 hours, after stopped reaction, adopt filtration or centrifugal method to obtain, by precipitated product, then using deionized water wash, obtain Bismuth tungstate nano-sheet after drying.
Acid-soluble bismuth salt described in step (1) is anhydrous or with the one in the Bismuth trinitrate of crystal water, bismuthyl carbonate, pearl white, Trichlorobismuthine or its combination.
Concentrated nitric acid quality described in step (1) is 1 ~ 5 times of acid-soluble bismuth salt quality.
5, the preparation method of a kind of Bismuth tungstate nano-sheet according to claim 2, is characterized in that: the quality of the deionized water described in step (1) is 1 ~ 4 times of the concentrated nitric acid quality added; The addition of deionized water need ensure that the massfraction of ammoniacal substance in final suspension is at more than 5wt%.
Tungstate described in step (1) is one in sodium wolframate, potassium wolframate or its combination.
Tungstate described in step (1), W elements is 1: 1 ~ 2 with the ratio of the amount of substance of bismuth element.
The salpeter solution being dissolved with bismuth salt described in step (1) is 1: 0.6 ~ 10 with the ratio of the ammonia soln volume being dissolved with tungstate.
The bismuth tungstate obtained by above-mentioned preparation method is Bi
2wO
6type, its crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match.Pattern is square nanometer sheet, and monolithic lamellar spacing is between 10 nanometer ~ 100 nanometers, long and wide between 1 micron ~ 20 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.This product the field such as to be prepared at Pollution abatement, environment protection, hygiene medical treatment, new forms of energy and is all had very high potential using value.
Accompanying drawing explanation
Fig. 1: the X-ray powder diffraction pattern of the Bismuth tungstate nano-sheet that (a) is obtained by embodiment 2; The X-ray powder diffraction pattern of b Bismuth tungstate nano-sheet that () is obtained by embodiment 6.
Fig. 2: the stereoscan photograph of the Bismuth tungstate nano-sheet obtained by embodiment 2.
Fig. 3: the stereoscan photograph of the Bismuth tungstate nano-sheet obtained by embodiment 2.
Fig. 4: the stereoscan photograph of the Bismuth tungstate nano-sheet obtained by embodiment 6.
Fig. 5: the stereoscan photograph of the Bismuth tungstate nano-sheet obtained by embodiment 6.
Embodiment
Below by embodiment, the present invention is further elaborated, and its object is only better to understand content of the present invention.Therefore, the cited case does not limit the scope of the invention.
Embodiment 1
1.8 a gram pearl white joins in 3.5 milliliters of concentrated nitric acids, add 12 ml deionized water after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately join in the ammoniacal liquor of 60 milliliter 15% by 1.2 gram of one tungstic acid hydrate sodium, stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the stainless steel autoclave of teflon lined, reacts 30 hours at the temperature of 423K.By precipitated product deionized water wash after reaction terminates, then vacuum-drying under 323K, obtains Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 60 nanometers of monolithic lamellar spacing, long and wide between 3 ~ 5 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 2
2.0 gram five nitric hydrate bismuths join in 4 milliliters of concentrated nitric acids, add 20 ml deionized water after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately 0.9 gram of one tungstic acid hydrate sodium being joined 50 ml concns is in the ammoniacal liquor of 25%, and stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the stainless steel autoclave of teflon lined, reacts 24 hours at the temperature of 393K.By precipitated product deionized water wash after reaction terminates, then constant pressure and dry under 343K, obtains Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 50 nanometers of monolithic lamellar spacing, long and wide between 4 ~ 7 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 3
1.9 a gram Trichlorobismuthine joins in 3 milliliters of concentrated nitric acids, add 15 ml deionized water after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately join in the ammoniacal liquor of 55 milliliter 18% by 1.0 gram of one tungstic acid hydrate sodium, stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the stainless steel autoclave of teflon lined, reacts 36 hours at the temperature of 403K.By precipitated product deionized water wash after reaction terminates, then constant pressure and dry under 353K, obtains Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 50 nanometers of monolithic lamellar spacing, long and wide between 2 ~ 4 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 4
1.2 grams of bismuthyl carbonates join in 3 milliliters of concentrated nitric acids.Add 8 ml deionized water after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately join in the ammoniacal liquor of 62 milliliter 15% by 0.7 gram of one tungstic acid hydrate sodium, stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the stainless steel autoclave of teflon lined, reacts 6 hours at the temperature of 473K.By precipitated product deionized water wash after reaction terminates, then vacuum-drying under 333K, obtains Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 40 nanometers of monolithic lamellar spacing, long and wide between 1 ~ 3 micron.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 5
1.5 grams of pearl whites join in 3 milliliters of concentrated nitric acids.Add 15 ml deionized water after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately join in the ammoniacal liquor of 60 milliliter 20% by 1.5 gram of eight tungstic acid hydrate potassium, stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the stainless steel autoclave of teflon lined, reacts 72 hours at the temperature of 413K.By precipitated product deionized water wash after reaction terminates, then vacuum-drying under 323K, obtains Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 80 nanometers of monolithic lamellar spacing, long and wide between 5 ~ 10 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 6
3.0 gram of five nitric hydrate bismuth joins in 5 milliliters of concentrated nitric acids.Add 18 ml deionized water after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately 1.6 gram of one tungstic acid hydrate sodium being joined 52 ml concns is in the ammoniacal liquor of 28%, and stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the stainless steel autoclave of teflon lined, reacts 24 hours at the temperature of 453K.By precipitated product deionized water wash after reaction terminates, then constant pressure and dry under 353K, obtains Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 100 nanometers of monolithic lamellar spacing, the length of most of nanometer sheet and wide between 1 ~ 10 micron.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 7
0.4 kilogram of five nitric hydrate bismuth joins in 0.6 liter of concentrated nitric acid, and join in 3 liters of deionized waters by the former after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately join in the ammoniacal liquor of 9 liter 12% by 0.16 kilogram of one tungstic acid hydrate sodium, stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into the autoclave that volume is 25 liters, reacts 24 hours at the temperature of 393K.By precipitated product deionized water wash after reaction terminates, then through spraying dry, obtain Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 80 nanometers of monolithic lamellar spacing, the length of most of nanometer sheet and wide between 5 ~ 10 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Embodiment 8
0.5 kilogram of five nitric hydrate bismuth joins in 0.8 liter of concentrated nitric acid, and join in 4 liters of deionized waters by the former after preliminary stirring, stirring and dissolving is diluted, and is designated as solution A.Separately join in the ammoniacal liquor of 10 liter 10% by 0.27 kilogram of eight tungstic acid hydrate potassium, stirring and dissolving, is designated as solution B.
Solution A is added drop-wise in solution B, and dropping limit, limit is stirred, and forms uniform suspension, then suspension is put into autoclave, reacts 18 hours at the temperature of 423K.By precipitated product deionized water wash after reaction terminates, then through spraying dry, obtain Bismuth tungstate nano-sheet.
Obtained bismuth tungstate (Bi
2wO
6) crystal formation and standard powdery diffractometry card (JCPDS:73-1126) match, pattern is the nanometer sheet of squarish, about 100 nanometers of monolithic lamellar spacing, the length of most of nanometer sheet and wide between 2 ~ 8 microns.Multi-disc Bismuth tungstate nano-sheet is stacked along the vertical direction of lamella, forms a kind of multilayer, square ordered stacks body.
Claims (1)
1. a preparation method for Bismuth tungstate nano-sheet, is characterized in that, comprises the steps:
(1) acid-soluble bismuth salt is joined in concentrated nitric acid, add deionized water after preliminary stirring and carry out dissolved dilution; In addition tungstate is joined stirring and dissolving in the ammoniacal liquor of 10 wt% ~ 28 wt%; Being added drop-wise to by the salpeter solution being dissolved with bismuth salt is dissolved with in the ammonia soln of tungstate, and dropping limit, limit is stirred, and forms uniform suspension;
(2) then hydro-thermal reaction process will be carried out at the temperature of suspension 373 ~ 473K in autoclave 6 ~ 72 hours, after stopped reaction, adopt filtration or centrifugal method to obtain, by precipitated product, then using deionized water wash, obtain Bismuth tungstate nano-sheet after drying; Monolithic lamellar spacing is 10 ~ 100 nanometers, and long and wide is 1 ~ 20 micron; Multi-disc Bismuth tungstate nano-sheet is stacked along same specific direction, forms a kind of multilayer, square ordered stacks body;
Acid-soluble bismuth salt described in step (1) is anhydrous or with the one in the Bismuth trinitrate of crystal water, bismuthyl carbonate, pearl white, Trichlorobismuthine or its combination;
Concentrated nitric acid quality described in step (1) is 1 ~ 5 times of acid-soluble bismuth salt quality;
The quality of the deionized water described in step (1) is 1 ~ 4 times of the concentrated nitric acid quality added; The addition of deionized water need ensure that the massfraction of ammoniacal substance in final suspension is at more than 5wt%;
Tungstate described in step (1) is one in sodium wolframate, potassium wolframate or its combination;
Tungstate described in step (1), W elements is 1:1 ~ 2 with the ratio of the amount of substance of bismuth element;
The salpeter solution being dissolved with bismuth salt described in step (1) is 1:0.6 ~ 10 with the ratio of the ammonia soln volume being dissolved with tungstate.
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| CN103611528B (en) * | 2013-12-05 | 2015-06-03 | 河南师范大学 | Method for preparing bismuth tungstate catalyst by taking egg white as template |
| CN104561979B (en) * | 2014-12-29 | 2017-11-14 | 中南大学 | The preparation method of bismuth tungstate film |
| CN104785260A (en) * | 2015-04-24 | 2015-07-22 | 上海电力学院 | Visible-light-driven photocatalyst for catalytic conversion of methane, as well as preparation method and application thereof |
| CN105170137B (en) * | 2015-06-03 | 2017-06-23 | 河南师范大学 | A kind of Bi with cubic structure2WO6The preparation method of photochemical catalyst |
| CN105457626A (en) * | 2016-01-25 | 2016-04-06 | 温州大学 | Preparation method and application of concave-surface bismuth tungstate nanosheet electrocatalyst |
| CN108906033A (en) * | 2018-07-16 | 2018-11-30 | 河南师范大学 | The method for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system |
| CN109225204A (en) * | 2018-10-19 | 2019-01-18 | 上海纳米技术及应用国家工程研究中心有限公司 | The preparation of Bismuth tungstate nano-sheet visible light catalyst for tetracycline wastewater processing and product and application |
| CN113083287B (en) * | 2021-04-29 | 2023-09-19 | 沈阳工业大学 | Bismuth and bismuth tungstate composite powder with nano-particle stacking lamellar structure and preparation method thereof |
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