CN108927137B - A kind of preparation method of carbon-doped bismuth oxide photocatalytic material - Google Patents
A kind of preparation method of carbon-doped bismuth oxide photocatalytic material Download PDFInfo
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- CN108927137B CN108927137B CN201810799992.7A CN201810799992A CN108927137B CN 108927137 B CN108927137 B CN 108927137B CN 201810799992 A CN201810799992 A CN 201810799992A CN 108927137 B CN108927137 B CN 108927137B
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- bismuth oxide
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 31
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 11
- GEVPUGOOGXGPIO-UHFFFAOYSA-N oxalic acid;dihydrate Chemical compound O.O.OC(=O)C(O)=O GEVPUGOOGXGPIO-UHFFFAOYSA-N 0.000 claims abstract description 8
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 13
- 238000000137 annealing Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 3
- 230000031700 light absorption Effects 0.000 abstract description 4
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 abstract 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Natural products OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 abstract 1
- 229940116316 dihydrate oxalic acid Drugs 0.000 abstract 1
- 230000005693 optoelectronics Effects 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000004298 light response Effects 0.000 description 2
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/18—Arsenic, antimony or bismuth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
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Abstract
本发明公开了一种碳掺杂氧化铋光催化材料的制备方法，将五水硝酸铋置于氧化铝坩埚中于500℃退火6h制得α‑Bi2O3粉末材料，再将制得的α‑Bi2O3粉末材料置于氧化铝坩埚中，加入二水合草酸粉末并混合均匀后于280℃退火50～200min制得碳掺杂氧化铋光催化材料。本发明制备过程简单可行，合成周期较短，相对于未掺杂的氧化铋，碳掺杂氧化铋光催化材料的光吸收边向长波方向移动，在400～500nm可见光波长范围内对光波的利用率较大，且光催化性能得到明显提升，在光电材料方面具有潜在应用价值。
The invention discloses a preparation method of carbon-doped bismuth oxide photocatalytic material. The bismuth nitrate pentahydrate is placed in an alumina crucible and annealed at 500 DEG C for 6 hours to obtain α-Bi 2 O 3 powder material, and then the prepared The α-Bi 2 O 3 powder material is placed in an alumina crucible, and the dihydrate oxalic acid powder is added and mixed uniformly, and then annealed at 280° C. for 50-200 min to obtain a carbon-doped bismuth oxide photocatalytic material. Compared with undoped bismuth oxide, the light absorption edge of the carbon-doped bismuth oxide photocatalytic material moves to the long wave direction, and the light wave is utilized in the visible light wavelength range of 400-500 nm. The photocatalytic performance is significantly improved, and it has potential application value in optoelectronic materials.
Description
Technical Field
The invention belongs to the technical field of synthesis of photoelectric materials, and particularly relates to a preparation method of a carbon-doped bismuth oxide photocatalytic material.
Background
The bismuth resource in China is rich, the annual output can reach more than 6000 tons in recent years, and the application is very wide. Bismuth-oxygen-based materials have a layered crystal structure, a proper forbidden band width and a special electronic structure of bismuth atoms, often show high activity in actual photocatalytic reactions, become an important photocatalytic material, and have received wide attention. Bismuth oxide is widely used for the manufacture of drugs and bismuth salts as a product after deep processing of bismuth source. Bismuth oxide belongs to bismuth-oxygen-based materials, is light yellow in appearance, has limited visible light response capability and lower photocatalytic activity. Based on the existing problems, the invention designs a preparation method of a carbon-doped bismuth oxide photocatalytic material with enhanced visible light response and improved photocatalytic activity.
Disclosure of Invention
The invention solves the technical problem of providing a preparation method of the carbon-doped bismuth oxide photocatalytic material with simple synthesis process and shorter period.
The invention adopts the following technical scheme for solving the technical problems, and the preparation method of the carbon-doped bismuth oxide photocatalytic material is characterized by comprising the following specific steps of: putting bismuth nitrate pentahydrate into an alumina crucible, and annealing for 6 hours at 500 ℃ to prepare alpha-Bi2O3Powder material, and the prepared alpha-Bi2O3And placing the powder material in an alumina crucible, adding oxalic acid dihydrate powder, uniformly mixing, and annealing at 280 ℃ for 50-200 min to obtain the carbon-doped bismuth oxide photocatalytic material.
Preferably, the alpha-Bi2O3The feeding mass ratio of the powder material to the oxalic acid dihydrate powder is 1: 1-1: 2.
The preparation method is simple and feasible in preparation process and short in synthesis period, compared with undoped bismuth oxide, the carbon-doped bismuth oxide photocatalytic material has the advantages that the light absorption edge moves towards the long-wave direction, the utilization rate of light waves in the visible light wavelength range of 400-500 nm is high, the photocatalytic performance is obviously improved, and the carbon-doped bismuth oxide photocatalytic material has potential application value in the aspect of photoelectric materials.
Drawings
FIG. 1 is an X-ray diffraction pattern of a carbon-doped bismuth oxide powder material prepared in example 1 of the present invention;
FIG. 2 is a powder absorption spectrum of a carbon-doped bismuth oxide powder material obtained in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of a carbon-doped bismuth oxide powder material prepared according to example 1 of the present invention;
FIG. 4 is a performance curve of rhodamine B degradation catalyzed by visible light of the carbon-doped bismuth oxide powder material prepared in example 1 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
4.85g of bismuth nitrate pentahydrate is put into an alumina crucible to be annealed for 6 hours at 500 ℃ to prepare alpha-Bi2O3Powder material, and 0.5g of the obtained alpha-Bi2O3The powder material is placed in an alumina crucible, added with 1.0g of oxalic acid dihydrate powder and annealed for 200min at 280 ℃ after being mixed evenly, thus obtaining the carbon-doped bismuth oxide powder material.
XRD analysis of the prepared carbon-doped bismuth oxide powder material revealed that the carbon-doped bismuth oxide powder material and α -Bi were present as shown in FIG. 12O3The diffraction peaks of the powder material are consistent with those of standard JCPDS cards 71-2274, no impurity peak appears, and the chemical formula is Bi2O3The crystal structure is monoclinic phase.
As shown in FIG. 2, the prepared carbon-doped bismuth oxide powder material is compared with alpha-Bi2O3The absorption of light by the powder material is enhanced and the wavelength band of light absorption appears red-shifted.
As shown in FIG. 3, the obtained carbon-doped bismuth oxide powder material has a prismatic morphology and many fine pores are distributed on the surface.
As shown in FIG. 4, after being excited by visible light for 120min, the degradation rate of the carbon-doped bismuth oxide powder material for degrading rhodamine B pollutants is 99.7%, which is much higher than that of undoped bismuth oxide.
Example 2
4.85g of bismuth nitrate pentahydrate is put into an alumina crucible to be annealed for 6 hours at 500 ℃ to prepare alpha-Bi2O3The product, 0.5g of the obtained alpha-Bi2O3The product is put into an alumina crucible, added with 0.5g of oxalic acid dihydrate powder, evenly mixed and annealed for 200min at 280 ℃ to prepare the carbon-doped bismuth oxide powder material.
Example 3
4.85g of bismuth nitrate pentahydrate is put into an alumina crucible to be annealed for 6 hours at 500 ℃ to prepare alpha-Bi2O3The product, 0.5g of the obtained alpha-Bi2O3The product is placed in aluminaAdding 1.0g of oxalic acid dihydrate powder into the crucible, uniformly mixing, and annealing at 280 ℃ for 50min to obtain the carbon-doped bismuth oxide powder material.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (1)
1. A preparation method of a carbon-doped bismuth oxide photocatalytic material is characterized by comprising the following specific steps: putting bismuth nitrate pentahydrate into an alumina crucible, and annealing for 6 hours at 500 ℃ to prepare alpha-Bi2O3Powder material, and the prepared alpha-Bi2O3Placing the powder material in an alumina crucible, adding oxalic acid dihydrate powder, uniformly mixing, and annealing at 280 ℃ for 50-200 min to obtain the carbon-doped bismuth oxide photocatalytic material, wherein alpha-Bi is2O3The feeding mass ratio of the powder material to the oxalic acid dihydrate powder is 1: 1-1: 2.
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| US7578455B2 (en) * | 2004-08-09 | 2009-08-25 | General Motors Corporation | Method of grinding particulate material |
| CN103521211A (en) * | 2013-10-31 | 2014-01-22 | 北京航空航天大学 | A kind of preparation method of In-doped Bi2O3 photocatalytic material |
| CN104148047A (en) * | 2014-08-31 | 2014-11-19 | 华东理工大学 | Macro preparation method for carbon doped zinc oxide-based visible-light catalyst |
| CN105268462A (en) * | 2015-07-03 | 2016-01-27 | 西南石油大学 | Preparation method of nitrogen doped bismuth-containing oxides at low temperature |
| CN106379938A (en) * | 2016-09-10 | 2017-02-08 | 河南师范大学 | A kind of method for preparing black α-Bi2O3 powder material |
| CN107552034A (en) * | 2017-08-21 | 2018-01-09 | 信阳师范学院 | A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet |
| CN107570214A (en) * | 2017-10-12 | 2018-01-12 | 湖北工业大学 | Possesses the preparation method of the paper substrate bismuth ferrite composite of multiphase adsoption catalysis function |
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Patent Citations (7)
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| US7578455B2 (en) * | 2004-08-09 | 2009-08-25 | General Motors Corporation | Method of grinding particulate material |
| CN103521211A (en) * | 2013-10-31 | 2014-01-22 | 北京航空航天大学 | A kind of preparation method of In-doped Bi2O3 photocatalytic material |
| CN104148047A (en) * | 2014-08-31 | 2014-11-19 | 华东理工大学 | Macro preparation method for carbon doped zinc oxide-based visible-light catalyst |
| CN105268462A (en) * | 2015-07-03 | 2016-01-27 | 西南石油大学 | Preparation method of nitrogen doped bismuth-containing oxides at low temperature |
| CN106379938A (en) * | 2016-09-10 | 2017-02-08 | 河南师范大学 | A kind of method for preparing black α-Bi2O3 powder material |
| CN107552034A (en) * | 2017-08-21 | 2018-01-09 | 信阳师范学院 | A kind of simple, quick method for preparing carbon doping Zinc oxide nano sheet |
| CN107570214A (en) * | 2017-10-12 | 2018-01-12 | 湖北工业大学 | Possesses the preparation method of the paper substrate bismuth ferrite composite of multiphase adsoption catalysis function |
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