CN109201089B - Preparation method of europium and selenium codoped titanium dioxide graphene oxide material for photocatalysis - Google Patents
Preparation method of europium and selenium codoped titanium dioxide graphene oxide material for photocatalysis Download PDFInfo
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- CN109201089B CN109201089B CN201811305026.1A CN201811305026A CN109201089B CN 109201089 B CN109201089 B CN 109201089B CN 201811305026 A CN201811305026 A CN 201811305026A CN 109201089 B CN109201089 B CN 109201089B
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- butyl titanate
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 22
- 239000011669 selenium Substances 0.000 title claims abstract description 18
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000004408 titanium dioxide Substances 0.000 title abstract description 5
- 229910052693 Europium Inorganic materials 0.000 title abstract description 4
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 title abstract description 4
- 238000007146 photocatalysis Methods 0.000 title abstract description 4
- 229910052711 selenium Inorganic materials 0.000 title abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 47
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims abstract description 23
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(3+);trinitrate Chemical compound [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000019441 ethanol Nutrition 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000001291 vacuum drying Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims description 20
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000011941 photocatalyst Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 239000000047 product Substances 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
-
- 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
- C01B32/50—Carbon dioxide
Abstract
The invention relates to a preparation method of a europium and selenium codoped titanium dioxide graphene oxide material for photocatalysis, which comprises the following steps: (1) dispersing selenium powder and graphene oxide in an acetic acid solution, adding a europium nitrate solution, and uniformly stirring to obtain a component A for later use; (2) at room temperature, dropwise adding the component A obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate, stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, sequentially washing the precipitate with ethanol and water, and vacuum-drying at 60 ℃ for 24h to obtain the Eu3+Se co-doping of TiO2a/GO material.
Description
Technical Field
The invention belongs to the field of photocatalytic materials, and particularly relates to a preparation method of a europium and selenium codoped titanium dioxide graphene oxide material for photocatalysis.
Background
The conventional titanium dioxide greatly limits the application thereof due to poor response to visible light, and the inventor found that Eu previously3 +Se co-doping of TiO2the/GO material can catalyze isopropanol to be oxidized into acetone under visible light, the acetone has high selectivity, and further research shows that the Eu is3+Se co-doping of TiO2the/GO material can also be used to catalytically oxidize acetaldehyde in the visible.
Disclosure of Invention
The invention provides a Eu3+Se co-doping of TiO2a/GO material, characterized in that said Eu3+Se co-doping of TiO2The preparation method of the/GO material comprises the following steps:
(1) dispersing selenium powder and graphene oxide in an acetic acid solution, adding a europium nitrate solution, and uniformly stirring to obtain a component A for later use;
(2) at room temperature, dropwise adding the component A obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate, stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, sequentially washing the precipitate with ethanol and water, and vacuum-drying at 60 ℃ for 24h to obtain the Eu3+Se co-doping of TiO2a/GO material.
In the step (1), the mass ratio of the selenium powder to the graphene oxide is 1:20, the concentration of an acetic acid solution is 1mol/L, the concentration of a europium nitrate solution is 0.1mol/L, 25mL of acetic acid solution is used for every gram of graphene oxide, and 10mL of europium nitrate solution is used; in the step (2), the absolute ethyl alcohol solution of the n-butyl titanate is prepared from the n-butyl titanate and absolute ethyl alcohol according to the mass ratio of 1:5, and the using amount of the n-butyl titanate is 2 times of the mass of the graphene oxide used for preparing the component A.
Another embodiment of the present invention provides the above Eu3+Se co-doping of TiO2The preparation method of the/GO material is characterized by comprising the following steps:
(1) dispersing selenium powder and graphene oxide in an acetic acid solution, adding a europium nitrate solution, and uniformly stirring to obtain a component A for later use;
(2) at room temperature, dropwise adding the component A obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate, stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, sequentially washing the precipitate with ethanol and water, and vacuum-drying at 60 ℃ for 24h to obtain the Eu3+Se co-doping of TiO2a/GO material.
In the step (1), the mass ratio of the selenium powder to the graphene oxide is 1:20, the concentration of an acetic acid solution is 1mol/L, the concentration of a europium nitrate solution is 0.1mol/L, 25mL of acetic acid solution is used for every gram of graphene oxide, and 10mL of europium nitrate solution is used; in the step (2), the absolute ethyl alcohol solution of the n-butyl titanate is prepared from the n-butyl titanate and absolute ethyl alcohol according to the mass ratio of 1:5, and the using amount of the n-butyl titanate is 2 times of the mass of the graphene oxide used for preparing the component A.
Another embodiment of the present invention provides the above Eu3+Se co-doping of TiO2Use of a/GO material as a photocatalyst. Preferably in applications where visible light is used to photocatalytically oxidize acetaldehyde to carbon dioxide.
Drawings
SEM image of product A in FIG. 1;
FIG. 2 SEM image of product C;
FIG. 3 is a graph showing the variation of carbon dioxide concentration in the product A-E catalytic acetaldehyde oxidation system;
FIG. 4 is a graph showing the change in acetaldehyde concentration in the product A-E catalytic acetaldehyde oxidation system.
Detailed Description
In order to facilitate a further understanding of the invention, the following examples are provided to illustrate it in more detail. However, these examples are only for better understanding of the present invention and are not intended to limit the scope or the principle of the present invention, and the embodiments of the present invention are not limited to the following.
Example 1
(1) Dispersing selenium powder (10mg) and graphene oxide (200mg) in an acetic acid solution (5mL, 1mol/L), adding a europium nitrate solution (2mL, 0.1mol/L), and uniformly stirring to obtain a component A for later use;
(2) at room temperature, dropwise adding the component A obtained in the step (1) into an absolute ethyl alcohol solution (prepared from 400mg of n-butyl titanate and 2g of absolute ethyl alcohol) of n-butyl titanate, stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, washing the precipitate with ethanol and water in sequence, and vacuum-drying at 60 ℃ for 24h to obtain the Eu3+Se co-doping of TiO2the/GO material (hereinafter referred to as product A).
Example 2
(1) Dispersing selenium powder (10mg) and graphene oxide (200mg) in an acetic acid solution (5mL, 1mol/L), and uniformly stirring to obtain a component A1 for later use;
(2) at room temperature, dropwise adding the component A1 obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate (prepared from 400mg of n-butyl titanate and 2g of absolute ethyl alcohol), stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, washing the precipitate with ethanol and water in sequence, and vacuum-drying at 60 ℃ for 24h to obtain the Se-doped TiO2the/GO material (hereinafter referred to as product B).
Example 3
(1) Dispersing graphene oxide (200mg) in an acetic acid solution (5mL, 1mol/L), adding a europium nitrate solution (2mL, 0.1mol/L), and uniformly stirring to obtain a component A2 for later use;
(2) at room temperature, dropwise adding the component A2 obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate (prepared from 400mg of n-butyl titanate and 2g of absolute ethyl alcohol), stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, washing the precipitate with ethanol and water in sequence, and vacuum-drying at 60 ℃ for 24h to obtain Eu3+Doped TiO 22the/GO material (hereinafter referred to as product C).
Example 4
(1) Dispersing graphene oxide (200mg) in an acetic acid solution (5mL, 1mol/L), and uniformly stirring to obtain a component A3 for later use;
(2) at room temperature, dropwise adding the component A3 obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate (prepared from 400mg of n-butyl titanate and 2g of absolute ethyl alcohol), stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, washing the precipitate with ethanol and water in sequence, and vacuum-drying at 60 ℃ for 24h to obtain TiO2the/GO material (hereinafter referred to as product D).
Example 5
(1) Dispersing selenium powder (2mg) and graphene oxide (200mg) in an acetic acid solution (5mL, 1mol/L), adding a europium nitrate solution (2mL, 0.1mol/L), and uniformly stirring to obtain a component A4 for later use;
(2) at room temperature, dropwise adding the component A4 obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate (prepared from 400mg of n-butyl titanate and 2g of absolute ethyl alcohol), stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, washing the precipitate with ethanol and water in sequence, and vacuum-drying at 60 ℃ for 24h to obtain Eu3+Se co-doping of TiO2the/GO material (hereinafter referred to as product E).
EXAMPLE 6 acetaldehyde photocatalytic oxidation experiment
Acetaldehyde photocatalytic oxidation experiment: weighing 100mg of products A-E respectively, irradiating with ultraviolet lamp, uniformly spreading and dispersing at the bottom of glass surface dish
The glass watch glass and 125mL of 500ppm acetaldehyde/pure air mixture were injected into a Tedlar bag, placed in a dark room for 2 hours to establish an equilibrium of adsorption and desorption between the products A-E and acetaldehyde, and then used with 3mW/cm2The products A-E were illuminated by LED lamps of light intensity (centre wavelength 435nm) and the acetaldehyde consumption and the concentration of the generated carbon dioxide were monitored in real time by on-line gas chromatography (3000AMIcro-GC, Agilent, TCD detector) with OV1 and PLOT-Q columns (FIGS. 3-4).
Claims (5)
1. Eu (Eu)3+Se co-doping of TiO2Use of a/GO material as a photocatalyst.
2. Use according to claim 1, characterized by the use of visible light for photocatalytic oxidation of acetaldehyde to carbon dioxide.
3. Use according to any of claims 1-2, characterized in that said Eu3+Se co-doping of TiO2The preparation method of the/GO material comprises the following steps:
(1) dispersing selenium powder and graphene oxide in an acetic acid solution, adding a europium nitrate solution, and uniformly stirring to obtain a component A for later use;
(2) at room temperature, dropwise adding the component A obtained in the step (1) into an absolute ethyl alcohol solution of n-butyl titanate, stirring for 0.5h, heating to 70 ℃, continuing stirring for 2h, filtering to obtain a precipitate, sequentially washing the precipitate with ethanol and water, and vacuum-drying at 60 ℃ for 24h to obtain the Eu3+Se co-doping of TiO2a/GO material.
4. The use of claim 3, wherein in step (1), the mass ratio of the selenium powder to the graphene oxide is 1:20, the concentration of the acetic acid solution is 1mol/L, the concentration of the europium nitrate solution is 0.1mol/L, 25mL of the acetic acid solution is used per gram of the graphene oxide, and 10mL of the europium nitrate solution is used.
5. The use according to claim 3, characterized in that the absolute ethanol solution of n-butyl titanate in step (2) is prepared by mixing n-butyl titanate and absolute ethanol according to a mass ratio of 1:5, and the amount of n-butyl titanate is 2 times of the mass of graphene oxide used in the preparation component A.
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| CN111548474A (en) * | 2020-05-11 | 2020-08-18 | 林多炉 | Nano TiO (titanium dioxide)2Antibacterial material of-graphene in-situ modified polyurethane and preparation method thereof |
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| CN102059110A (en) * | 2010-12-02 | 2011-05-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of double-rare earth co-doped nanometer titanium dioxide photocatalyst |
| CN102992397A (en) * | 2012-12-13 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for rare earth element-doped titanium dioxide nano material |
| CN103872293A (en) * | 2014-03-18 | 2014-06-18 | 中国科学院化学研究所 | Novel lithium ion battery electrode material and application of lithium ion battery electrode material |
| CN103861575A (en) * | 2014-02-27 | 2014-06-18 | 常州耀春格瑞纺织品有限公司 | Method for preparing doped-modified TiO2/graphene composite material |
| CN104474791A (en) * | 2014-11-07 | 2015-04-01 | 桂林新竹大自然生物材料有限公司 | Microcrystalline bamboo-charcoal cellular pottery-texture air filter panel with catalytic function and preparation method thereof |
| CN104596994A (en) * | 2014-12-15 | 2015-05-06 | 浙江大学 | Europium-doped titanium dioxide/graphene oxide composite film and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102059110A (en) * | 2010-12-02 | 2011-05-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of double-rare earth co-doped nanometer titanium dioxide photocatalyst |
| CN102992397A (en) * | 2012-12-13 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for rare earth element-doped titanium dioxide nano material |
| CN103861575A (en) * | 2014-02-27 | 2014-06-18 | 常州耀春格瑞纺织品有限公司 | Method for preparing doped-modified TiO2/graphene composite material |
| CN103872293A (en) * | 2014-03-18 | 2014-06-18 | 中国科学院化学研究所 | Novel lithium ion battery electrode material and application of lithium ion battery electrode material |
| CN104474791A (en) * | 2014-11-07 | 2015-04-01 | 桂林新竹大自然生物材料有限公司 | Microcrystalline bamboo-charcoal cellular pottery-texture air filter panel with catalytic function and preparation method thereof |
| CN104596994A (en) * | 2014-12-15 | 2015-05-06 | 浙江大学 | Europium-doped titanium dioxide/graphene oxide composite film and preparation method thereof |
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