CN105056935A - Indium oxide-bismuth vanadate compound photocatalyst as well as preparation method and application of photocatalyst - Google Patents
Indium oxide-bismuth vanadate compound photocatalyst as well as preparation method and application of photocatalyst Download PDFInfo
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- CN105056935A CN105056935A CN201510501356.8A CN201510501356A CN105056935A CN 105056935 A CN105056935 A CN 105056935A CN 201510501356 A CN201510501356 A CN 201510501356A CN 105056935 A CN105056935 A CN 105056935A
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Abstract
The invention discloses a preparation method and application of a novel indium oxide-bismuth vanadate compound photocatalyst. The preparation method comprises the following steps: (1) dissolving bismuth nitrate powder and indium nitrate powder into nitric acid to prepare an acidic mixed solution, and dissolving ammonium metavanadate into a sodium hydroxide solution to prepare a sodium vanadate solution; (2) then mixing the solutions prepared in the step (1), stirring to generate an orange-yellow sediment, then adding an alkaline solution to adjust the pH value to be 7, and fully stirring; (3) conducting hydrothermal reaction on a mixed solution obtained in the step (2), and conducting calcination to prepare the indium oxide-bismuth vanadate compound photocatalyst. The method is low in production cost, simple and feasible, and the photocatalyst has high visible-light activity, and can be utilized for photocatalysis to degrade methyl blue (MB).
Description
Technical field
The present invention relates to inorganic nano photocatalyst material field, particularly a kind of composite photo-catalyst and preparation method thereof.
Background technology
Light-catalyzed reaction is that photocatalyst material utilizes luminous energy to carry out a kind of mode of Substance Transformation, is a kind of chemical reaction carried out under material acts on catalyst and light while.Photocatalysis is by the emerging research field of numerous subject crossing such as catalytic chemistry, Semiconductor Physics, Optical Electro-Chemistry, environmental science and material science.When world today's problem of environmental pollution and energy crisis more and more serious; photocatalysis technology can directly utilize solar energy as reaction light source to drive the feature of reaction using it, and becomes a kind of environmental pollution of getting most of the attention and repair purification techniques and clean energy resource production technology.Utilize photocatalysis technology, can realize the degraded of organic pollutions all types of in environment, making it final mineralising is avirulent carbon dioxide and water, thus realizes the purification of water body and air; Solar energy can be converted into again can for the electric energy of the mankind; Sunshine photocatalytic water can also be utilized to produce clean energy hydrogen, thus substitute the mankind be about to exhausted fossil fuel etc. can not the energy again.
Traditional photocatalytic semiconductor material titanium dioxide makes because of its wide energy gap the ultraviolet light utilized in solar spectrum that it can only be limited, but cannot utilize visible ray.So, increasing researcher start more energy put into explore and find have visible light-responded while there is the novel photocatalyst of high catalytic activity.In the last few years, many researchers found, band-gap energy is that the pucherite of 2.4eV possesses very high photoresponse ability at visible region, can, at light degradation organic pollution under visible light conditions, be a kind of photochemical catalyst having very much potential use.But simple pucherite is also faced with some problems as photochemical catalyst, such as: specific area is too small, adsorption capacity is poor, and photo-generated carrier is difficult to be separated, and the easy compound of electron hole pair etc., these defects all limit the photocatalysis performance of pucherite.
Summary of the invention
The problem to be solved in the present invention is, it is too small that traditional pucherite monolithic catalyst has specific area, adsorption capacity is poor, and photo-generated carrier is difficult to be separated, the defects such as the easy compound of electron hole pair, these defects all limit the photocatalysis performance of pucherite, construct one and can promote that electric charge is efficiently separated, indium oxide Nanoparticle Modified composite bismuth vanadium photocatalyst with highlight catalytic active and preparation method thereof, in this composite photo-catalyst, indium oxide nano particle is compound in the surface of pucherite discretely, be conducive to exposing highly active indium oxide-pucherite boundary, at environment pollution control, the fields such as the energy are with a wide range of applications, the preparation method of this composite photo-catalyst is simple, with low cost, reproducible simultaneously, can meet volume production requirement well.
A preparation method for indium oxide-composite bismuth vanadium photocatalyst, comprises the steps:
(1) bismuth nitrate and indium nitrate powder are dissolved in obtained acid mixed solution in nitric acid, ammonium metavanadate are dissolved in sodium hydroxide solution and are mixed with sodium vanadate solution; Wherein, the mol ratio of ammonium metavanadate and bismuth nitrate, indium nitrate is 1:1:1;
(2) then by solution mixing obtained for step (1), stir, generate orange-yellow sediment, then adding alkaline solution adjust ph is 7, fully stirs;
(3) mixed liquor step (2) obtained after hydro-thermal reaction, then is calcined, i.e. obtained indium oxide-composite bismuth vanadium photocatalyst.
The temperature of step (3) hydro-thermal reaction is 150 ~ 200 DEG C, and the reaction time is 20 ~ 30h; Calcining heat is 400 ~ 600 DEG C, and calcination time is 1.5 ~ 3.0h.
The temperature of step (3) hydro-thermal reaction is 180 DEG C, and the reaction time is 24h; Calcining heat is 500 DEG C, and calcination time is 2h.
Described step (2) described alkaline solution is sodium hydroxide solution.
Product after described hydro-thermal reaction is cooled to room temperature, after washed with de-ionized water, calcines after filtration, drying, grinding again.
The temperature of described drying is 60 DEG C, and the time is 24h.
The concentration of step (1) described nitric acid is 4M, and the concentration of sodium hydroxide solution is 4M.
Indium oxide-composite bismuth vanadium photocatalyst prepared by said method, described pucherite is block, and diameter is 500-600nm, and indium oxide nano particle is compound in pucherite surface discretely, and the particle diameter of described indium oxide nano particle is 10-50nm.
Both indium oxide and pucherite are carried out compound by the present invention, it is a kind of effective modification technology that indium oxide and pucherite carry out compound, pass through compound, indium oxide-pucherite heterojunction structure is built between indium oxide and pucherite, in heterojunction structure, light induced electron and hole respectively to pucherite and indium oxide transfer, thus improve the separative efficiency of photogenerated charge, realize effective separation of photo-generated carrier, and then improve the photocatalysis performance of material.Composite photo-catalyst of the present invention under visible light, can carry out Methyl blueness (MB).
Compared with prior art, tool of the present invention has the following advantages:
(1) the present invention constructs the discrete composite photo-catalyst being compound in pucherite of a kind of indium oxide nano particle, this is compared with traditional block pucherite monolithic catalyst, composite catalyst possesses larger specific area, is conducive to the catalytic activity improving catalyst.
(2) indium oxide-composite bismuth vanadium photocatalyst of preparing of the present invention, possesses the visible light-responded ability better than traditional pucherite monolithic catalyst, is conducive to the catalytic activity improving catalyst.
(3) present invention achieves the compound of indium oxide and pucherite, define indium oxide-pucherite heterojunction structure, this structure is very beneficial for the separation of photo-generated carrier, reduces the combined efficiency of electron hole pair, improves the catalytic performance of catalyst.
(4) preparation method of the present invention is simple, with low cost, reproducible, low to the requirement of equipment, can meet volume production requirement well.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of the indium oxide-composite bismuth vanadium photocatalyst prepared by embodiment 1;
Fig. 2 is the transmission electron microscope picture (TEM) of the indium oxide-composite bismuth vanadium photocatalyst prepared by embodiment 1;
Fig. 3 is the XRD collection of illustrative plates of the indium oxide-composite bismuth vanadium photocatalyst prepared by embodiment 1;
Fig. 4 is the uv-visible absorption spectra figure (UV-Vis) of the indium oxide-composite bismuth vanadium photocatalyst prepared by embodiment 1;
Fig. 5 is the indium oxide-composite bismuth vanadium photocatalyst Methyl blueness design sketch under visible light prepared by embodiment 1, is referenced as blank, pure indium oxide and pucherite.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is more specifically described in detail, but embodiments of the present invention are not limited thereto, for the technological parameter do not indicated especially, can refer to routine techniques and carry out.
Embodiment 1
Under normal temperature and pressure, take the Bi (NO of 2.42g
3)
35H
2in (the NO of O and 1.95g
3)
35H
2o powder, in beaker A, adds the nitric acid that 20mL concentration is 4M, obtains settled solution after fully stirring; Separately take the NH with 0.58g
4vO
3in beaker B, add the NaOH that 20mL concentration is 4M, after fully stirring, obtain settled solution; Then when rapid stirring, dropwise in A beaker to be added in B beaker in solution, obtain orange-yellow sediment, add the NaOH solution that concentration is 1M, adjusted to ph is 7, after fully stirring 30min, is transferred in the hydrothermal reaction kettle of 100mL by this orange solution, under 180 DEG C of conditions, hydro-thermal reaction 24h.To be cooled to room temperature, by product with after washed with de-ionized water several, the baking oven being placed in 60 DEG C processes 24h, is positioned in the Muffle furnace of 500 DEG C after cooling through mortar process again, calcining 2h.To be cooled to room temperature, by gained powder agate mortar porphyrize, obtain In
2o
3/ BiVO
4composite catalyst powder 2.54g.
Embodiment 2
Under normal temperature and pressure, take the Bi (NO of 4.82g
3)
35H
2in (the NO of O and 3.90g
3)
35H
2o powder, in beaker A, adds the nitric acid that 20mL concentration is 4M, obtains settled solution after fully stirring; Separately take the NH with 1.16g
4vO
3in beaker B, add the NaOH that 20mL concentration is 4M, after fully stirring, obtain settled solution; Then when rapid stirring, dropwise in A beaker to be added in B beaker in solution, obtain orange-yellow sediment, add the NaOH solution that concentration is 1M, adjusted to ph is 7, after fully stirring 30min, is transferred in the hydrothermal reaction kettle of 100mL by this orange solution, under 180 DEG C of conditions, hydro-thermal reaction 24h.To be cooled to room temperature, by product with after washed with de-ionized water several, the baking oven being placed in 60 DEG C processes 24h, is positioned in the Muffle furnace of 500 DEG C after cooling through mortar process again, calcining 2h.To be cooled to room temperature, by gained powder agate mortar porphyrize, obtain In
2o
3/ BiVO
4composite catalyst powder 5.34g.
Embodiment 3
Under normal temperature and pressure, take the Bi (NO of 4.82g
3)
35H
2in (the NO of O and 3.91g
3)
35H
2o powder, in beaker A, adds the nitric acid that 20mL concentration is 4M, obtains settled solution after fully stirring; Separately take the NH with 1.16g
4vO
3in beaker B, add the NaOH that 20mL concentration is 4M, after fully stirring, obtain settled solution; Then when rapid stirring, dropwise in A beaker to be added in B beaker in solution, obtain orange-yellow sediment, add the NaOH solution that concentration is 1M, adjusted to ph is 7, after fully stirring 30min, is transferred in the hydrothermal reaction kettle of 100mL by this orange-yellow sediment, under 180 DEG C of conditions, hydro-thermal reaction 24h.To be cooled to room temperature, by product with after washed with de-ionized water several, the baking oven being placed in 60 DEG C processes 24h, is positioned in the Muffle furnace of 500 DEG C after cooling through mortar process again, calcining 2h.To be cooled to room temperature, by gained powder agate mortar porphyrize, obtain In
2o
3/ BiVO
4composite catalyst powder 5.46g.
Claims (10)
1. a preparation method for indium oxide-composite bismuth vanadium photocatalyst, is characterized in that, comprises the steps:
(1) bismuth nitrate and indium nitrate powder are dissolved in obtained acid mixed solution in nitric acid, ammonium metavanadate are dissolved in sodium hydroxide solution and are mixed with sodium vanadate solution;
(2) then by solution mixing obtained for step (1), stir, generate orange-yellow sediment, then adding alkaline solution adjust ph is 7, fully stirs;
(3) mixed liquor step (2) obtained after hydro-thermal reaction, then is calcined, i.e. obtained indium oxide-composite bismuth vanadium photocatalyst.
2. method according to claim 1, is characterized in that, the mol ratio of step (1) described ammonium metavanadate and bismuth nitrate, indium nitrate is 1:1:1.
3. method according to claim 2, is characterized in that, the temperature of step (3) hydro-thermal reaction is 150 ~ 200 DEG C, and the reaction time is 20 ~ 30h; Calcining heat is 400 ~ 600 DEG C, and calcination time is 1.5 ~ 3.0h.
4. method according to claim 3, is characterized in that, the temperature of step (3) hydro-thermal reaction is 180 DEG C, and the reaction time is 24h; Calcining heat is 500 DEG C, and calcination time is 2h.
5. the preparation method according to claim 1 or 2 or 3 or 4, it is characterized in that, described step (2) described alkaline solution is sodium hydroxide solution.
6. the preparation method according to claim 1 or 2 or 3 or 4, it is characterized in that, the product after described hydro-thermal reaction is cooled to room temperature, after washed with de-ionized water, calcines after filtration, drying, grinding again.
7. the method according to claim 1 or 2 or 3 or 4, is characterized in that, the temperature of described drying is 60 DEG C, and the time is 24h.
8. the method according to claim 1 or 2 or 3 or 4, it is characterized in that, the concentration of step (1) described nitric acid is 4M, the concentration of sodium hydroxide solution is 4M.
9. indium oxide-composite bismuth vanadium photocatalyst of preparing of claim 1 ~ 8 any one method, it is characterized in that, described pucherite is block, and diameter is 500-600nm, indium oxide nano particle is compound in pucherite surface discretely, and the particle diameter of described indium oxide nano particle is 10-50nm.
10. the application of composite photo-catalyst described in claim 9, is characterized in that, described composite photo-catalyst is used for carrying out Methyl blueness under visible light.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115582113A (en) * | 2022-09-23 | 2023-01-10 | 南昌大学 | General synthesis method for in-situ construction of indium oxide modified zinc oxide-zinc sulfide heterostructure photocatalytic water splitting hydrogen production material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012008838A1 (en) * | 2010-07-16 | 2012-01-19 | Universiteit Twente | Photocatalytic water splitting |
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012008838A1 (en) * | 2010-07-16 | 2012-01-19 | Universiteit Twente | Photocatalytic water splitting |
| CN103623803A (en) * | 2012-08-30 | 2014-03-12 | 上海纳晶科技有限公司 | Visible light photocatalyst and preparation method therefor |
Non-Patent Citations (1)
| Title |
|---|
| J.Z.YIN ET AL: ""Enhancement of the visible light photocatalytic activity of heterojunction In2O3/BiVO4 composites"", 《APPLIED PHYSICS A》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115582113A (en) * | 2022-09-23 | 2023-01-10 | 南昌大学 | General synthesis method for in-situ construction of indium oxide modified zinc oxide-zinc sulfide heterostructure photocatalytic water splitting hydrogen production material |
| CN115582113B (en) * | 2022-09-23 | 2023-08-29 | 南昌大学 | General synthesis method for in-situ construction of indium oxide modified zinc oxide-zinc sulfide heterostructure photocatalytic water splitting hydrogen production material |
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Application publication date: 20151118 |