CN101983928B - Preparation method of titanate nanotube codoped with ions of nitrogen and rare earth elements - Google Patents
Preparation method of titanate nanotube codoped with ions of nitrogen and rare earth elements Download PDFInfo
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- CN101983928B CN101983928B CN 201010537902 CN201010537902A CN101983928B CN 101983928 B CN101983928 B CN 101983928B CN 201010537902 CN201010537902 CN 201010537902 CN 201010537902 A CN201010537902 A CN 201010537902A CN 101983928 B CN101983928 B CN 101983928B
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Abstract
The invention discloses a preparation method of a titanate nanotube codoped with ions of nitrogen and rare earth elements, relating to ion exchange doping. The invention aims at providing a preparation method of a titanate nanotube codoped with ions of nitrogen and rare earth elements, and the titanate nanotube obtained by the method has good visible light activity. The technical scheme of the invention is as follows: the preparation method of a titanate nanotube codoped with ions of nitrogen and rare earth elements comprises a titanate nanotube production method: (1) adding 1 part by mass of titanate nanotubes to a mixed water solution containing NH4<+> ions and ions of rare earth elements, stirring at room temperature until ion exchange equilibrium, cleaning the titanate nanotubes with deionized water, drying and dewatering, wherein the concentration of the mixed water solution is 0.01-0.5M; and (2) calcining the dry doped titanate nanotubes in a calcining furnace at 300-800 DEG C to obtain the titanate nanotubes codoped with ions of nitrogen and rare earth elements. The method provided by the invention is used for doping the titanate nanotubes.
Description
Technical field:
The present invention relates to a kind of ion-exchange doping, the particularly preparation method of a kind of nitrogen element and rare earth element ion codoped titanate radical nanopipe.
Background technology:
Hydrothermal method is preparation TiO
2The common method of nanotube.With TiO
2Nanoparticle at high temperature carries out a series of chemical reaction with concentrated alkali solution, then makes TiO through overpickling, calcining
2Nanotube.The method is simple to operate, with low cost.It is generally acknowledged, in fact the nanotube of hydrothermal method preparation can be referred to as metatitanic acid or titanate nanotube, and it consists of H
2Ti
3O
7, Na
xH
2-xTi
3O
7, H
2Ti
5O
11H
2O or H
2Ti
4O
9H
2O。But the visible light activity of this titanate radical nanopipe is undesirable.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of nitrogen element and rare earth element ion codoped titanate radical nanopipe.The visible light activity of the titanate radical nanopipe that obtains with this method is good.Technical scheme of the present invention is that the preparation method of a kind of nitrogen element and rare earth element ion codoped titanate radical nanopipe comprises the titanate radical nanopipe production method, it is characterized in that: (1) is put into 1 mass parts titanate radical nanopipe and is contained NH
4 +In the mixed aqueous solution of ion and rare earth element ion, the concentration of described solution is 0.01-0.5M, after at room temperature stirring reaches ion-exchange equilibrium, use washed with de-ionized water, the dry moisture of removing, (2) the doped titanic acid nanotube of drying is placed in calcining furnace and calcines under 300-800 ℃, namely make nitrogen element and rare earth element ion codoped titanate radical nanopipe.The present invention has the good remarkable advantage of visible light activity of simple for process and prepared titanate radical nanopipe compared with the prior art.
Embodiment:
With the following Examples the present invention is elaborated,
Embodiment 1
(1) adopt known hydrothermal method to prepare titanate radical nanopipe.1.0 g TiO
2Add in the 10 M NaOH aqueous solution, stir and put into autoclave 150-220 ℃ of reaction 24-36 h after 20 minutes, take out with washed with de-ionized water and immerse acidifying 5-8 h in 0.1MHCl after neutral, then be washed till neutrality with deionized water.Grind after 80 ℃ of drying 10 h, namely make titanate radical nanopipe.
(2) getting the above-mentioned titanate radical nanopipe for preparing of 1g puts into and contains NH
4 +In the mixing solutions of ion and rare earth element ion, NH
4 +Ion and rare earth element ion concentration ratio are 1:1, and both total concns are 0.01M, at room temperature stir 24 h and reach ion-exchange equilibrium, then with 80 ℃ of dryings after washed with de-ionized water 10 hours.
(3) titanate radical nanopipe of doping nitrogen element and rare earth element ion is namely made in the calcining under 300 ℃ in calciner of the titanate radical nanopipe after adulterating.
Embodiment 2
(1) adopt known hydrothermal method to prepare titanate radical nanopipe.1.0 g TiO
2Add in the 10 M NaOH aqueous solution, stir and put into autoclave 150-220 ℃ of reaction 24-36 h after 20 minutes, take out with washed with de-ionized water and immerse acidifying 5-8 h in 0.1MHCl after neutral, then be washed till neutrality with deionized water.Grind after 80 ℃ of drying 10 h, namely make titanate radical nanopipe.
(2) getting the above-mentioned titanate radical nanopipe for preparing of 1g puts into and contains NH
4 +In the mixing solutions of ion and rare earth element ion, NH
4 +Ion and rare earth element ion concentration ratio are 1:2, and both total concns are 0.1 M, at room temperature stir 24 h and reach ion-exchange equilibrium, then with 80 ℃ of dryings after washed with de-ionized water 10 hours.
(3) titanate radical nanopipe of doping nitrogen element and rare earth element ion is namely made in the calcining under 500 ℃ in calciner of the titanate radical nanopipe after adulterating.
Embodiment 3
(1) adopt known hydrothermal method to prepare titanate radical nanopipe.1.0 g TiO
2Add in the 10 M NaOH aqueous solution, stir and put into autoclave 150-220 ℃ of reaction 24-36 h after 20 minutes, take out with washed with de-ionized water and immerse acidifying 5-8 h in 0.1MHCl after neutral, then be washed till neutrality with deionized water.Grind after 80 ℃ of drying 10 h, namely make titanate radical nanopipe.
(2) getting the above-mentioned titanate radical nanopipe for preparing of 1g puts into and contains NH
4 +In the mixing solutions of ion and rare earth element ion, NH
4 +Ion and rare earth element ion concentration ratio are 1:3, and both total concns are 0.5M, at room temperature stir 24 h and reach ion-exchange equilibrium, then with 80 ℃ of dryings after washed with de-ionized water 10 hours.
(3) titanate radical nanopipe of doping nitrogen element and rare earth element ion is namely made in the calcining under 800 ℃ in calciner of the titanate radical nanopipe after adulterating.
Claims (1)
1. the preparation method of a nitrogen element and rare earth element ion codoped titanate radical nanopipe, comprise the titanate radical nanopipe production method, and it is characterized in that: (1) is with 1.0 g TiO
2Add in the 10 M NaOH aqueous solution, stir and put into autoclave 150-220 ℃ of reaction 24-36 h after 20 minutes, taking-up is immersed acidifying 5-8 h in 0.1MHCl with washed with de-ionized water after neutral, then be washed till neutrality with deionized water, grind after 80 ℃ of drying 10 h, namely make titanate radical nanopipe, (2) are put into the 1g titanate radical nanopipe and are contained NH
4 +In the mixed aqueous solution of ion and rare earth element ion, NH
4 +The concentration ratio of ion and rare earth element ion is 1:1, total concn both is 0.01M, at room temperature stir 24h and reach ion-exchange equilibrium, with 80 ℃ of dry 10h after washed with de-ionized water, remove moisture, (3) dried doped titanic acid nanotube is placed in calcining furnace and calcines under 300 ℃, namely make nitrogen element and rare earth element ion codoped titanate radical nanopipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010537902 CN101983928B (en) | 2010-11-10 | 2010-11-10 | Preparation method of titanate nanotube codoped with ions of nitrogen and rare earth elements |
Applications Claiming Priority (1)
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|---|---|---|---|
| CN 201010537902 CN101983928B (en) | 2010-11-10 | 2010-11-10 | Preparation method of titanate nanotube codoped with ions of nitrogen and rare earth elements |
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|---|---|
| CN101983928A CN101983928A (en) | 2011-03-09 |
| CN101983928B true CN101983928B (en) | 2013-06-05 |
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| CN 201010537902 Expired - Fee Related CN101983928B (en) | 2010-11-10 | 2010-11-10 | Preparation method of titanate nanotube codoped with ions of nitrogen and rare earth elements |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723442A (en) * | 2009-12-08 | 2010-06-09 | 东北林业大学 | Method for preparing nitrogen-doped titanic acid nano tube by hydrothermal cosolvent method |
-
2010
- 2010-11-10 CN CN 201010537902 patent/CN101983928B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723442A (en) * | 2009-12-08 | 2010-06-09 | 东北林业大学 | Method for preparing nitrogen-doped titanic acid nano tube by hydrothermal cosolvent method |
Non-Patent Citations (3)
| Title |
|---|
| Hanjin Liu et al..N-Doped Trititanate Nanotubes: Preparation, Characterization and Visible-Light Sensitivity.《Bioinformatics and Biomedical Engineering (iCBBE), 2010 4th International Conference on》.2010,第1-6页. * |
| 于爱敏 等.可见光响应Cr,N-共掺杂钛酸盐纳米管的水热法合成及表征.《石油学报(石油加工)》.2008,第245-248页. * |
| 于爱敏等.可见光响应Cr N-共掺杂钛酸盐纳米管的水热法合成及表征.《石油学报（石油加工）》.2008 |
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| CN101983928A (en) | 2011-03-09 |
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Inventor after: Liu Guoguang Inventor after: Liu Haijin Inventor after: Wang Yingling Inventor after: Lv Wenying Inventor after: Xie Youhai Inventor before: Liu Guoguang Inventor before: Liu Haijin Inventor before: Xie Youhai Inventor before: Lv Wenying Inventor before: Wang Yingling |
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Free format text: CORRECT: INVENTOR; FROM: LIU GUOGUANG LIU HAIJIN XIE YOUHAI LV WENYING WANG YINGLING TO: LIU GUOGUANG LIU HAIJIN WANG YINGLING LV WENYING XIE YOUHAI |
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