CN101791548A - Visible light catalyst BiVO4 and preparation method thereof - Google Patents
Visible light catalyst BiVO4 and preparation method thereof Download PDFInfo
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- CN101791548A CN101791548A CN 201010152232 CN201010152232A CN101791548A CN 101791548 A CN101791548 A CN 101791548A CN 201010152232 CN201010152232 CN 201010152232 CN 201010152232 A CN201010152232 A CN 201010152232A CN 101791548 A CN101791548 A CN 101791548A
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Abstract
The invention discloses a visible light catalyst BiVO4 and a preparation method thereof. The BiVO4 is powder, the crystalline phase is monoclinic crystal serial scheelite structure, and the feature thereof is in a three-dimensional connected pore channel structure. In the preparation method, ethanediol is utilized as solvent, and bismuth salt and vanadium salt are respectively used as a Bi source and a V source for preparing the three-dimensional connected pore channel structural BiVO4. The preparation method is as follows: dissolving bismuth salt and vanadium salt into ethanediol according to the proportion that Bi/ V equals to 1:0.5-1:2 to prepare solution the Bi ion concentration of which is 0.05-0.5mol.L<-1>; forming even settled solution, and then transferring the settled solution to a constant-temperature water bath tank of 50-90 DEG C to preserve heat for 2-10 days; and after obtaining flocks, centrifuging, washing, drying and finally calcining obtained powder at the temperature of 350-600 DEG C for 1-3h in air environment. In the invention, no surfactant is utilized, and the catalyst with novel structure and very large specific surface area is obtained after simple heat preservation in the water bath tank and later-stage low temperature heat treatment. The catalyst has smaller particles and higher photocatalysis activity, thus being applied to degrading organic pollutants by visible light catalyst.
Description
Technical field
The invention belongs to the photocatalyst material field, be specifically related to a kind of novel three-dimensional connected pore channel structure, visible light catalyst B iVO
4The preparation method, the resulting catalyst harmful substance in the environment that can be used for degrading.
Background technology
In the last few years, environmental pollution and energy crisis were serious day by day to the challenge that human survival brings, and photocatalysis technology arises at the historic moment as a kind of advanced oxidation process technology, and had obtained significant development.Titanium dioxide (TiO
2) owing to its stable chemical property, superior catalytic activity, nontoxic, lower-price characteristic, become research photochemical catalyst the most widely.But, since the restriction of the energy gap of broad (3.2ev), TiO
2Can only utilize ultraviolet light less than 388nm, and few to the utilization of the visible light that accounts for solar energy 45%.Therefore, exploitation efficiently utilizes the visible light responsive photocatalyst of visible light to have high economic worth and practical prospect.
In the excited by visible light photochemical catalyst, bismuth-system compound oxide is because unique crystal structure and electronic structure becomes the research focus in the visible light catalytic agent material.Pucherite (BiVO
4) as a kind of representational photochemical catalyst, BiVO with monocline phase
4Than cubic phase BiVO
4Show higher photocatalytic activity.The pucherite of traditional solid reaction process preparation is because particle is thick, specific area is little, its photocatalysis performance is relatively poor, adopt the mode of adding template agent and surfactant to adjust the appearance structure of material and use more hydro-thermal method at present more, complicated operation, cost an arm and a leg.
Summary of the invention
The object of the present invention is to provide a kind of preparation three-dimensional communication pore passage structure visible light catalyst BiVO
4And preparation method thereof, visible light catalyst BiVO
4Have the three-dimensional communication pore passage structure, particle is less, and has bigger specific area; Preparation method's technology is simple, and is with low cost, and energy consumption is low.
A kind of visible light catalyst BiVO provided by the invention
4, it is characterized in that this visible light catalyst BiVO
4Be powder, crystalline phase is the monoclinic system scheelite-type structure, and its pattern is the three-dimensional communication pore passage structure.
Above-mentioned visible light catalyst BiVO
4The preparation method comprises the steps:
(1) be to be dissolved in the ethylene glycol in 1: 0.5～1: 2 according to the mol ratio of the V ion in Bi ion and the vanadic salts in the bismuth salt, ultrasonic, stir, being prepared into the Bi ion concentration is 0.05～0.5molL
-1Settled solution;
(2) prepared settled solution is transferred in the constant water bath box, setting holding temperature is 50～90 ℃, and temperature retention time is 2～10 days;
(3) resulting precipitation distilled water centrifuge washing is used the alcohol centrifuge washing again, and oven dry evaporates residual alcohol, obtains powder;
(4) with the powder that obtains at 350～600 ℃ down behind calcining 1～3h, obtain visible light catalyst BiVO
4
The present invention prepares resulting catalyst and exists with the powder form, and crystalline phase is the monoclinic system scheelite-type structure, and its pattern is the three-dimensional communication pore passage structure.Particularly, characteristics of the present invention are:
(1) adopts water-bath heating (being constant water bath box) preparation visible light catalyst BiVO
4Powder, technology is simple, energy consumption is low.
(2) do not use surfactant, reduced the synthetic cost of material.
(3) catalyst powder has the three-dimensional communication pore passage structure, the pattern novelty, and particle is little, has bigger specific area.
(4) degraded of industrial dye rhodamine B (RhB) has been had than the degradation rate of the material of conventional solid-state method preparation increased substantially.
Description of drawings
Fig. 1 is the three-dimensional communication pore structure BiVO that water-bath adds hot preparation
4XRD figure spectrum;
Fig. 2 is the three-dimensional communication pore structure BiVO that water-bath adds hot preparation
4Field emission scanning electron microscope figure;
Fig. 3 is the three-dimensional communication pore structure BiVO that water-bath adds hot preparation
4Transmission electron microscope picture;
Fig. 4 is the three-dimensional communication pore structure BiVO that water-bath adds hot preparation
4Pore size distribution curve;
Fig. 5 be the preparation sample under radiation of visible light, the concentration of RhB is curve over time.
The specific embodiment
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with example.
Example 1
2.4255g five water bismuth nitrate (Bi (NO
3)
35H
2O) being dissolved in 100ml ethylene glycol (EG), to be prepared into the Bi ion concentration be 0.05molL
-1Solution after, according to Bi: V=1: 1 adds 0.5849g ammonium metavanadate (NH
4VO
3), sonic oscillation 20min, and fully stirring is dissolved it fully.After treating the solution clear, transfer in the constant water bath box and be incubated 7 days acquisition flocky precipitates down in 60 ℃.The EG clear liquid is removed, and adding distil water washing, centrifugal so repeatedly after 5 times, with alcohol washing, centrifugal 2 times, is dried the sediment that obtains in baking oven.Dry thing is calcined 2.5h down, acquisition three-dimensional communication pore passage structure visible light catalyst BiVO in 400 ℃
4Through XRD analysis (Fig. 1), the principal phase of material is the pucherite of monoclinic system scheelite-type structure, corresponding standard card JCPD fileNo.01-075-1866.Field emission scanning electron microscope and transmission electron microscope results have been showed three-dimensional communication hole (Fig. 2) intuitively, and the existence of mesoporous (Fig. 3), and grain diameter is at 50～80nm, and mesoporous is 40～50nm.Pore size distribution curve (Fig. 4) has confirmed a kind of existence of macroporous/mesoporous hierarchy.
Photocatalytic activity is an evaluation model with the degraded rhodamine aqueous solution (RhB).The 350W xenon lamp adds the optical filter of 420nm as light source, and wavelength-filtered is less than the light wave of 420nm; Catalyst amount 50mg joins 5mgL
-1RhB solution 100ml in, after dark condition down stirs 1h, continuous light 4h, and every 1h sample thief point, get the change in concentration of clear liquid after centrifugal with ultraviolet-visible spectrophotometer test RhB, its degradation effect as shown in Figure 5, the sample of traditional solid sintering technology preparation is as reference.
Example 2
5.7916g five water acetic acid bismuth (Bi (CH
3COO)
35H
2O) being dissolved in 150ml ethylene glycol (EG) formation Bi ion concentration is 0.1molL
-1Behind the solution, according to Bi: V=1: 1.5, add 2.6320g ammonium metavanadate (NH
4VO
3), sonic oscillation 20min, and fully stirring makes its dissolving.After treating the solution clear, transfer in the constant water bath box and be incubated 2 days acquisition flocky precipitates down in 90 ℃.The EG clear liquid is removed, and adding distil water washing, centrifugal so repeatedly after 5 times, with alcohol washing, centrifugal 2 times, is dried the sediment that obtains in baking oven.Dry thing is calcined 3h down, acquisition three-dimensional communication pore passage structure visible light catalyst BiVO in 350 ℃
4
Example 3
3.1534g bismuth chloride (BiCl
3) being dissolved in 200ml ethylene glycol (EG), to form the Bi ion concentration be 0.5molL
-1Behind the solution, according to Bi: V=1: 2, add 3.6782g sodium vanadate (Na
3VO
4), sonic oscillation 20min, and fully stirring makes its dissolving.After treating the solution clear, transfer in the constant water bath box and be incubated 4 days acquisition flocky precipitates down in 80 ℃.The EG clear liquid is removed, and adding distil water washing, centrifugal so repeatedly after 5 times, with alcohol washing, centrifugal 2 times, is dried the sediment that obtains in baking oven.Dry thing is calcined 1.5h down, acquisition three-dimensional communication pore passage structure visible light catalyst BiVO in 500 ℃
4
Example 4
7.8835g bismuth chloride (BiCl
3) being dissolved in 100ml ethylene glycol (EG), to form the Bi ion concentration be 0.25molL
-1Behind the solution, according to Bi: V=1: 0.5, add 1.4623g ammonium metavanadate (NH
4VO
3), sonic oscillation 20min, and fully stirring makes its dissolving.After treating the solution clear, transfer in the constant water bath box and be incubated 10 days acquisition flocky precipitates down in 50 ℃.The EG clear liquid is removed, and adding distil water washing, centrifugal so repeatedly after 5 times, with alcohol washing, centrifugal 2 times, is dried the sediment that obtains in baking oven.Dry thing is calcined 1h down, acquisition three-dimensional communication pore passage structure visible light catalyst BiVO in 600 ℃
4
Example 5-18
Adopt each component and proportioning thereof in the table 1, can obtain required visible light catalyst BiVO equally according to example 1 to 4 described preparation process
4
Table 1
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment and accompanying drawing.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (3)
1. visible light catalyst BiVO
4, it is characterized in that this visible light catalyst BiVO
4Be powder, crystalline phase is the monoclinic system scheelite-type structure, and its pattern is the three-dimensional communication pore passage structure.
2. visible light catalyst BiVO
4The preparation method, it is characterized in that its step comprises:
(1) be to be dissolved in the ethylene glycol in 1: 0.5～1: 2 according to the mol ratio of the V ion in Bi ion and the vanadic salts in the bismuth salt, ultrasonic, stir, being prepared into the Bi ion concentration is 0.05～0.5molL
-1Settled solution;
(2) prepared settled solution is transferred in the constant water bath box, setting holding temperature is 50～90 ℃, and temperature retention time is 2～10 days;
(3) resulting precipitation distilled water centrifuge washing is used the alcohol centrifuge washing again, and oven dry evaporates residual alcohol, obtains powder;
(4) with the powder that obtains at 350～600 ℃ down behind calcining 1～3h, obtain visible light catalyst BiVO
4
3. visible light catalyst BiVO according to claim 2
4The preparation method is characterized in that, in the step (1), bismuth salt is nitrate, acetate or the villaumite that contains Bi, and vanadic salts is the vanadate that contains V.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489290A (en) * | 2011-11-11 | 2012-06-13 | 东华大学 | Preparation method of nano bismuth vanadate photocatalyst loaded on active carbon fiber |
| CN103950978A (en) * | 2014-04-09 | 2014-07-30 | 河南师范大学 | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure |
| CN106345496A (en) * | 2015-07-17 | 2017-01-25 | 广东工业大学 | Composite semiconductor photocatalytic material and preparation method thereof |
| CN108558703A (en) * | 2018-05-30 | 2018-09-21 | 徐州诺克非医药科技有限公司 | A kind of synthetic method of medicine intermediate chlorine ketone |
| CN108636420A (en) * | 2018-03-14 | 2018-10-12 | 西安建筑科技大学 | A kind of pucherite-franklinite composite photo-catalyst, preparation method and applications |
| CN108940314A (en) * | 2018-08-07 | 2018-12-07 | 东北大学秦皇岛分校 | A kind of comprehensive water-body processing BiVO4/ CdS compound and its preparation method and application |
| CN109331848A (en) * | 2018-11-15 | 2019-02-15 | 河海大学 | Visible light-responded Fe3O4Quantum dot modifies BiOCl/BiVO4Preparation method |
| CN109778304A (en) * | 2019-03-20 | 2019-05-21 | 广州大学 | A kind of vanadium doping bismuth sulfide nano line crystal film and its preparation method and application |
| CN109865512A (en) * | 2019-03-05 | 2019-06-11 | 西安理工大学 | A method of preparing α-bismuth niobate photocatalyst |
| CN110327965A (en) * | 2019-08-14 | 2019-10-15 | 齐鲁工业大学 | A kind of two dimension pucherite/graphene/carbonitride composite material and preparation method and application |
| CN112316936A (en) * | 2020-11-23 | 2021-02-05 | 华中科技大学 | BiVO4Interface photocatalyst, preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654397A (en) * | 2009-09-09 | 2010-02-24 | 山东大学 | Method for catalyzing and reducing ethanol with carbon dioxide under visible light |
-
2010
- 2010-04-22 CN CN 201010152232 patent/CN101791548A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101654397A (en) * | 2009-09-09 | 2010-02-24 | 山东大学 | Method for catalyzing and reducing ethanol with carbon dioxide under visible light |
Non-Patent Citations (1)
| Title |
|---|
| 《Eur. J. Inorg. Chem.》 20090910 Wenzong Yin et al. BiVO4 Hollow Nanospheres: Anchoring Synthesis, Growth Mechanism, and Their Application in Photocatalysis 第2009卷, 第29-30期 2 * |
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102489290A (en) * | 2011-11-11 | 2012-06-13 | 东华大学 | Preparation method of nano bismuth vanadate photocatalyst loaded on active carbon fiber |
| CN103950978A (en) * | 2014-04-09 | 2014-07-30 | 河南师范大学 | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure |
| CN103950978B (en) * | 2014-04-09 | 2015-03-11 | 河南师范大学 | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure |
| CN106345496B (en) * | 2015-07-17 | 2019-04-23 | 广东工业大学 | A kind of compound semiconductor photocatalytic material and preparation method thereof |
| CN106345496A (en) * | 2015-07-17 | 2017-01-25 | 广东工业大学 | Composite semiconductor photocatalytic material and preparation method thereof |
| CN108636420A (en) * | 2018-03-14 | 2018-10-12 | 西安建筑科技大学 | A kind of pucherite-franklinite composite photo-catalyst, preparation method and applications |
| CN108558703A (en) * | 2018-05-30 | 2018-09-21 | 徐州诺克非医药科技有限公司 | A kind of synthetic method of medicine intermediate chlorine ketone |
| CN108940314A (en) * | 2018-08-07 | 2018-12-07 | 东北大学秦皇岛分校 | A kind of comprehensive water-body processing BiVO4/ CdS compound and its preparation method and application |
| CN108940314B (en) * | 2018-08-07 | 2021-03-16 | 东北大学秦皇岛分校 | BiVO (BiVO) for comprehensive treatment of water body4/CdS compound and preparation method and application thereof |
| CN109331848A (en) * | 2018-11-15 | 2019-02-15 | 河海大学 | Visible light-responded Fe3O4Quantum dot modifies BiOCl/BiVO4Preparation method |
| CN109865512A (en) * | 2019-03-05 | 2019-06-11 | 西安理工大学 | A method of preparing α-bismuth niobate photocatalyst |
| CN109865512B (en) * | 2019-03-05 | 2022-02-01 | 西安理工大学 | Method for preparing alpha-bismuth niobate photocatalyst |
| CN109778304A (en) * | 2019-03-20 | 2019-05-21 | 广州大学 | A kind of vanadium doping bismuth sulfide nano line crystal film and its preparation method and application |
| CN109778304B (en) * | 2019-03-20 | 2020-07-31 | 广州大学 | Vanadium-doped bismuth sulfide nanowire crystal film and preparation method and application thereof |
| CN110327965A (en) * | 2019-08-14 | 2019-10-15 | 齐鲁工业大学 | A kind of two dimension pucherite/graphene/carbonitride composite material and preparation method and application |
| CN112316936A (en) * | 2020-11-23 | 2021-02-05 | 华中科技大学 | BiVO4Interface photocatalyst, preparation method and application thereof |
| CN112316936B (en) * | 2020-11-23 | 2022-03-29 | 华中科技大学 | BiVO4Interface photocatalyst, preparation method and application thereof |
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Open date: 20100804 |