CN104028264A - Regularly quadrangular bismuth-series oxysalt Bi2WO6 and preparation method thereof - Google Patents

Regularly quadrangular bismuth-series oxysalt Bi2WO6 and preparation method thereof Download PDF

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CN104028264A
CN104028264A CN201410258706.8A CN201410258706A CN104028264A CN 104028264 A CN104028264 A CN 104028264A CN 201410258706 A CN201410258706 A CN 201410258706A CN 104028264 A CN104028264 A CN 104028264A
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oxysalt
preparation
bismuth
prism shape
distilled water
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CN104028264B (en
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陈刚
李春梅
孙净雪
董红军
吕查德
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Harbin Institute of Technology
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Abstract

The invention discloses regularly quadrangular bismuth-series oxysalt Bi2WO6 and a preparation method thereof. The invention aims to solve the technical problem that the conventional Bi2WO6 prepared by a molten-salt growth method is low in degradation capability. The regularly quadrangular bismuth-series oxysalt Bi2WO6 refers to regularly quadrangular granules which are formed by gathering nanosheets in a directional mode in parallel, wherein the edges and the corners of the granules are rounded. The preparation method comprises the following steps: dripping a Na2WO4.2H2O solution into emulsion of Bi(NO3)3, stirring and reacting to obtain a mixed solution, centrifuging to separate a solid-phase product, and drying to obtain a precursor; mixing the precursor and a fused salt according to a mass ratio of 1 to (3-7), putting the mixture into a furnace at the temperature of 340-360 DEG C, and reacting for 4-6 hours to obtain the regularly quadrangular bismuth-series oxysalt Bi2WO6. The regularly quadrangular bismuth-series oxysalt Bi2WO6 can serve as a photocatalyst and is applied to the field of photocatalysis.

Description

A kind of four-prism shape bismuth is oxysalt Bi 2wO 6and preparation method thereof
Technical field
The present invention relates to bismuth is oxysalt Bi 2wO 6and preparation method thereof.
Background technology
In today of 21 century, along with economic develop rapidly, incident environmental problem has become the severeest problem of human society.Utilizing organic pollution in solar energy photocatalytic degradation of sewage to solve this problem more and more gets more and more people's extensive concerning.Traditional photochemical catalyst TiO 2because it has larger band gap magnitude, only under the irradiation of ultraviolet light, just can show photocatalysis characteristic, and ultraviolet light only accounts for 3%～4% of sunshine, this has just limited TiO 2the practical application of this photochemical catalyst.Therefore, the efficient visible light responsible photocatalytic material of development of new, the pollutant effectively utilizing in sunshine degradation of sewage is one of main path solving environmental pollution.
In recent years, a kind of novel visible light catalytic material Bi with visible light-responded and the good narrow band gap of visible light catalysis activity 2wO 6(energy gap is only 2.8eV left and right), has caused that researchers pay close attention to widely.Bismuth tungstate is a kind of simple layer structure oxide, has WO 6and Bi 2o 2the perovskite-like lamellar structure forming, mainly has following feature: good Uv and visible light response; Heat endurance; Cost is relatively low; Environmental friendliness.Therefore, research and development Bi 2wO 6catalysis material, will increase the utilization rate of solar energy, aspect the improvement of problem of environmental pollution and the Application and Development of new forms of energy, is having great meaning.
The method of preparing photochemical catalyst bismuth tungstate has a variety of; wherein molten-salt growth method is because its manufacture craft is simple; required synthesis temperature is low; time is short; output is high; high and the salt of sample degree of crystallinity can be recycled, and the advantages such as environment can not pollute is considered to most probable and realizes the method that industrial scale is produced photochemical catalyst.In recent years, Qianjiang China waited people to report the Bi preparing by molten-salt growth method 2wO 6ceramic powder, yet the Bi making 2wO 6for irregular sheet-like morphology, and its degradation property is poor, and the efficiency of Visible Light Induced Photocatalytic rhodamine B only can reach 40% in 2h.
Summary of the invention
The present invention will solve the existing Bi preparing with molten-salt growth method 2wO 6the poor technical problem of degradation capability, and a kind of four-prism shape bismuth is provided, be oxysalt Bi 2wO 6and preparation method thereof.
A kind of four-prism shape bismuth of the present invention is oxysalt Bi 2wO 6, be by nanometer sheet parallel orientation, to be assembled the four-prism shape particle of the corner angle rounding forming.
Above-mentioned four-prism shape bismuth is oxysalt Bi 2wO 6preparation method, carry out according to the following steps:
One, press Bi (NO 3) 35H 2o and Na 2wO 42H 2the mol ratio of O is 2:1, takes Bi (NO 3) 35H 2o and Na 2wO 42H 2o;
Two, take distilled water as solvent, the Bi (NO that step 1 is taken 3) 35H 2o joins in distilled water, with ultrasonic concussion, processes, and obtains Bi (NO 3) 3emulsion; By Na 2wO 42H 2o dissolves with distilled water, obtains Na 2wO 42H 2o solution;
Three, under constantly stirring, by the Na of step 2 preparation 2wO 42H 2o solution splashes into Bi (NO 3) 3emulsion in, after dropwising, stir 1～2 hour, obtain mixed liquor;
Four, centrifugation after distilled water washing for mixed liquor step 3 being obtained, then that solid formation is dry, obtain presoma;
Five, press KNO 3and NaNO 3mol ratio be that 1:1 is by KNO 3and NaNO 3be mixed, ground and mixed is even, obtains salt-mixture;
Six, by the mass ratio of presoma and salt-mixture, be 1:3～7, presoma and salt-mixture ground and mixed is even, obtain mixed-powder;
Seven, mixed-powder step 6 being obtained is placed in crucible, is placed on temperature and is in the stove of 340～360 ℃ to keep reaction 4～6h; After reaction finishes, absolute ethyl alcohol and/or distilled water cyclic washing for the material in crucible, be then placed in baking oven and be dried, and obtaining four-prism shape bismuth is oxysalt Bi 2wO 6.
The bismuth-containing oxygen hydrochlorate Bi that the present invention adopts molten-salt growth method to prepare 2wO 6photochemical catalyst, the method is that a kind of cheapness is simple, can realize and obtain high-crystallinity at short notice, the uniform Bi of pattern 2wO 6.Sample productive rate is higher simultaneously, up to 75%, as the fused salt of reaction, also can recycle, and this is just for industrial-scale production improves theory support.This method appropriate design selects the allocation ratio of fused salt and the temperature conditions of molten salt react ion to prepare the Bi of four-prism shape 2wO 6it can be used as the catalyst of light-catalyzed reaction, have visible light-responded preferably, this catalyst shows the photocatalysis performance of higher degradating organic dye rhodamine B under visible ray simultaneously, under the radiation of visible light of λ >400nm, degradable organic pollution rhodamine B only needs 40 minutes, and is degradation of dye rather than simply cycloreversion reaction completely.Bi of the present invention 2wO 6the Photocatalytic Degradation Property of catalyst obviously improves.Bi of the present invention 2wO 6can act on photocatalysis field.
Accompanying drawing explanation
Fig. 1 is oxysalt Bi for testing the bismuth that in 1 prepared by molten-salt growth method 2wO 6the XRD spectra of photochemical catalyst;
Fig. 2 is oxysalt Bi for testing the bismuth that in 1 prepared by molten-salt growth method 2wO 6the SEM spectrogram of photochemical catalyst;
Fig. 3 is oxysalt Bi for testing the bismuth that in 1 prepared by molten-salt growth method 2wO 6the TEM spectrogram in four-prism front;
Fig. 4 is that the bismuth that in test 1 prepared by molten-salt growth method is oxysalt Bi 2wO 6the TEM spectrogram of four-prism body side surface;
Fig. 5 is oxysalt Bi for testing the bismuth that in 1 prepared by molten-salt growth method 2wO 6the degradable organic pollutant spectrogram of photochemical catalyst;
Fig. 6 is oxysalt Bi for testing the bismuth that in 1 prepared by molten-salt growth method 2wO 6the UV, visible light of the different degradation times of photochemical catalyst absorbs spectrogram;
Fig. 7 is oxysalt Bi for testing the bismuth that in 2 prepared by molten-salt growth method 2wO 6the SEM spectrogram of photochemical catalyst;
Fig. 8 is oxysalt Bi for testing the bismuth that in 3 prepared by molten-salt growth method 2wO 6the SEM spectrogram of photochemical catalyst.
The specific embodiment
The specific embodiment one: a kind of four-prism shape bismuth of present embodiment is oxysalt Bi 2wO 6, be by nanometer sheet parallel orientation, to be assembled the four-prism shape particle of the corner angle rounding forming.
The length of side of the four-prism bottom surface of the four-prism shape particle of present embodiment is 1～2 μ m, and height is 0.8～1.2 μ m; The thickness of nanometer sheet is 8～12nm.
The specific embodiment two: the four-prism shape bismuth described in the specific embodiment one is oxysalt Bi 2wO 6preparation method, carry out according to the following steps:
One, press Bi (NO 3) 35H 2o and Na 2wO 42H 2the mol ratio of O is 2:1, takes Bi (NO 3) 35H 2o and Na 2wO 42H 2o;
Two, take distilled water as solvent, the Bi (NO that step 1 is taken 3) 35H 2o joins in distilled water, with ultrasonic concussion, processes, and obtains Bi (NO 3) 3emulsion; By Na 2wO 42H 2o dissolves with distilled water, obtains Na 2wO 42H 2o solution;
Three, under constantly stirring, by the Na of step 2 preparation 2wO 42H 2o solution splashes into Bi (NO 3) 3emulsion in, after dropwising, stir 1～2 hour, obtain mixed liquor;
Four, centrifugation after distilled water washing for mixed liquor step 3 being obtained, then that solid formation is dry, obtain presoma;
Five, press KNO 3and NaNO 3mol ratio be that 1:1 is by KNO 3and NaNO 3be mixed, ground and mixed is even, obtains salt-mixture;
Six, by the mass ratio of presoma and salt-mixture, be 1:3～7, presoma and salt-mixture ground and mixed is even, obtain mixed-powder;
Seven, mixed-powder step 6 being obtained is placed in crucible, is placed on temperature and is in the stove of 300 ℃～400 ℃ to keep reaction 4～6h; After reaction finishes, absolute ethyl alcohol and/or distilled water cyclic washing for the material in crucible, be then placed in baking oven and be dried, and obtaining four-prism shape bismuth is oxysalt Bi 2wO 6.
The specific embodiment three: that present embodiment is different from the specific embodiment two is Bi (NO in step 2 3) 35H 2the amount of substance of O is 1mol:(5～10 with the ratio of distilled water volume) mL.Other is identical with the specific embodiment one.
The specific embodiment four: that present embodiment is different from the specific embodiment two or three is Na in step 2 2wO 42H 2the amount of substance of O is 1mol:(10～15 with the ratio of distilled water volume) mL.Other is identical with the specific embodiment one or two.
The specific embodiment five: what present embodiment was different from one of specific embodiment two to four is that temperature dry in step 4 is at 80～100 ℃.Other is identical with one of specific embodiment two to four.
The specific embodiment six: present embodiment is different from one of specific embodiment two to five is that in step 6, the mass ratio of presoma and salt-mixture is 1:5.Other is identical with one of specific embodiment two to five.
In this molten-salt growth method preparation process, the ratio of presoma and salt-mixture is very crucial parameter, and the ratio of presoma and salt-mixture has larger impact to the pattern of product.
The specific embodiment seven: present embodiment is different from one of specific embodiment two to six is that reaction temperature in step 7 is 350 ℃.Other is identical with one of specific embodiment two to six.
In this molten-salt growth method preparation process, the selection of reaction temperature is also a key.
With following verification experimental verification beneficial effect of the present invention:
Test 1: the four-prism shape bismuth of this test is oxysalt Bi 2wO 6preparation method, carry out according to the following steps:
One, take Bi (NO 3) 3.5H 2o (1mmol, 0.485g), Na 2wO 4.2H 2o (0.5mmol, 0.169g); KNO 3(0.1mol, 10.1g) and NaNO 3(0.1mol, 8.5g);
Two, take distilled water as solvent, the Bi (NO that step 1 is taken 3) 3.5H 2o adds 7mL distilled water, and ultrasonic concussion is processed 30 minutes, obtains white Bi (NO 3) 3emulsion; By Na 2wO 4.2H 2o (0.5mmol) adds in 6mL water and dissolves, and obtains Na 2wO 4.2H 2o solution;
Three, under constantly stirring, by the Na of step 2 preparation 2wO 4.2H 2o solution slowly splashes into Bi (NO 3) 3emulsion in, after dropwising, stir 1 hour, obtain mixture;
Four, centrifugation after distilled water cyclic washing for mixture step 3 being obtained, dry in 80 ℃ of baking ovens afterwards, obtain presoma;
Five, take 10.1g KNO 3(0.1mol) with 8.5g NaNO 3(0.1mo l); KNO 3and NaNO 3together, ground and mixed 30 minutes, mixes it to solids mixing, obtains KNO 3and NaNO 3salt-mixture;
Six, the salt-mixture ground and mixed that presoma 1g step 4 being obtained and 5g step 5 obtain 30 minutes, obtains mixture;
Seven, mixture step 6 being obtained is placed in crucible, is placed on temperature and is in the Muffle furnace of 350 ℃ to keep reaction 4h; After reaction finishes, the material in crucible is first used absolute ethanol washing 3 times, then with distilled water washing 3 times, is finally placed in 80 ℃ of baking ovens and is dried 12 hours, and obtaining four-prism shape bismuth is oxysalt Bi 2wO 6.
The four-prism shape bismuth that this test obtains is oxysalt Bi 2wO 6xRD spectra as shown in Figure 1, wherein a is the Bi of this test preparation 2wO 6xRD spectra, b is 73-1126 Bi in PDF card 2wO 6standard spectrogram, contrast knownly, the bismuth of this test preparation is oxysalt Bi 2wO 6really be Bi 2wO 6, and well-crystallized.
The bismuth that Fig. 2 obtains for this test is oxysalt Bi 2wO 6stereoscan photograph, as can be seen from Figure 2, the Bi of this test preparation 2wO 6the four-prism that is shaped as corner angle rounding, the length of side of its bottom surface is 2 μ m, height is 1 μ m.
The bismuth that Fig. 3 obtains for this test is oxysalt Bi 2wO 6the transmission electron microscope photo in four-prism front, as can be seen from Figure 3, the four-prism of this corner angle rounding was formed by directed gathering of uniform ultrathin nanometer sheet;
Fig. 4 is that the bismuth that this test obtains is oxysalt Bi 2wO 6the transmission electron microscope photo of four-prism body side surface; The thickness of nanometer sheet is about 10nm as can be seen from Figure 4.
By the Bi of this test preparation 2wO 6carry out Degrading experiment, process of the test is as follows: by 0.05g Bi 2wO 6sample joins in the rhodamine B solution of 100ml, and under dark room conditions, evenly magnetic agitation stirs 1h to reach adsorption equilibrium, and now rhodamine B concentration is C 0the degrading activity of detecting catalyst under radiation of visible light more afterwards, light source is 300W xenon lamp, use optical filter to filter ultraviolet light (λ >400nm), carrying out along with reaction, at interval of within 10 minutes, get 3ml liquid from reactant liquor, through centrifugation (10000 revs/min), obtain settled solution, concentration is C.1-C/C 0embody the degradation rate of rhodamine B under this time.Meanwhile, to taking out solution testing ultraviolet-visible absorption spectroscopy, paint and prepare C/C 0curve over time.Wherein the UV, visible light of different degradation times absorbs spectrogram as shown in Figure 5, and in figure, a is that the UV, visible light of degradation time while being 0 minute absorbs spectrogram; B is that the UV, visible light of degradation time while being 10 minutes absorbs spectrogram; C is that the UV, visible light of degradation time while being 20 minutes absorbs spectrogram; D is that the UV, visible light of degradation time while being 30 minutes absorbs spectrogram; E is that the UV, visible light of degradation time while being 40 minutes absorbs spectrogram.As can be seen from Figure 5, along with the increase of degradation time, absorption intensity reduces, and illustrates that rhdamine B is constantly degraded until degrade completely.From ultraviolet-visible absorption spectroscopy, figure it can also be seen that, rhodamine B is to degrade completely, rather than simple cycloreversion reaction.
C/C 0as shown in Figure 6, in Fig. 6, a is the Bi with this test preparation to curve over time 2wO 6c/C 0curve over time, b is with the P25 powder check experiment of degrading, the C/C obtaining 0curve over time.As can be seen from Figure 6, the Bi of preparation 2wO 6its degrading activity of sample, far above P25, further confirms four-prism Bi 2wO 6sample has higher photocatalytic activity, can be used as a kind of desirable catalysis material.
Test 2: what this test was different from test 1 is in step 6, by the Bi that 1g step 4 is obtained 2wO 6the salt-mixture ground and mixed that the presoma of photochemical catalyst and 7g step 5 obtain 30 minutes, obtains mixture; Other step is all identical with test 1 with parameter.
The bismuth that this test obtains is oxysalt Bi 2wO 6stereoscan photograph as shown in Figure 7, as can be seen from Figure 7, the Bi of this test preparation 2wO 6, its shape has the four-prism of corner angle rounding, and the length of side of its bottom surface is 2 μ m, and height is 1 μ m, also has the particle of irregular pattern.The Bi of preparation 2wO 6sample can make rhodamine B degradable in 70 minutes.
Test 3: what this test was different from test 1 is in step 6, by the Bi that 1g step 4 is obtained 2wO 6the salt-mixture ground and mixed that the presoma of photochemical catalyst and 3g step 5 obtain 30 minutes, obtains mixture; Other step is all identical with test 1 with parameter.
The bismuth that this test obtains is oxysalt Bi 2wO 6stereoscan photograph as shown in Figure 8, as can be seen from Figure 8, the Bi of this test preparation 2wO 6, its shape has the four-prism of corner angle rounding, and the length of side of its bottom surface is 2 μ m, and height is 1 μ m, also has the particle of irregular pattern.The Bi2WO6 sample of preparation can make rhodamine B degradable in 80 minutes.
Test 1,2 and 3, the presoma of employing is different from the ratio of salt-mixture, when wherein the ratio of presoma and salt-mixture is 1:5, the Bi obtaining 2wO 6the four-prism shape of the pattern corner angle rounding that is well-crystallized, and the Bi obtaining in test 2 and 3 2wO 6the particle that has other shapes, crystallization is not fine, with comparing of well-crystallized, degradation effect is slightly poor.

Claims (7)

1. a four-prism shape bismuth is oxysalt Bi 2wO 6, it is characterized in that this Bi 2wO 6by nanometer sheet parallel orientation, to be assembled the four-prism shape particle of the corner angle rounding forming.
2. preparation a kind of four-prism shape bismuth claimed in claim 1 is oxysalt Bi 2wO 6method, it is characterized in that the method carries out according to the following steps:
One, press Bi (NO 3) 35H 2o and Na 2wO 42H 2the mol ratio of O is 2:1, takes Bi (NO 3) 35H 2o and Na 2wO 42H 2o;
Two, take distilled water as solvent, the Bi (NO that step 1 is taken 3) 35H 2o joins in distilled water, with ultrasonic concussion, processes, and obtains Bi (NO 3) 3emulsion; By Na 2wO 42H 2o dissolves with distilled water, obtains Na 2wO 42H 2o solution;
Three, under constantly stirring, by the Na of step 2 preparation 2wO 42H 2o solution splashes into Bi (NO 3) 3emulsion in, after dropwising, stir 1～2 hour, obtain mixed liquor;
Four, centrifugation after distilled water washing for mixed liquor step 3 being obtained, then that solid formation is dry, obtain presoma;
Five, press KNO 3and NaNO 3mol ratio be that 1:1 is by KNO 3and NaNO 3be mixed, ground and mixed is even, obtains salt-mixture;
Six, by the mass ratio of presoma and salt-mixture, be 1:3～7, presoma and salt-mixture ground and mixed is even, obtain mixed-powder;
Seven, mixed-powder step 6 being obtained is placed in crucible, is placed on temperature and is in the stove of 340～360 ℃ to keep reaction 4～6h; After reaction finishes, absolute ethyl alcohol and/or distilled water cyclic washing for the material in crucible, be then placed in baking oven and be dried, and obtaining four-prism shape bismuth is oxysalt Bi 2wO 6.
3. a kind of four-prism shape bismuth according to claim 2 is oxysalt Bi 2wO 6preparation method, it is characterized in that Bi (NO in step 2 3) 35H 2the amount of substance of O is 1mol:(5～10 with the ratio of distilled water volume) mL.
4. according to a kind of four-prism shape bismuth described in claim 2 or 3, be oxysalt Bi 2wO 6preparation method, it is characterized in that Na in step 2 2wO 42H 2the amount of substance of O is 1mol:(10～15 with the ratio of distilled water volume) mL.
5. according to a kind of four-prism shape bismuth described in claim 2 or 3, be oxysalt Bi 2wO 6preparation method, it is characterized in that temperature dry in step 4 is at 80～100 ℃.
6. according to a kind of four-prism shape bismuth described in claim 2 or 3, be oxysalt Bi 2wO 6preparation method, it is characterized in that in step 5, the mass ratio of presoma and salt-mixture is 1:5.
7. according to a kind of four-prism shape bismuth described in claim 2 or 3, be oxysalt Bi 2wO 6preparation method, it is characterized in that the reaction temperature in step 7 is 350 ℃.
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CN106629613A (en) * 2016-12-20 2017-05-10 华中科技大学 Preparation method of ionic intercalation type two-dimensional material
CN111617784A (en) * 2020-06-23 2020-09-04 盐城工学院 Preparation method and application of two-dimensional layered bismuth oxychloride-Fe doped modified photocatalytic material
CN114984993A (en) * 2022-05-26 2022-09-02 南京林业大学 N, S quantum dot/bismuth tungstate composite photocatalyst and preparation method and application thereof

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CN103301833A (en) * 2013-02-04 2013-09-18 上海交通大学 Yb<3+>-Tm<3+>-Li<+> triple-doped Bi2WO6/CNTs (carbon nanotubes) upconversion photocatalytic material
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Publication number Priority date Publication date Assignee Title
CN106629613A (en) * 2016-12-20 2017-05-10 华中科技大学 Preparation method of ionic intercalation type two-dimensional material
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CN111617784A (en) * 2020-06-23 2020-09-04 盐城工学院 Preparation method and application of two-dimensional layered bismuth oxychloride-Fe doped modified photocatalytic material
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CN114984993B (en) * 2022-05-26 2024-01-26 南京林业大学 N, S quantum dot/bismuth tungstate composite photocatalyst, and preparation method and application thereof

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