CN109201088A - A kind of Eu3+, Se codope TiO2/ GO material and its application in photocatalysis - Google Patents
A kind of Eu3+, Se codope TiO2/ GO material and its application in photocatalysis Download PDFInfo
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- CN109201088A CN109201088A CN201811304956.5A CN201811304956A CN109201088A CN 109201088 A CN109201088 A CN 109201088A CN 201811304956 A CN201811304956 A CN 201811304956A CN 109201088 A CN109201088 A CN 109201088A
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- CN
- China
- Prior art keywords
- codope
- codope tio
- tetrabutyl titanate
- acetum
- graphene oxide
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 239000000463 material Substances 0.000 title claims abstract description 24
- 230000001699 photocatalysis Effects 0.000 title abstract description 4
- 238000007146 photocatalysis Methods 0.000 title abstract description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 22
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000003647 oxidation Effects 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 57
- 238000003756 stirring Methods 0.000 claims description 22
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 19
- 229960004756 ethanol Drugs 0.000 claims description 19
- 235000019441 ethanol Nutrition 0.000 claims description 19
- 239000011669 selenium Substances 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910021389 graphene Inorganic materials 0.000 claims description 16
- 230000001376 precipitating effect Effects 0.000 claims description 11
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 9
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 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 description 8
- 238000010792 warming Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- -1 graphite alkene Chemical class 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000013049 sediment Substances 0.000 description 5
- 229910052693 Europium Inorganic materials 0.000 description 4
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 4
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical class [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/27—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
- C07C45/32—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
- C07C45/37—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
- C07C45/39—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a secondary hydroxyl group
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of Eu3+, Se codope TiO2/ GO material and its application in photocatalysis, pass through Eu3+, Se codope make TiO2It is acetone that/GO material is catalyzed isopropanol oxidation under visible light, and being selected from property of acetone is high.
Description
Technical field
The invention belongs to field of photocatalytic material, and in particular to a kind of Eu3+, Se codope TiO2/ GO material and its in light
Application in catalysis.
Background technique
For traditional titanium dioxide class due to significantly limiting its application to visible light-responded difference, the present invention passes through Eu3+、Se
Codope obtains a kind of new E u that can be catalyzed isopropanol oxidation under visible light as acetone3+, Se codope TiO2/ GO material.
Summary of the invention
The present invention provides a kind of Eu3+, Se codope TiO2/ GO material, it is characterised in that the Eu3+, Se codope TiO2/
The preparation method of GO material includes the following steps:
(1) selenium powder, graphene oxide are dispersed in acetum, europium nitrate solution is added, stirs evenly, obtains component A
It is spare；
(2) at room temperature, the component A that step (1) obtains is added drop-wise in the ethanol solution of tetrabutyl titanate, is stirred
It is warming up to 70 DEG C after 0.5h to continue after stirring 2h, filters to obtain precipitating, after precipitating successively uses ethyl alcohol, water washing, under the conditions of 60 DEG C
Vacuum drying is for 24 hours up to the Eu3+, Se codope TiO2/ GO material.
The mass ratio of selenium powder described in step (1) and graphene oxide is 1:20, and the concentration of acetum is 1mol/L, nitre
The concentration of sour europium solution is 0.1mol/L, and every gram of graphene oxide uses 25mL acetum, uses europium nitrate solution 10mL；Step
Suddenly the ethanol solution of tetrabutyl titanate is that tetrabutyl titanate is configured to dehydrated alcohol 1:5 in mass ratio in (2), metatitanic acid
The dosage of N-butyl is 2 times that formulation components A uses graphene oxide quality.
Another embodiment of the present invention provides above-mentioned Eu3+, Se codope TiO2The preparation method of/GO material, feature
It is to include the following steps:
(1) selenium powder, graphene oxide are dispersed in acetum, europium nitrate solution is added, stirs evenly, obtains component A
It is spare；
(2) at room temperature, the component A that step (1) obtains is added drop-wise in the ethanol solution of tetrabutyl titanate, is stirred
It is warming up to 70 DEG C after 0.5h to continue after stirring 2h, filters to obtain precipitating, after precipitating successively uses ethyl alcohol, water washing, under the conditions of 60 DEG C
Vacuum drying is for 24 hours up to the Eu3+, Se codope TiO2/ GO material.
The mass ratio of selenium powder described in step (1) and graphene oxide is 1:20, and the concentration of acetum is 1mol/L, nitre
The concentration of sour europium solution is 0.1mol/L, and every gram of graphene oxide uses 25mL acetum, uses europium nitrate solution 10mL；Step
Suddenly the ethanol solution of tetrabutyl titanate is that tetrabutyl titanate is configured to dehydrated alcohol 1:5 in mass ratio in (2), metatitanic acid
The dosage of N-butyl is 2 times that formulation components A uses graphene oxide quality.
Another embodiment of the present invention provides above-mentioned Eu3+, Se codope TiO2/ GO material is answered as photochemical catalyst
With.It is preferred that being the application in acetone in visible light catalytic oxidation isopropanol.
Detailed description of the invention
The SEM of Fig. 1 product A schemes；
The SEM of Fig. 2 products C schemes；
Fig. 3 product A-E is catalyzed the variation diagram of acetone concentration in isopropanol oxidation system；
Fig. 4 product A-E is catalyzed the variation diagram of isopropyl alcohol concentration in isopropanol oxidation system.
Specific embodiment
For the ease of a further understanding of the present invention, examples provided below has done more detailed description to it.But
It is that these embodiments are only not supposed to be a limitation to the present invention or implementation principle for better understanding invention, reality of the invention
The mode of applying is not limited to the following contents.
Embodiment 1
(1) it takes selenium powder (10mg), graphene oxide (200mg) to be dispersed in acetum (5mL, 1mol/L), nitre is added
Sour europium solution (2mL, 0.1mol/L), stirs evenly, it is spare to obtain component A；
(2) at room temperature, the component A that step (1) obtains is added drop-wise to the ethanol solution of tetrabutyl titanate (by 400mg
Tetrabutyl titanate and 2g dehydrated alcohol are prepared) in, it is warming up to 70 DEG C after stirring 0.5h and continues after stirring 2h, filters to obtain precipitating, sink
It forms sediment successively with after ethyl alcohol, water washing, is dried in vacuo under the conditions of 60 DEG C for 24 hours up to the Eu3+, Se codope TiO2/ GO material
(hereinafter referred to as product A).
Embodiment 2
(1) selenium powder (10mg), graphene oxide (200mg) is taken to be dispersed in acetum (5mL, 1mol/L), stirring is equal
It is even, it is spare to obtain component A1；
(2) at room temperature, the component A1 that step (1) obtains is added drop-wise to the ethanol solution of tetrabutyl titanate (by 400mg
Tetrabutyl titanate and 2g dehydrated alcohol are prepared) in, it is warming up to 70 DEG C after stirring 0.5h and continues after stirring 2h, filters to obtain precipitating, sink
It forms sediment successively with after ethyl alcohol, water washing, is dried in vacuo under the conditions of 60 DEG C and adulterates TiO for 24 hours up to Se2/ GO material (hereinafter referred to as produces
Product B).
Embodiment 3
(1) it takes graphene oxide (200mg) to be dispersed in acetum (5mL, 1mol/L), europium nitrate solution is added
(2mL, 0.1mol/L), stirs evenly, and it is spare to obtain component A2；
(2) at room temperature, the component A2 that step (1) obtains is added drop-wise to the ethanol solution of tetrabutyl titanate (by 400mg
Tetrabutyl titanate and 2g dehydrated alcohol are prepared) in, it is warming up to 70 DEG C after stirring 0.5h and continues after stirring 2h, filters to obtain precipitating, sink
It forms sediment successively with after ethyl alcohol, water washing, is dried in vacuo under the conditions of 60 DEG C for 24 hours up to Eu3+Adulterate TiO2/ GO material is (hereinafter referred to as
Products C).
Embodiment 4
(1) it takes graphene oxide (200mg) to be dispersed in acetum (5mL, 1mol/L), stirs evenly, obtain component A3
It is spare；
(2) at room temperature, the component A3 that step (1) obtains is added drop-wise to the ethanol solution of tetrabutyl titanate (by 400mg
Tetrabutyl titanate and 2g dehydrated alcohol are prepared) in, it is warming up to 70 DEG C after stirring 0.5h and continues after stirring 2h, filters to obtain precipitating, sink
It forms sediment successively with after ethyl alcohol, water washing, is dried in vacuo under the conditions of 60 DEG C for 24 hours up to TiO2/ GO material (hereinafter referred to as product D).
Embodiment 5
(1) it takes selenium powder (2mg), graphene oxide (200mg) to be dispersed in acetum (5mL, 1mol/L), nitric acid is added
Europium solution (2mL, 0.1mol/L), stirs evenly, and it is spare to obtain component A4；
(2) at room temperature, the component A4 that step (1) obtains is added drop-wise to the ethanol solution of tetrabutyl titanate (by 400mg
Tetrabutyl titanate and 2g dehydrated alcohol are prepared) in, it is warming up to 70 DEG C after stirring 0.5h and continues after stirring 2h, filters to obtain precipitating, sink
It forms sediment successively with after ethyl alcohol, water washing, is dried in vacuo under the conditions of 60 DEG C for 24 hours up to Eu3+, Se codope TiO2/ GO material is (following
Abbreviation product E).
6 isopropanol photochemical catalytic oxidation of embodiment experiment
Isopropanol photochemical catalytic oxidation experiment: 100mg product A-E is weighed respectively after ultraviolet light irradiation, evenly laid out dispersion
In glass surface ware bottomIsopropanol/the pure air for being 500ppm by the glass surface ware and 125mL concentration
Mixed gas is injected into Tedlar transparent bag, is placed in darkroom the suction for being kept for establish between product A-E and isopropanol for 2 hours
Attached desorption balance, then uses 3mW/cm2The LED light (central wavelength 435nm) of light intensity is irradiated product A-E, passes through band
There is online gas-chromatography (3000A Micro-GC, Agilent, TCD detector) real-time monitoring of OV1 and PLOT-Q chromatographic column different
Propyl alcohol consumption and the variation (Fig. 3-4) for generating acetone concentration.
Claims (5)
1. a kind of Eu3+, Se codope TiO2/ GO material, it is characterised in that the Eu3+, Se codope TiO2The preparation of/GO material
Method includes the following steps:
(1) selenium powder, graphene oxide are dispersed in acetum, europium nitrate solution is added, stirs evenly, it is spare to obtain component A；
(2) at room temperature, the component A that step (1) obtains is added drop-wise in the ethanol solution of tetrabutyl titanate, after stirring 0.5h
It is warming up to 70 DEG C to continue after stirring 2h, filters to obtain precipitating, precipitating is successively with after ethyl alcohol, water washing, and vacuum is dry under the conditions of 60 DEG C
It is dry for 24 hours up to the Eu3+, Se codope TiO2/ GO material.
2. Eu described in claim 13+, Se codope TiO2/ GO material, it is characterised in that selenium powder and oxygen described in step (1)
The mass ratio of graphite alkene is 1:20, and the concentration of acetum is 1mol/L, and the concentration of europium nitrate solution is 0.1mol/L, every gram
Graphene oxide uses 25mL acetum, uses europium nitrate solution 10mL.
3. the described in any item Eu of claim 1-23+, Se codope TiO2/ GO material, it is characterised in that metatitanic acid in step (2)
The ethanol solution of N-butyl is that tetrabutyl titanate is configured to dehydrated alcohol 1:5 in mass ratio, the use of tetrabutyl titanate
Amount is 2 times that formulation components A uses graphene oxide quality.
4. the described in any item Eu of claim 1-33+, Se codope TiO2Application of/GO the material as photochemical catalyst.
5. application as claimed in claim 4, it is characterised in that preferably in the application that visible light catalytic oxidation isopropanol is in acetone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811304956.5A CN109201088B (en) | 2018-11-02 | 2018-11-02 | Eu (Eu)3+Se co-doping of TiO2/GO material and its application in photocatalysis |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811304956.5A CN109201088B (en) | 2018-11-02 | 2018-11-02 | Eu (Eu)3+Se co-doping of TiO2/GO material and its application in photocatalysis |
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| Publication Number | Publication Date |
|---|---|
| CN109201088A true CN109201088A (en) | 2019-01-15 |
| CN109201088B CN109201088B (en) | 2021-06-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811304956.5A Active CN109201088B (en) | 2018-11-02 | 2018-11-02 | Eu (Eu)3+Se co-doping of TiO2/GO material and its application in photocatalysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111643A (en) * | 2020-01-17 | 2020-05-08 | 西华大学 | Rare earth doped RGO/titanium dioxide efficient photocatalyst and preparation method thereof |
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|---|---|---|---|---|
| CN102212365A (en) * | 2011-04-12 | 2011-10-12 | 东华大学 | Preparation method for europium-doping calcium titanate fluorescent powder |
| 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 |
| CN108212138A (en) * | 2016-12-09 | 2018-06-29 | 北京有色金属研究总院 | A kind of preparation process of lanthanum and graphene oxide codope lightweight catalysis material |
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- 2018-11-02 CN CN201811304956.5A patent/CN109201088B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212365A (en) * | 2011-04-12 | 2011-10-12 | 东华大学 | Preparation method for europium-doping calcium titanate fluorescent powder |
| 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 |
| CN108212138A (en) * | 2016-12-09 | 2018-06-29 | 北京有色金属研究总院 | A kind of preparation process of lanthanum and graphene oxide codope lightweight catalysis material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111111643A (en) * | 2020-01-17 | 2020-05-08 | 西华大学 | Rare earth doped RGO/titanium dioxide efficient photocatalyst and preparation method thereof |
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