CN101190801B - Preparation of metal ion doping titanium dioxide line pipe by ion exchange method - Google Patents
Preparation of metal ion doping titanium dioxide line pipe by ion exchange method Download PDFInfo
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- CN101190801B CN101190801B CN200610114748A CN200610114748A CN101190801B CN 101190801 B CN101190801 B CN 101190801B CN 200610114748 A CN200610114748 A CN 200610114748A CN 200610114748 A CN200610114748 A CN 200610114748A CN 101190801 B CN101190801 B CN 101190801B
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- line pipe
- metal ion
- preparation
- layered titanate
- ion
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Abstract
The invention provides an ion exchange method to prepare metal ion mixed titanium oxide (TiO2) line pipe material and the steps comprise that: lamellar sodium titanate line pipe material which is converted by metal ions is treated for 4-40 hours at the temperature of 60-240 DEG C in a reactor with water; or the lamellar sodium titanate line pipe material mixed with metal saline solution is treatedfor 4-40 hours at a temperature of 60-240 DEG C in a reactor to obtain metal ion mixed TiO2 line pipe material. The preparation process is simple, the reaction conditions are easy to control and theproduct obtained has grant potential application in optical catalysis or photoelectric conversion field and luminescence material field.
Description
(1) technical field
The invention provides and a kind ofly prepare metal ion doped titanium dioxide (TiO with ion exchange method
2) method of line pipe, belong to the technical field of preparation doping type line pipe.
(2) background technology
At opto-electronic conversion or photocatalysis field, TiO
2Be very useful material, still, utilizing its effect and bad aspect the visible light, therefore, people wish to improve this performance by metal ion mixing.Have been found that metal ion mixing TiO
2Can significantly improve opto-electronic conversion or photocatalysis efficiency.
(3) summary of the invention
The purpose of this invention is to provide a kind of brand-new, simple and easily preparation method, synthesize the metal ion content metal ion doped titanium dioxide line pipe of control easily.
The invention provides and a kind ofly prepare metal ion doped titanium dioxide (TiO with ion exchange method
2) method of line pipe, this metal ion is to be incorporated into TiO
2In the line pipe, its method is:
Take by weighing an amount of layered titanate line pipe (preparation method of this layered titanate line pipe, document Ji T H sees reference, Tang M Y, Liu G R and Qi X Y, Adv.Mater.Res.2006,11-12,603), it is mixed with water-soluble aqueous metal salt, room temperature～240 ℃ ion-exchange 2～35 hours, make the layered titanate line pipe that contains the metal ion that exchanges, then, the layered titanate line pipe that will contain the metal ion that exchanges is put into reactor, and adds suitable quantity of water, reacted 4～40 hours at 60～240 ℃, obtain metal ion mixing TiO
2Line pipe;
Perhaps, directly aqueous metal salt is mixed in reactor with the layered titanate line pipe, and between 60～240 ℃, handle 4～40 hours, just can make metal ion mixing TiO
2Line pipe.
Wherein, this metal-salt is selected for use: Manganous chloride tetrahydrate (MnCl
2), manganous acetate (Mn (Ac)
2), cobalt chloride (CoCl
2), cobaltous acetate (Co (Ac)
2), iron protochloride (FeCl
2), iron trichloride (FeCl
3), cupric chloride (CuCl
2), copper sulfate (CuSO
4), nickelous chloride (NiCl
2), europium nitrate (Eu (NO
3)
3), Silver Nitrate (AgNO
3), indium chloride (InCl
3).
Wherein, this layered titanate line pipe is selected for use: Na-Ti-O, K-Ti-O.
Wherein, in reactor, prepare metal ion mixing TiO by ion exchange method
2The preparation process of line pipe is new building-up process.
Wherein, using certain reaction temperature (60～240 ℃) and reaction times (4～40 hours), is that the layered titanate line pipe of the metal ion that exchanges in order to contain changes metal ion mixing TiO into
2Line pipe.
Wherein, the method that contains the layered titanate line pipe of the metal ion that exchanges by ion exchange method preparation is: use the aqueous metal salt of solvable water directly to mix with the layered titanate line pipe, carry out ion-exchange under the condition of room temperature～240 ℃ and 2～35 hours.
Wherein, directly aqueous metal salt is mixed in reactor with the layered titanate line pipe, handled between 60～240 ℃ 4～40 hours, this an amount of aqueous metal salt is put into reactor with the layered titanate line pipe.
Wherein, new preparation metal ion mixing TiO
2The process of line pipe is meant that this building-up process is the process of direct ion permutoid reaction.
Wherein, when carrying out ion-exchange, water-soluble metal-salt directly mixes in reactor with layered titanate, does not need to add other material again.
The invention provides and a kind ofly prepare metal ion doped titanium dioxide (TiO with ion exchange method
2) method of line pipe, its advantage is: employed raw material is cheap and easy to get; Simple to operate easy to control; Doped Ti O
2Metal ion content in the line pipe is easy to control; Metal ion mixing TiO
2The pattern of line pipe remains unchanged substantially.
(4) description of drawings
Fig. 1: preparation metal ion mixing TiO
2The schema of line pipe.
The manganese ion doping TiO that Fig. 2: embodiment 2 prepares
2The electromicroscopic photograph of line pipe.
Manganese that Fig. 3: embodiment 8 prepares and cobalt ion codoped TiO
2The electromicroscopic photograph of line pipe.
The ion doping TiO that Fig. 4: embodiment 1, example 4 and example 10 prepare
2The X-ray diffraction of line pipe (XRD) spectrogram.
(5) embodiment
The present invention is described in further detail below in conjunction with embodiment.
The invention provides and a kind ofly prepare metal ion doped titanium dioxide (TiO with ion exchange method
2) method of line pipe, its preparation process is:
Take by weighing an amount of metal-salt, be dissolved in the water, add the layered titanate line pipe again and mix, in room temperature～240 ℃, carry out ion-exchange under the condition of 2～35 hours time, make and contain the layered titanate line pipe of the metal ion of exchange to some extent; Then,, be placed in the reactor, between 60～240 ℃, reacted 4～40 hours this layered titanate line pipe and the suitable quantity of water of the metal ion of exchange to some extent of containing.Specific examples is as follows:
Experimental example 1:With 1.0g Cadmium chloride fine powder (CdCl
2) be dissolved in the 30mL water, add 1.5g layered titanate (Na-Ti-O) line pipe, carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, to filter, washing makes and contains ion Cd
2+The layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Cd at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 2:With 1.0g Manganous chloride tetrahydrate (MnCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, to filter, washing makes and contains Mn
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Mn at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 3:With 1.0g manganous acetate (Mn (Ac)
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, to filter, washing makes and contains ion Mn
2+The layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Mn at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 4:With 0.1g Manganous chloride tetrahydrate (MnCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), directly react 10h at 160 ℃, can make Mn
2+Ion doping TiO
2Line pipe.
Experimental example 5:With 1.0g zinc chloride (ZnCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Zn
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Zn at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 6:With 1.0g cobalt chloride (CoCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Co
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Co at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 7:With 0.2g cobalt chloride (CoCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), react 10h at 160 ℃, can make Co
2+Ion doping TiO
2Line pipe.
Experimental example 8:With 0.5g cobalt chloride (CoCl
2) and 0.5g MnCl
2Be dissolved in jointly in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Mn
2+And Co
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Mn at 160 ℃
2+And Co
2+Ion doping TiO
2Line pipe.
Experimental example 9:With 0.1g mercury chloride (HgCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Hg
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Hg at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 10:With 1.0g lead acetate (Pb (Ac)
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Pb
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Pb at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 11:With 1.0g cupric chloride (CuCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Cu
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Cu at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 12:With 1.0g cupric chloride (CuCl
2) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Cu
2+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 2.0mL ethanol and 30mL water, react 10h, can make Cu at 160 ℃
2+Ion doping TiO
2Line pipe.
Experimental example 13:With 1.0g chromium chloride (CrCl
3) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Cr
3+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Cr at 160 ℃
3+Ion doping TiO
2Line pipe.
Experimental example 14:With 0.2g chromium chloride (CrCl
3) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), react 10h at 160 ℃, can make Cr
3+Ion doping TiO
2Line pipe.
Experimental example 15:With 0.2g Silver Nitrate (AgNO
3) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Ag
+Ionic layered titanate line pipe.Get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Ag at 160 ℃
+Ion doping TiO
2Line pipe.
Experimental example 16:With 0.2g europium nitrate (Eu (NO
3)
3) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), carry out ion-exchange 15h at 100 ℃, be as cold as room temperature, filtration is washed, and makes to contain Eu
3+Ionic layered titanate line pipe. get this line pipe 1.5g that exchanges and put into reactor again, and add 30mL water, react 10h, can make Eu at 160 ℃
3+Ion doping TiO
2Line pipe.
Experimental example 17:With 0.2g europium nitrate (Eu (NO
3)
3) be dissolved in the 30mL water, add 1.5g layered titanate line pipe (Na-Ti-O), react 10h at 160 ℃, can make Eu
3+Ion doping TiO
2Line pipe.
Claims (6)
1. method with preparation of metal ion doping titanium dioxide line pipe by ion exchange method, it is characterized in that: its preparation method is: take by weighing aequum layered titanate line pipe, it is mixed with water-soluble aqueous metal salt, in room temperature～240 ℃, under the condition of 2～35 hours time, by ion exchange method, make the layered titanate line pipe that contains the metal ion that exchanges; Then, the layered titanate line pipe that will contain the metal ion that exchanges is put into reactor, adds required water gaging, is heated to 60～240 ℃, and remains on and reacted under this temperature 4～40 hours, makes metal ion mixing TiO
2Line pipe.
2. method with preparation of metal ion doping titanium dioxide line pipe by ion exchange method, it is characterized in that: its preparation method is: get the aequum aqueous metal salt and put into reactor with the layered titanate line pipe, be heated to 60～240 ℃, and remain on and reacted under this temperature 4～40 hours, by ion-exchange and thermal treatment, make metal ion mixing TiO
2Line pipe.
3. a kind of method according to claim 1 with preparation of metal ion doping titanium dioxide line pipe by ion exchange method, it is characterized in that: this metal-salt is selected for use: Manganous chloride tetrahydrate, manganous acetate, cobalt chloride, cobaltous acetate, iron protochloride, iron trichloride, cupric chloride, copper sulfate, nickelous chloride, europium nitrate, Silver Nitrate, indium chloride.
4. a kind of method with preparation of metal ion doping titanium dioxide line pipe by ion exchange method according to claim 1, it is characterized in that: this layered titanate line pipe is selected for use: Na-Ti-O or K-Ti-O.
5. a kind of method according to claim 2 with preparation of metal ion doping titanium dioxide line pipe by ion exchange method, it is characterized in that: this metal-salt is selected for use: Manganous chloride tetrahydrate, manganous acetate, cobalt chloride, cobaltous acetate, iron protochloride, iron trichloride, cupric chloride, copper sulfate, nickelous chloride, europium nitrate, Silver Nitrate, indium chloride.
6. a kind of method with preparation of metal ion doping titanium dioxide line pipe by ion exchange method according to claim 2, it is characterized in that: this layered titanate line pipe is selected for use: Na-Ti-O or K-Ti-O.
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| CN1657186A (en) * | 2005-03-21 | 2005-08-24 | 付飘敏 | Preparation method of modified film by nanometer titanium dioxide doped of noble metal rare earth oxide |
| WO2006087841A1 (en) * | 2005-02-17 | 2006-08-24 | Osaka University | Titanium oxide nanotube and process for producing the same |
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| WO2006087841A1 (en) * | 2005-02-17 | 2006-08-24 | Osaka University | Titanium oxide nanotube and process for producing the same |
| CN1657186A (en) * | 2005-03-21 | 2005-08-24 | 付飘敏 | Preparation method of modified film by nanometer titanium dioxide doped of noble metal rare earth oxide |
Non-Patent Citations (6)
| Title |
|---|
| Liliane Magalhaes Nunes, Antonio Gouveia deSouza,Robson Fernandes de Farias,.Synthesis of new compounds involving layered titanatesandniobates with copper(II).Journal of Alloys and CompoundsVolume319 Issues1-2.2001,Volume319(Issues1-2),94-99. |
| Liliane Magalhaes Nunes, Antonio Gouveia deSouza,Robson Fernandes de Farias,.Synthesis of new compounds involving layered titanatesandniobates with copper(II).Journal of Alloys and CompoundsVolume319 Issues1-2.2001,Volume319(Issues1-2),94-99. * |
| Mingdeng Wei, Yoshinari Konishi,Haoshen Zhou,Hideki Sugihara, Hironori Arakawa,.Formation of nanotubes TiO2 from layered titanateparticlesbyasoft chemical process.Solid State CommunicationsVolume133 Issue8.2005,Volume133(Issue8),493-497. |
| Mingdeng Wei, Yoshinari Konishi,Haoshen Zhou,Hideki Sugihara, Hironori Arakawa,.Formation of nanotubes TiO2 from layered titanateparticlesbyasoft chemical process.Solid State CommunicationsVolume133 Issue8.2005,Volume133(Issue8),493-497. * |
| Viviane de A. Cardoso, Antonio G. de Souza, PatríciaP.C.Sartoratto, Liliane M. Nunes,.The ionic exchange process of cobalt, nickel and copper(II)inalkaline and acid-layered titanates.Colloids and Surfaces A: Physicochemical and Engineering Aspects,Volume248 Issues1-3.2004,Volume248(Issues1-3),145-149. |
| Viviane de A. Cardoso, Antonio G. de Souza, PatríciaP.C.Sartoratto, Liliane M. Nunes,.The ionic exchange process of cobalt, nickel and copper(II)inalkaline and acid-layered titanates.Colloids and Surfaces A: Physicochemical and Engineering Aspects,Volume248 Issues1-3.2004,Volume248(Issues1-3),145-149. * |
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