CN101234781A - Method for preparing high pure brookite type titanium dioxide nano-tube - Google Patents
Method for preparing high pure brookite type titanium dioxide nano-tube Download PDFInfo
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- CN101234781A CN101234781A CNA2008100706781A CN200810070678A CN101234781A CN 101234781 A CN101234781 A CN 101234781A CN A2008100706781 A CNA2008100706781 A CN A2008100706781A CN 200810070678 A CN200810070678 A CN 200810070678A CN 101234781 A CN101234781 A CN 101234781A
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Abstract
The invention provides a method for preparing brookite-type titanium dioxide nanotube of high-purity. Under lower temperature and under the condition that no surfactant and template agent is added, the method uses a simple hydrothermal method to prepare pure-phase brookite-type titanium dioxide nanotube with simple operation, low cost, stable performance, high purity and mass synthesis; length of the prepared brookite-type titanium dioxide nanotube is about a plurality of nanometers to tens of nanometers ; inner diameter is 5-6nm; the nanotube has high purity; the prepared brookite-type titanium dioxide nanotube is the excellent photocatalysis material which can be widely used for fields such as photodegradation of organic pollutant.
Description
Technical field
The invention belongs to field of nano material preparation, more specifically relate to a kind of preparation method of high pure brookite type titanium dioxide nano-tube.
Background technology
Brookite type titanium dioxide generally generates under the occurring in nature high-temperature and high-pressure conditions, is difficult to synthetic pure phase brookite with manual method.Therefore, the research of relevant brookite type titanium dioxide performance report seldom.It is reported that brookite type titanium dioxide has good photocatalysis performance.Although the synthetic pure phase brookite type titanium dioxide nanoparticle of report is arranged, the brookite type titanium dioxide nano material of one-dimentional structure (nanowires/nanotubes/nanometer rod/nano belt) also is not in the news.The relevant report that the preparation brookite type titanium dioxide nano-tube is not also arranged at present.
Goal of the invention
The preparation method who the purpose of this invention is to provide a kind of high pure brookite type titanium dioxide nano-tube, this method is added under the condition of any tensio-active agent and template at a lower temperature and not, prepared the pure phase brookite type titanium dioxide nano-tube with simple hydrothermal method, easy and simple to handle, cost is low, stable performance, the purity height, can synthesize in a large number, the brookite type titanium dioxide nano-tube length of preparation is about several nanometers to tens micron, internal diameter 5～6 nanometers.
The present invention adopts simple hydrothermal method preparation, the preparation method is: with 1～3 gram titania powder and 20～50 ml concns is the alkaline solution of 10 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 24～72h under 373～423K, the product pH value that generates is adjusted to 10～11, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 453～473K, react 24h, behind the distilled water thorough washing, dry 1～40h obtains final high pure brookite type titanium dioxide nano-tube under 323～373K.
Remarkable advantage of the present invention is: the present invention adopts simple hydrothermal method, add at a lower temperature and not under the condition of any tensio-active agent and template and prepared the pure phase brookite type titanium dioxide nano-tube, easy and simple to handle, cost is low, stable performance, the purity height, can synthesize in a large number, the brookite type titanium dioxide nano-tube length of preparation is about several nanometers to tens micron, internal diameter 5-6 nanometer.Brookite type titanium dioxide nano-tube of the present invention is a kind of good photocatalyst material, can be widely used in the aspect of photodegradation organic pollutant.The titanate nanotube presoma is that it consists of Na by sophisticated hydrothermal method synthetic
2Ti
2-xTi
3O
7This nanotube is the laminate structure that TiO6 forms by the mode on common limit, contains Na ion and H ion between layer and the layer.Discharge at Na ion that is higher than interlayer under the hydrothermal condition of 453K and H ion, and laminate structure changes, form highly purified brookite nanotube.
Description of drawings
Fig. 1 is the transmission electron microscope photo of product of the present invention, and wherein (a) part is the low power transmission electron microscope photo, and (b) part is the high power transmission electron microscope photo.
Embodiment
With 1～3 gram titania powder and 20～50 ml concns is the alkaline solution of 10 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 24～72h under 373～423K, the product pH value that generates is adjusted to 10～11, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 453～473K, react 24h, behind the distilled water thorough washing, dry 1～40h obtains final high pure brookite type titanium dioxide nano-tube under 323～373K.
Described alkaline solution is a caustic soda soln.The product pH value of described generation is regulated hydrochloric acid or the nitric acid that adopts 0.1～0.5 mol.The described dry constant pressure and dry that adopts.
The nanotube of preparation is the structure of multilayer scroll, its length 1nm～20 μ m, and internal diameter 5～6nm, purity is more than 99%.
The present invention of following examples specific description, but the present invention is not limited only to this.
Embodiment 1
Be the alkaline solution of 10 mol at first with 2.5g titania powder and 20 ml concns, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 24h under 373K, the product pH value that generates is adjusted to 11, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 453K, react 24h, behind the distilled water thorough washing, dry 1h obtains final high pure brookite type titanium dioxide nano-tube under 323K.Described alkaline solution is a caustic soda soln.The product pH value of described generation is regulated hydrochloric acid or the nitric acid that adopts 0.1～0.5 mol.The described dry constant pressure and dry that adopts.
The nanotube of preparation is the structure of multilayer scroll, its length 1nm～20 μ m, and internal diameter 5～6nm, purity is more than 99%.
Embodiment 2
Be the alkaline solution of 10 mol at first with 1g titania powder and 20 ml concns, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 72h under 373K, the product pH value that generates is adjusted to 10, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 453K, react 24h, behind the distilled water thorough washing, dry 1h obtains final high pure brookite type titanium dioxide nano-tube under 323K.Described alkaline solution is a caustic soda soln.The product pH value of described generation is regulated the hydrochloric acid that adopts 0.1 mol.The described dry constant pressure and dry that adopts.
The nanotube of preparation is the structure of multilayer scroll, its length 1nm～20 μ m, and internal diameter 5～6nm, purity is more than 99%.
Embodiment 3
Be the alkaline solution of 10 mol at first with 3g titania powder and 50 ml concns, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 30h under 423K, the product pH value that generates is adjusted to 11, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 473K, react 24h, behind the distilled water thorough washing, dry 40h obtains final high pure brookite type titanium dioxide nano-tube under 373K.Described alkaline solution is a caustic soda soln.The product pH value of described generation is regulated the nitric acid that adopts 0.5 mol.The described dry constant pressure and dry that adopts.
The nanotube of preparation is the structure of multilayer scroll, its length 1nm～20 μ m, and internal diameter 5～6nm, purity is more than 99%.
Embodiment 4
Be the alkaline solution of 10 mol at first with 2g titania powder and 30 ml concns, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 40h under 413K, the product pH value that generates is adjusted to 11, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 463K, react 24h, behind the distilled water thorough washing, dry 20h obtains final high pure brookite type titanium dioxide nano-tube under 353K.Described alkaline solution is a caustic soda soln.The product pH value of described generation is regulated hydrochloric acid or the nitric acid that adopts 0.3 mol.The described dry constant pressure and dry that adopts.
The nanotube of preparation is the structure of multilayer scroll, its length 1nm～20 μ m, and internal diameter 5～6nm, purity is more than 99%.
Embodiment 5
Be the alkaline solution of 10 mol at first with 2g titania powder and 30 ml concns, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 60h under 373K, the product pH value that generates is adjusted to 10.5, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 473K, react 24h, behind the distilled water thorough washing, dry 30h obtains final high pure brookite type titanium dioxide nano-tube under 353K.Described alkaline solution is a caustic soda soln.The product pH value of described generation is regulated hydrochloric acid or the nitric acid that adopts 0.4 mol.The described dry constant pressure and dry that adopts.
The nanotube of preparation is the structure of multilayer scroll, its length 1nm～20 μ m, and internal diameter 5～6nm, purity is more than 99%.
Claims (5)
1. the preparation method of a high pure brookite type titanium dioxide nano-tube, it is characterized in that: adopt simple hydrothermal method preparation, described preparation method is: with 1～3 gram titania powder and 20～50 ml concns is the alkaline solution of 10 mol, thorough mixing is even in stainless steel autoclave or polytetrafluoroethylcontainer container, mixture reacts 24～72h under 373～423K, the product pH value that generates is adjusted to 10～11, be placed on again in stainless steel autoclave or the polytetrafluoroethylcontainer container and under 453～473K, react 24h, behind the distilled water thorough washing, dry 1～40h obtains final high pure brookite type titanium dioxide nano-tube under 323～373K.
2. the preparation method of high pure brookite type titanium dioxide nano-tube according to claim 1, it is characterized in that: described alkaline solution is a caustic soda soln.
3. the preparation method of high pure brookite type titanium dioxide nano-tube according to claim 1 is characterized in that: the hydrochloric acid or the nitric acid of product pH value adjusting employing 0.1～0.5 mol of described generation.
4. the preparation method of high pure brookite type titanium dioxide nano-tube according to claim 1 is characterized in that: the described dry constant pressure and dry that adopts.
5. the preparation method of high pure brookite type titanium dioxide nano-tube according to claim 1, it is characterized in that: the nanotube of described preparation is the structure of multilayer scroll, its length 1nm～20 μ m, internal diameter 5～6nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880057A (en) * | 2010-06-04 | 2010-11-10 | 山东轻工业学院 | Method for preparing high-purity brookite titanium dioxide with controlled appearance |
| MD4063C1 (en) * | 2010-02-18 | 2011-03-31 | Технический университет Молдовы | Method for producing nanotubes of titanium dioxide on a titanium substrate |
| CN103288126A (en) * | 2013-05-14 | 2013-09-11 | 哈尔滨工程大学 | Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent |
| CN104525167A (en) * | 2014-12-16 | 2015-04-22 | 浙江理工大学 | Titanium dioxide nano tube and preparation method thereof |
| CN110963473A (en) * | 2019-12-23 | 2020-04-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon/titanium nitride nanotube composite material |
-
2008
- 2008-02-29 CN CNA2008100706781A patent/CN101234781A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| MD4063C1 (en) * | 2010-02-18 | 2011-03-31 | Технический университет Молдовы | Method for producing nanotubes of titanium dioxide on a titanium substrate |
| CN101880057A (en) * | 2010-06-04 | 2010-11-10 | 山东轻工业学院 | Method for preparing high-purity brookite titanium dioxide with controlled appearance |
| CN103288126A (en) * | 2013-05-14 | 2013-09-11 | 哈尔滨工程大学 | Method of preparing titanium dioxide nanotube with assistance of cationic surface active agent |
| CN104525167A (en) * | 2014-12-16 | 2015-04-22 | 浙江理工大学 | Titanium dioxide nano tube and preparation method thereof |
| CN110963473A (en) * | 2019-12-23 | 2020-04-07 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon/titanium nitride nanotube composite material |
| CN110963473B (en) * | 2019-12-23 | 2022-12-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of carbon/titanium nitride nanotube composite material |
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