CN105536845A - Method for simultaneously doping ferrum and nitrogen to TiO2 by using ferric o-phenanthroline - Google Patents
Method for simultaneously doping ferrum and nitrogen to TiO2 by using ferric o-phenanthroline Download PDFInfo
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- CN105536845A CN105536845A CN201510972546.8A CN201510972546A CN105536845A CN 105536845 A CN105536845 A CN 105536845A CN 201510972546 A CN201510972546 A CN 201510972546A CN 105536845 A CN105536845 A CN 105536845A
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- phenanthroline
- iron
- tio
- nitrogen
- ethanol
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 33
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- 230000001699 photocatalysis Effects 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 229910052742 iron Inorganic materials 0.000 claims description 28
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 25
- 239000007787 solid Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 7
- 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 6
- 229910002551 Fe-Mn Inorganic materials 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 230000000593 degrading effect Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 3
- 150000004696 coordination complex Chemical class 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 abstract 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 8
- 239000012456 homogeneous solution Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052755 nonmetal Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- -1 iron ion Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- B01J27/24—Nitrogen compounds
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
-
- 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
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- General Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Electromagnetism (AREA)
- Catalysts (AREA)
Abstract
The invention relates to a method for simultaneously doping ferrum and nitrogen to TiO2 by using ferric o-phenanthroline. The obtained material can efficiently degrade an organic pollutant, i.e., p-nitrophenol under visible light. The method comprises the steps: preparing a solution from o-phenanthroline, uniformly mixing the solution with FeSO4 and n-butyl titanate, and transferring the mixture to a hydrothermal kettle for reaction; and separating a sample after the reaction ends, carrying out washing, carrying out drying, and then carrying out calcining, thereby obtaining the product. The method is characterized by simultaneously doping ferrum and nitrogen to TiO2 by using an organic metal complex, i.e., ferric o-phenanthroline, and the obtained material has efficient photocatalytic performance.
Description
Technical field
The present invention relates to nanometer semiconductor oxidation field of material technology, particularly relate to one and utilize phenanthroline to close iron simultaneously to TiO
2the method of doping iron, nitrogen.
Background technology
Titanium dioxide (TiO
2) be a kind of stable in physicochemical property, safety non-toxic, conductor oxidate with low cost, form Strong oxdiative atmosphere under light illumination, almost all organic poison matter exhaustive oxidations can be resolved into carbon dioxide, the small-molecule substance that water etc. are nontoxic.Solar energy is clean and the energy of economy, TiO
2the performance that solar energy can be utilized to carry out catalysis makes it receive great concern in the application in degraded environmental pollution field.But TiO
2band gap wider, for 3.2eV, this makes it to absorb and accounts for the ultraviolet light (λ < 387nm) reaching ground solar energy less than 5%, effectively can not utilize in sunshine the energy of the visible ray accounting for large absolutely number, the utilization rate of energy solar energy is extremely low.Therefore, inquire into TiO
2modification, widening its absorbance spectrum and move to visible ray, thus improve utilization rate to solar energy, is current TiO
2the focus of photochemical catalyst research.
A large amount of research experiment shows, effectively can widen TiO by doping
2photoresponse scope, improve its photocatalytic activity.At present for TiO
2the method of doping is a lot, mainly can be divided into metal-doped and nonmetal doping.Metal ion mixing can at TiO
2introduce defect in lattice or change degree of crystallinity, compound affect light induced electron and hole be separated so that change doping TiO afterwards
2catalytic activity.Nonmetal doping improves TiO
2active principle is commonly considered as at TiO
2middle introducing Lattice Oxygen room, or part Lacking oxygen is replaced by nonmetalloid, reduces TiO
2energy gap, thus widen TiO
2photoresponse scope.But doping metals or the nonmetal charge balance that may destroy system individually sometimes, produces the complex centre in light induced electron, hole, thus reduces photocatalysis efficiency.In recent years, some metals and nonmetalloid codope TiO
2significantly improve the separative efficiency in light induced electron and hole, show the visible light catalysis activity better than single doped catalyst, this is considered to relevant with the cooperative effect between doped chemical.
Present metal and nonmetal codope study general are added respectively by the material of each component, and such as, Xie Yongbing etc. first use double-deck hydro-thermal legal system for the TiO of metal ion mixing
2, then under ammonia atmosphere, N doping is carried out in high-temperature roasting, thus obtains metal, nitrogen co-doped TiO
2[a kind of codope TiO
2catalysts and its preparation method, application number: 201410053505.4]; Liu Yiming etc. utilize sputtering technology, and substep mixes Ag and N, obtains Ag, the TiO of N codope
2[a kind of Ag, N codope TiO
2the preparation method of nano thin-film and the application of nano thin-film thereof, application number: 201510307342.2]; Fan Xiaoyun etc. utilize nitrogenous acetic acid solution and water-soluble copper compound to TiO
2middle copper doped and nitrogen [copper-nitrogen codope photocatalysis material of titanium dioxide, application number: 201110144191.5].
In the methods of the invention, what provide a kind of novelty prepares Fe-Mn cycle and transference TiO
2method.Utilize phenanthroline can form the characteristic of compound with iron ion coordination, close the such entirety of iron with phenanthroline and provide source of iron and nitrogenous source, to TiO simultaneously
2middle doping iron and nitrogen.Source of iron and nitrogenous source exist with the form of same compound, and make iron, nitrogen can play synergy better, and adulterates more even, and the product obtained compares respectively with the iron that independent source of iron and nitrogenous source obtain, nitrogen co-doped TiO
2there is better performance.
The present invention relates to a kind of newly to TiO
2the method of doping iron, nitrogen, raw material is easy to get, and cost is low, simple to operate, and described method has no report.
Summary of the invention
One is the object of the present invention is to provide to utilize phenanthroline to close iron simultaneously to TiO
2the method of doping iron, nitrogen, the present invention takes following means:
(1) tetrabutyl titanate is dissolved in ethanol, ratio is 3mL tetrabutyl titanate/10mL ethanol.Add FeSO wherein again
47H
2o, ratio is 0.03gFeSO
47H
2o/10mL ethanol;
(2) phenanthroline is dissolved in ethanol, ratio is 0.06g phenanthroline/10mL ethanol;
(3) under constantly stirring, (2) gained solution is slowly added to (1) gained solution, mixes;
(4) (3) gained solution is added to hydrothermal reaction kettle, by the centrifugation of gained solid, cleaning, oven dry after 180 DEG C of reaction 24h;
(5), after (4) gained solid abrasive is thin, in Muffle furnace, namely product is obtained after 300 DEG C of calcining 4h.
The material use phenanthroline of gained closes the such entirety of iron provides source of iron and nitrogenous source simultaneously, prepares Fe-Mn cycle and transference TiO
2.
The material of gained has good photocatalytic activity, p-nitrophenol of can degrading under visible light.
Advantage of the present invention is: utilize phenanthroline to close iron and integrally provide source of iron and nitrogenous source simultaneously, make iron, nitrogen can play synergy better, adulterate more even; Raw material is easy to get, and cost is low, simple to operate; Products obtained therefrom has excellent photocatalysis performance, can utilize the organic pollution p-nitrophenol of Visible Light Induced Photocatalytic pole difficult degradation.
Accompanying drawing explanation
The Fe-Mn cycle and transference TiO that the embodiment 1 that Fig. 1 is the present invention obtains
2fT-IR figure;
The Fe-Mn cycle and transference TiO that the embodiment 1 that Fig. 2 is the present invention obtains
2visible Light Induced Photocatalytic p-nitrophenol.
Detailed description of the invention
Embodiment 1
Under continuous stirring, 3mL tetrabutyl titanate is dissolved in 10mL ethanol, then adds 0.03gFeSO wherein
47H
2o, dissolves completely and obtains homogeneous solution A; Under continuous stirring, 0.06g phenanthroline is dissolved in 10mL ethanol, obtains homogeneous solution B; Under constantly stirring, B solution is slowly added in solution A, obtains homogeneous solution.Gained solution is added 180 DEG C of reaction 4h in hydrothermal reaction kettle.After reaction terminates, by the centrifugation of gained solid, replace cleaning more than three times with deionized water and ethanol, after oven dry, grinding.Muffle furnace 300 DEG C calcining 4 hours put into by the solid obtained by porphyrize, both obtains product.
Embodiment 2
Under continuous stirring, 6mL tetrabutyl titanate is dissolved in 20mL ethanol, then adds 0.06gFeSO wherein
47H
2o, dissolves completely and obtains homogeneous solution A; Under continuous stirring, 0.12g phenanthroline is dissolved in 20mL ethanol, obtains homogeneous solution B; Under constantly stirring, B solution is slowly added in solution A, obtains homogeneous solution.Gained solution is added 180 DEG C of reaction 4h in hydrothermal reaction kettle.After reaction terminates, by the centrifugation of gained solid, replace cleaning more than three times with deionized water and ethanol, after oven dry, grinding.Muffle furnace 300 DEG C calcining 4 hours put into by the solid obtained by porphyrize, both obtains product.
Claims (3)
1. one kind utilizes phenanthroline to close iron simultaneously to TiO
2the method of doping iron, nitrogen, is characterized in that:
(1) tetrabutyl titanate is dissolved in ethanol, ratio is 3mL tetrabutyl titanate/10mL ethanol; Add FeSO wherein again
47H
2o, ratio is 0.03gFeSO
47H
2o/10mL ethanol;
(2) phenanthroline is dissolved in ethanol, ratio is 0.06g phenanthroline/10mL ethanol;
(3) under constantly stirring, (2) gained solution is slowly added to (1) gained solution, mixes;
(4) (3) gained solution is added to hydrothermal reaction kettle, by the centrifugation of gained solid, cleaning, oven dry after 180 DEG C of reaction 24h;
(5), after (4) gained solid abrasive is thin, in Muffle furnace, namely product is obtained after 300 DEG C of calcining 4h.
2. one according to claim 1 utilizes phenanthroline to close iron simultaneously to TiO
2the method of doping iron, nitrogen, is characterized in that: the material use phenanthroline of gained closes the such entirety of iron provides source of iron and nitrogenous source simultaneously, prepares Fe-Mn cycle and transference TiO
2.
3. one according to claim 1 utilizes phenanthroline to close iron simultaneously to TiO
2the method of doping iron, nitrogen, is characterized in that: the material of gained has good photocatalytic activity, p-nitrophenol of can degrading under visible light.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510972546.8A CN105536845B (en) | 2015-12-23 | 2015-12-23 | It is a kind of to close iron simultaneously to TiO using phenanthroline2The method of doping iron, nitrogen |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510972546.8A CN105536845B (en) | 2015-12-23 | 2015-12-23 | It is a kind of to close iron simultaneously to TiO using phenanthroline2The method of doping iron, nitrogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105536845A true CN105536845A (en) | 2016-05-04 |
| CN105536845B CN105536845B (en) | 2019-04-05 |
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ID=55816681
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510972546.8A Expired - Fee Related CN105536845B (en) | 2015-12-23 | 2015-12-23 | It is a kind of to close iron simultaneously to TiO using phenanthroline2The method of doping iron, nitrogen |
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| Country | Link |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611520A (en) * | 2013-12-06 | 2014-03-05 | 江南大学 | Method for preparing molecular imprinting-doped TiO2 with high catalytic degradation activity under visible light |
| CN104383953A (en) * | 2014-11-24 | 2015-03-04 | 武汉纺织大学 | Active carbon-loaded nitrogen-doped cobalt catalyst and preparation method and application thereof |
-
2015
- 2015-12-23 CN CN201510972546.8A patent/CN105536845B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103611520A (en) * | 2013-12-06 | 2014-03-05 | 江南大学 | Method for preparing molecular imprinting-doped TiO2 with high catalytic degradation activity under visible light |
| CN104383953A (en) * | 2014-11-24 | 2015-03-04 | 武汉纺织大学 | Active carbon-loaded nitrogen-doped cobalt catalyst and preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 孙灿: "纳米TiO2光催化剂的水热法合成及掺杂改性", 《西安理工大学硕士学位论文》 * |
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