CN110624531A - Preparation method and application of bismuth titanate photocatalyst - Google Patents
Preparation method and application of bismuth titanate photocatalyst Download PDFInfo
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- CN110624531A CN110624531A CN201910891317.1A CN201910891317A CN110624531A CN 110624531 A CN110624531 A CN 110624531A CN 201910891317 A CN201910891317 A CN 201910891317A CN 110624531 A CN110624531 A CN 110624531A
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- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 17
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 25
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910003074 TiCl4 Inorganic materials 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 53
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000007540 photo-reduction reaction Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 12
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 229910052797 bismuth Inorganic materials 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 229910052719 titanium Inorganic materials 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 2
- 239000010936 titanium Substances 0.000 abstract 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000007810 chemical reaction solvent Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 6
- 230000009467 reduction Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000010757 Reduction Activity Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000011426 transformation method Methods 0.000 description 1
Classifications
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
Abstract
A preparation method and application of a bismuth titanate photocatalyst, belongs to the technical field of photocatalytic materials, and aims to provide a preparation method of a novel high-efficiency photocatalytic material, which uses Bi (NO)3)3·5H2O is a bismuth source, TiCl4Or Ti (OC)4H9)4Taking a titanium source, deionized water or dilute nitric acid solution as a reaction solvent, sodium hydroxide as a mineralizer, reacting at 150-250 ℃ for 12-24 h, taking out, repeatedly washing the precipitate with absolute ethyl alcohol and deionized water until the surface is neutral, drying in an oven at 70 ℃ to obtain milky white powder, namely Bi4Ti3O12Bismuth titanate. The preparation process is mild and controllable, and has the advantages of simple process, easy operation and no by-product. Bi4Ti3O12Energy band structure and light-driven CO2The oxidation-reduction potential of the valence band and the conduction band required for producing CO is matched, and the CO-production catalyst shows excellent performanceDifferential activity, selectivity and stability.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a preparation method and application of a bismuth titanate photocatalyst.
Background
Solar light driven CO2The green conversion not only can solve the environmental problem caused by greenhouse effect, but also fully utilizes the renewable energy source solar energy, namely CO2One of the ideal ways of resource utilization.
The development of novel semiconductor photocatalytic material is that solar light drives CO2One of the key scientific problems of green conversion. At present, the unique layered structure and electronic structure of the Bi-containing photocatalytic material are very attractive high-activity photocatalytic material systems at present. Wherein, bismuth titanate (Bi)4Ti3O12) Containing two elements of Bi and Ti, is composed of [ Bi2O2]2+And [ Bi ]2Ti3O10]2-Perovskite layered structure [ formed alternatelyMater. Sci. Eng. B-Adv., 2018, 229: 160-172[ MEANS FOR solving PROBLEMS ] is provided. The first principle method is to calculate and find that Bi4Ti3O12The conduction band consists of Ti 3d and Bi 6p orbitals, the valence band is formed by hybridization of O2 p and Bi 6s orbitals, the generation and separation of photoexcited electron-hole pairs can be effectively promoted by the interaction between Bi and O atoms and the combination of the chemical states of Bi 6s and Bi 6p in the valence band and the conduction band, thereby reducing the band gap and increasing the response capability to visible light [ the band gapAppl. Catal. B: Environ., 2016, 180698 706 ]. Of particular importance is intrinsic Bi4Ti3O12The semiconductor has a valence band position of +2.85 eV and a conduction band position of-0.23 eV corresponding to the oxidation potential of water and CO2Reduction potential [Chem. Eng. J., 2019, 362: 588-599Is a photo-reduction of CO2The ideal material of the material.
Disclosure of Invention
The invention aims to provide a preparation method of a novel high-efficiency photocatalytic material, namely Bi4Ti3O12Has unique layered structure, can effectively reduce the recombination of electron-hole pairs, has proper band gap value and reasonable oxidation-reduction potential, and shows good light-driven reduction of CO2Capability. The photocatalytic material prepared by the method is used for solar light-driven reduction of CO2The method is simple and controllable, the process condition is mild, the raw materials are cheap and easy to obtain, and the method is used for preparing CO, and can be used for preparing CO with other CO2Compared with the reduction method, the process is carried out at normal temperature and normal pressure, solar energy is directly utilized without additional consumption of other energy, the carbon can be really recycled, and the CO is considered as the most promising CO2And (3) a transformation method.
The invention adopts the following technical scheme:
a preparation method of a bismuth titanate photocatalyst comprises the following steps:
first, 2.0-5.0 g Bi (NO)3)3·5H2Dissolving O in 20-40 mL of deionized water or dilute nitric acid to form a solution A;
second, 0.1-1 mL TiCl4Or Ti (OC)4H9)4Dropwise adding the mixed solution into 20-40 mL of deionized water to form a solution B, dissolving 4.0-10.0 g of NaOH in 30-60 mL of deionized water to form a solution C, and sequentially dropwise adding the solution B and the solution C into the solution A to form a solution D;
thirdly, stirring the solution D at room temperature for 0.5-1 h, transferring the solution D to a polytetrafluoroethylene reaction kettle, placing the reaction kettle in an oven, reacting at 150-250 ℃ for 12-24 h, taking out the reaction kettle, cooling the reaction kettle to room temperature, repeatedly washing the precipitate with absolute ethyl alcohol and deionized water until the surface of the precipitate is neutral, placing the precipitate in the oven for drying at 70 ℃, and obtaining a sample, namely Bi4Ti3O12Bismuth titanate.
Application of bismuth titanate photocatalyst to photo-reduction of CO2。
The invention has the following beneficial effects:
1. the invention combines TiO2With the characteristics of the Bi-based photocatalytic material, a photocatalyst containing Ti and Bi elements simultaneously is constructedThe material is converted to exert the synergistic effect of the electronic state energy level distribution of the two metal elements, so that the response to visible light is enhanced, the recombination of photo-generated electron hole pairs is reduced, and the catalytic activity is enhanced.
2. The invention provides a Bi4Ti3O12The preparation method of the photocatalyst has the advantages of simple and controllable method, mild process conditions, cheap and easily-obtained raw materials, no need of high temperature and high pressure, environment-friendly process, no generation of harmful byproducts and the like, and the prepared sample has the advantages of high efficiency of photo-reduction of CO2Capability.
Drawings
FIG. 1 shows Bi in example 1 of the present invention4Ti3O12An X-ray diffraction (XRD) pattern of the photocatalyst;
FIG. 2 shows Bi in example 2 of the present invention4Ti3O12An X-ray diffraction (XRD) pattern of the photocatalyst;
FIG. 3 shows Bi in example 3 of the present invention4Ti3O12An X-ray diffraction (XRD) pattern of the photocatalyst;
FIG. 4 shows Bi in examples 1 to 3 of the present invention4Ti3O12Different light source driven CO of photocatalyst2Reduction to CO yield is shown schematically.
Detailed Description
A preparation method of a bismuth titanate photocatalyst comprises the following steps:
first, 2.0-5.0 g Bi (NO)3)3·5H2Dissolving O in 20-40 mL of deionized water or dilute nitric acid to form a solution A;
second, 0.1-1 mL TiCl4Or Ti (OC)4H9)4Dropwise adding the mixed solution into 20-40 mL of deionized water to form a solution B, dissolving 4.0-10.0 g of NaOH in 30-60 mL of deionized water to form a solution C, and sequentially dropwise adding the solution B and the solution C into the solution A to form a solution D;
thirdly, stirring the solution D at room temperature for 0.5-1 h, transferring the solution D to a polytetrafluoroethylene reaction kettle, placing the reaction kettle in an oven, reacting at 150-250 ℃ for 12-24 h, taking out the reaction kettle, cooling the reaction kettle to room temperature, and adding absolute ethyl alcoholRepeatedly washing the precipitate with deionized water until the surface is neutral, drying in an oven at 70 deg.C to obtain a sample, i.e. Bi4Ti3O12Bismuth titanate.
The medicine reagents used in the invention are all analytically pure.
Example 1
1）2.0 g Bi(NO3)3·5H2Dissolving O in 20 mL of deionized water to form a solution A;
2）0.1 mL Ti(OC4H9)4dropwise adding the mixed solution into 20 mL of deionized water to form a solution B, dissolving 4.0 g of NaOH in 30 mL of deionized water to form a solution C, and sequentially dropwise adding the formed solution B and the formed solution C into the solution A to form a solution D;
3) stirring the solution D at room temperature for 1 h, transferring to a polytetrafluoroethylene reaction kettle, placing in an oven, reacting at 150 ℃ for 12 h, taking out, cooling the reaction kettle to room temperature, repeatedly washing the precipitate with absolute ethyl alcohol and deionized water until the surface is neutral, placing in the oven for drying at 70 ℃ to obtain a sample, namely Bi4Ti3O12Bismuth titanate.
Example 2
1）3.0 g Bi(NO3)3·5H2Dissolving O in 25 mL of deionized water to form a solution A;
2）0.5 mL TiCl4dropwise adding the mixed solution into 30 mL of deionized water to form a solution B, dissolving 8 g of NaOH into 40 mL of deionized water to form a solution C, and sequentially dropwise adding the formed solution B and the formed solution C into the solution A to form a solution D;
3) stirring the solution D at room temperature for 1 h, transferring to a polytetrafluoroethylene reaction kettle, placing in an oven, reacting at 180 ℃ for 16 h, taking out, cooling the reaction kettle to room temperature, repeatedly washing the precipitate with absolute ethyl alcohol and deionized water until the surface is neutral, placing in the oven for drying at 70 ℃ to obtain a sample, namely Bi4Ti3O12Bismuth titanate.
Example 3
1）5.0 g Bi(NO3)3·5H2Dissolving O in 40 mL of dilute nitric acid solution to form a solution A;
2）1 mL Ti(OC4H9)4dropwise adding the mixed solution into 40 mL of deionized water to form a solution B, dissolving 10 g of NaOH into 60 mL of deionized water to form a solution C, and sequentially dropwise adding the formed solution B and the formed solution C into the solution A to form a solution D;
3) stirring the solution D at room temperature for 1 h, transferring the solution D to a polytetrafluoroethylene reaction kettle, placing the reaction kettle in an oven, reacting at 250 ℃ for 18 h, taking out the reaction kettle, cooling the reaction kettle to room temperature, repeatedly washing the precipitate with absolute ethyl alcohol and deionized water until the surface of the precipitate is neutral, placing the precipitate in the oven at 70 ℃ for drying, and obtaining a sample, namely Bi4Ti3O12Bismuth titanate.
Example 4
Bi prepared by examples 1 to 3 of the present invention4Ti3O12Photocatalyst for CO2The reduction activity test comprises the following specific steps: 0.02 g of photocatalyst is put into 50 mL of water, the photoreactor system is vacuumized, and a certain amount of CO is introduced into a closed circulating system2. Under the irradiation of ultraviolet light, visible light and simulated sunlight, the gas chromatography automatically samples and analyzes once every 1 h, and the measured CO yield of the gas phase reduction product is respectively 30.4, 15.2 and 40.7; 47.2, 20.6 and 50.2; 77.2, 30.5 and 103.4. mu. mol. g-1·h-1。
Claims (2)
1. A preparation method of a bismuth titanate photocatalyst is characterized by comprising the following steps: the method comprises the following steps:
first, 2.0-5.0 g Bi (NO)3)3·5H2Dissolving O in 20-40 mL of deionized water or dilute nitric acid to form a solution A;
second, 0.1-1 mL TiCl4Or Ti (OC)4H9)4Dropwise adding the mixed solution into 20-40 mL of deionized water to form a solution B, dissolving 4.0-10.0 g of NaOH in 30-60 mL of deionized water to form a solution C, and sequentially dropwise adding the solution B and the solution C into the solution A to form a solution D;
thirdly, stirring the solution D at room temperature for 0.5-1 h, transferring the solution D to a polytetrafluoroethylene reaction kettle, placing the reaction kettle in an oven, and reacting at 150-250 DEG CTaking out after 12-24 h, cooling the reaction kettle to room temperature, repeatedly washing the precipitate with absolute ethyl alcohol and deionized water until the surface is neutral, and drying in an oven at 70 ℃ to obtain a sample, namely Bi4Ti3O12Bismuth titanate.
2. Application of bismuth titanate photocatalyst to photo-reduction of CO2。
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Cited By (4)
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| CN112023912A (en) * | 2020-08-31 | 2020-12-04 | 陕西科技大学 | Bismuth-based photocatalyst loaded with elemental bismuth and preparation method and application thereof |
| CN112516990A (en) * | 2020-12-22 | 2021-03-19 | 南京工业大学 | Synthetic method and application of layered perovskite type photocatalyst |
| CN112745841A (en) * | 2020-12-25 | 2021-05-04 | 广西大学 | Alkali metal reinforced bismuth titanate-based up-conversion fluorescent material and preparation method thereof |
| CN115318274A (en) * | 2022-08-10 | 2022-11-11 | 齐鲁工业大学 | Bismuth/bismuth titanate heterojunction hollow nanosphere and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112023912A (en) * | 2020-08-31 | 2020-12-04 | 陕西科技大学 | Bismuth-based photocatalyst loaded with elemental bismuth and preparation method and application thereof |
| CN112023912B (en) * | 2020-08-31 | 2023-06-13 | 陕西科技大学 | Bismuth-based photocatalyst loaded with elemental bismuth, and preparation method and application thereof |
| CN112516990A (en) * | 2020-12-22 | 2021-03-19 | 南京工业大学 | Synthetic method and application of layered perovskite type photocatalyst |
| CN112745841A (en) * | 2020-12-25 | 2021-05-04 | 广西大学 | Alkali metal reinforced bismuth titanate-based up-conversion fluorescent material and preparation method thereof |
| CN115318274A (en) * | 2022-08-10 | 2022-11-11 | 齐鲁工业大学 | Bismuth/bismuth titanate heterojunction hollow nanosphere and preparation method and application thereof |
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Application publication date: 20191231 |