CN1994558A - Method for preparing unidimensional TiO2 hollow structured photocatalyst using vanadium oxide nanobelt as template - Google Patents
Method for preparing unidimensional TiO2 hollow structured photocatalyst using vanadium oxide nanobelt as template Download PDFInfo
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Abstract
The invention relates to a method for using vanadia nanometer band as template to produce one-dimension TiO2 hollow optical catalyst, wherein said method comprises that: dissolving titanium tetrafluoride into deionized water; immerges the vanadia nanometer band into said solution to be treated at low temperature to obtain the final catalyst. The invention uses vanadia nanometer band template to induce the deposition of TiO2 nanometer particle to form corn-frame structure and the vanadia nanometer band template is dissolved by HF to form hollow structure. The inventive method can simplify the TiO2 surface deposition (or growth) and template removing process, to overcome the group and hard separate problems of powder optical catalyst.
Description
Technical field
The present invention relates to the one dimension TiO that is easy to separate
2The preparation method of hollow structured photocatalyst the invention still further relates to the simple and easy template preparing technical field of other oxide hollow structure material.
Technical background
In recent years, in order to solve serious environmental pollution problem day by day, the research and development of heterogeneous catalysis material have been subjected to countries in the world government and researcher's extensive attention, because this class catalysis material can be widely used in the purification of air, the sterilizing of water, the degraded of hazardous contaminant and removal etc. in the water.In all kinds of oxide semiconductor catalysis materials, facts have proved that the most suitable quilt of titanium dioxide is environmental applications widely, because titanium dioxide has the inertia of biological and chemical, very strong oxidability, the strong anti-light and the ability of chemical attack etc.The powder titanium dioxide optical catalyst, owing to have higher specific surface area, thereby the degraded to pollutant shows very high photocatalysis efficiency in wastewater treatment and water treatment procedure.Yet, because the grain diameter of powder art photochemical catalyst is less, making photochemical catalyst be easy to reunite in reaction system reclaims out with being difficult to separate from reactant mixture after light-catalyzed reaction, particularly in industrial wastewater photocatalysis treatment process, because separation difficulty causes the turnover rate of powder photocatalyst big, has seriously limited the development of photocatalysis technology.Thereby the length that is easy to separate and reclaims is at micron-sized one dimension TiO
2The preparation of photochemical catalyst has caused widely to be paid attention to.
At one dimension TiO
2In the preparation process of hollow structured photocatalyst, the most commonly used is the template synthetic method.The template synthetic method normally uses collosol and gel, electrochemical deposition and EFI method etc. with TiO
2Particle is deposited on the inwall (as porous aluminium) of template surface (as polymer fiber) or tubular form.Yet, all be unbodied TiO usually with the structural material of method for preparing
2, thereby must be again remove template and could form hollow-core construction through the method for high-temperature heat treatment or dissolved corrosion, this just causes template complicated in preparing the hollow material process.Simultaneously, in removing the process of template, cause the destruction of hollow-core construction, thereby this has just limited the extensive use of template through regular meeting.In order to simplify template at preparation TiO
2Must experience TiO in the hollow structured photocatalyst
2In the complex process of template surface deposition (or growth) and template removal, and, develop low temperature crystallized one dimension TiO from the consideration of energy-conservation aspect
2The simple and easy template technology of preparing of hollow structured photocatalyst is inevitable.
Summary of the invention
According to present domestic and international research present situation, consider complexity and the titanium dioxide powder photocatalyst deficiency that in use exist of common template in preparation hollow structure material process, the present invention proposes a kind of is template one step preparation one dimension TiO with vanadium oxide nanometer band
2The method of hollow structured photocatalyst.Adopt method of the present invention can prepare length 5-400 micron, specific area 50-90 rice
2/ gram is by the TiO of diameter in the 10-55 nanometer
2The molecular one dimension TiO of nanoparticle
2Hollow structured photocatalyst.
With vanadium oxide nanometer band is template one step preparation one dimension TiO
2The basic principle of hollow structured photocatalyst: the hydrolysis formula of titanium tetrafluoride in deionized water is: TiF
4+ H
2O → Ti (OH)
4+ 4HF.Therefore the hydrolysis of titanium tetrafluoride is forming TiO
2In the time of particle, also produced accessory substance HF.Experiment showed, that in HF solution (pH is 1.7) adds a certain amount of vanadium oxide nanometer band, when temperature be controlled at 25-60 ℃ and be incubated 3-6 hour after, vanadium oxide nanometer band can dissolve the formation settled solution fully.Therefore we propose one dimension TiO
2The forming process of hollow structured photocatalyst: TiO at first
2Nano particle carries out heterogeneous nucleation and growth (as Figure 1A 1), TiO afterwards on the both sides of vanadium oxide nanometer belt surface
2Nano particle from the both sides of nanometer band gradually to the interstitial growth of band, up to the nanometer band fully by TiO
2Nano particle coats and forms nucleocapsid structure (as Figure 1A 2).Simultaneously, because the continuous hydrolysis of titanium tetrafluoride causes the increase of HF concentration in the reaction solution, thereby after nucleocapsid structure formed, vanadium oxide nanometer band was dissolved by HF gradually, causes the formation (as Figure 1A 3) of hollow-core construction.
According to above-mentioned analysis, realize that the technical scheme of the object of the invention is:
A kind of is that template prepares one dimension TiO with vanadium oxide nanometer band
2The method of hollow structured photocatalyst is characterized in that low temperature template preparation method, and preparation process is followed successively by:
1st, the length with the vanadium oxide nanometer band template of Hydrothermal Preparation is the 10-400 micron, and width is the 100-300 nanometer, and thickness is the 20-50 nanometer;
2nd, titanium tetrafluoride being dissolved in deionized water for stirring and evenly forming reaction solution, is 0-6 with the pH value of 1 mol hydrochloric acid and 1 mol NaOH conditioned reaction solution, and wherein the molar concentration of titanium tetrafluoride is the 0.001-0.1 mol;
3rd, 0.001 gram vanadium oxide nanometer band of step 1 preparation is immersed in 60 milliliters of reaction solutions of step 2 preparation, puts into temperature after the sealing and be 30-90 ℃ baking oven insulation and handled 8-20 hour, must contain white depositions solution;
4th, take out the reaction solution that insulation is handled through step 3, white depositions is filtered, and wash respectively with deionized water and absolute ethyl alcohol, vacuum drying in 50-80 ℃ at last can obtain one dimension TiO
2Hollow structured photocatalyst.
The preferred for preparation condition of this method is: the concentration of titanium tetrafluoride is the 0.005-0.05 mol in the reaction solution; The pH of solution is 1-3; Reaction temperature is 50-70 ℃; Reaction time is 10-15 hour; The white reaction product that obtains washes 3-5 time respectively with deionized water and absolute ethyl alcohol; Vacuum drying temperature is 50-80 ℃; 4-10 hour vacuum drying time.
Preparation method's step of described vanadium oxide nanometer band template is:
1st, the ammonium metavanadate of 0.01-0.1 gram and the PEG400 of 0.1-0.5 gram are joined in 30 ml deionized water, stir;
2nd, the pH with 1 mol hydrochloric acid and 1 mol NaOH regulating step, 1 gained solution is 2-4;
3rd, the resulting reaction solution of step 2 is put into 50 milliliters water heating kettle, be incubated 20-30 hour down, generate vanadium oxide nanometer band precipitation at 180-200 ℃;
4th, with behind the resulting sedimentation and filtration of step 3, wash 3-5 time respectively, at 50-80 ℃ of following vacuum drying 4-10 hour, promptly obtain vanadium oxide nanometer band then with deionized water and absolute ethyl alcohol.
The present invention is said to be used to prepare TiO
2The template of hollow-core construction can also be a vanadium oxide nanostructured with other special appearance as nanometer rods, nanotube, nanofiber, nanoneedle, nano particle etc. except vanadium oxide nanometer band.
The photocatalytic activity of one-dimensional titanium dioxide hollow structured photocatalyst characterizes by the photocatalytic degradation methyl orange solution.Experimentation is as follows: 0.02 gram titanium dioxide optical catalyst is dispersed in 25 milliliters of methyl orange aqueous solutions (3.1 * 10 are housed
-5Mol) in the quartz glass groove (52W * 155L * 20H millimeter).The wavelength of ultraviolet source (Cole-Parmer Instrument Co.) is 365 nanometers, and power is 15 watts.The average intensity that impinges upon the methyl orange liquid level be 112 microwatts/centimetre
2, its size is to be measured by the UV radiometer that Beijing Normal University produces.Every 20 minutes, reaction solution carried out isolated by filtration earlier, measured the methyl orange concentration in the reaction solution then.In the degradation solution concentration of methyl orange by ultraviolet-visible absorption spectroscopy measure (UV-2550, SHIMADZU, Japan).
Description of drawings
Fig. 1 one dimension TiO
2The formation mechanism of hollow-core construction (the latter half difference corresponding templates of figure is at the cross section in each stage): wherein A1 is TiO
2Nano particle carries out heterogeneous nucleation and growth on vanadium oxide nanometer belt surface both sides; A2 is TiO
2Nano particle gradually to the interstitial growth of band, forms nucleocapsid structure from the both sides of nanometer band; A3 is dissolved by HF gradually by vanadium oxide nanometer band, causes the formation of hollow-core construction
(B1 is B2) with one dimension TiO for the vanadium oxide nanometer band template of Fig. 2 embodiment 1 preparation
2Hollow structured photocatalyst (B3, FESEM picture B4)
The vanadium oxide nanometer band template (C1) and the one dimension TiO of Fig. 3 embodiment 1 preparation
2The XRD figure spectrum of hollow structured photocatalyst (C2)
The one dimension TiO of Fig. 4 embodiment 1 preparation
2TEM of hollow structured photocatalyst (D1) and HRTEM (D2) picture; What insert among the figure D1 is corresponding electron diffraction diagram
The one dimension TiO of Fig. 5 embodiment 1 preparation
2Hollow structured photocatalyst to the photocatalytic degradation of methyl orange: E1 for not adding photochemical catalyst; E2 is for adding one dimension TiO
2Hollow structured photocatalyst.
The specific embodiment
Embodiment 1:
The preparation of vanadium oxide nanometer band template: 0.06 gram ammonium metavanadate and 0.25 gram PEG400 are joined in 30 ml deionized water and stir, the pH value to 3 of regulating above-mentioned solution with 1 mol hydrochloric acid and 1 mol NaOH.Then reaction solution is transferred in 50 milliliters the water heating kettle 190 ± 2 ℃ of insulations 24 hours down.After reaction is finished,, and wash respectively 3 times, in 60 ± 2 ℃ of following vacuum drying 8 hours, promptly obtain vanadium oxide nanometer band at last with deionized water and absolute ethyl alcohol the sediment isolated by filtration.Fig. 2 B1 and 2B2 have shown the field emission scanning electron microscope picture of vanadium oxide nanometer band.As can be seen from the figure, be the nanometer band structure with the prepared product of this hydrothermal method, its length is at the 10-400 micron, and width is the 100-300 nanometer, and thickness probably is 35 nanometers.Fig. 3 C1 has shown the XRD figure spectrum of prepared nanometer band structure, shows that its crystal structure is the stratiform vanadium oxide.According to the elemental composition analysis of XPS, the molecular formula of this nanometer band is VO
2.360.49H
2O.
One dimension TiO
2The preparation of hollow structured photocatalyst: titanium tetrafluoride is dissolved in deionized water for stirring evenly forms reaction solution, 0.001 gram vanadium oxide nanometer band is immersed in the TiF that 60 ml concns are 0.005 mol
4In the reaction solution, the pH of solution is about 1.9, is that 60 ± 2 ℃ baking oven insulation was handled 12 hours putting into temperature after the reaction solution sealing.Take out reaction solution, white depositions is filtered, and wash respectively 3 times,, can obtain one dimension TiO in 60 ± 2 ℃ of vacuum drying 8 hours with deionized water and absolute ethyl alcohol
2Hollow structured photocatalyst.Fig. 2 B3 and 2B4 have shown one dimension TiO
2The field emission scanning electron microscope picture of hollow structured photocatalyst.As can be seen from the figure, prepared TiO
2Photochemical catalyst has kept the pattern of nanometer band template, and its length is usually greater than 5 microns.Simultaneously, the TiO of this one dimension
2Structure is made up of at the granule of 10-55 nanometer many particle diameters.The XRD figure spectrum (Fig. 3 C2) of this sample shows that its crystal structure is pure anatase TiO
2, and do not have the existence of vanadium oxide phase.TEM among Fig. 4 D1 has proved prepared one dimension TiO
2Sample is a hollow-core construction.HRTEM (Fig. 4 D2) has proved further that also the crystal structure of this hollow-core construction is the anatase phase simultaneously.
Fig. 5 is one dimension TiO
2Hollow structured photocatalyst is to the degradation curve of methyl orange solution.As can be seen, when not adding photochemical catalyst, ultraviolet lighting can not cause the decline of methyl orange concentration from Fig. 5 E1.On the contrary, methyl orange concentration a little a bit rises, and this mainly is because a small amount of evaporation of water is arranged under illumination, causes due to the rising of methyl orange concentration.When adding prepared one dimension TiO
2During hollow photochemical catalyst (Fig. 5 E2), along with the prolongation of light application time, methyl orange concentration descends rapidly, shows that methyl orange effectively degraded by photochemical catalyst.
TiO for practical application
2Photochemical catalyst, except should having high photocatalytic activity, its Preparation of catalysts process should be tried one's best simply, and particularly employed catalyst is easy to separate from solution and can reuses after photocatalysis wastewater treatment and water purification.Nanometer powder titanium dioxide optical catalyst such as P25, owing to have higher specific surface area, thereby the degraded of all contaminations is shown very high photocatalysis efficiency.Yet,, make photochemical catalyst in reaction system, be easy to reunite and reclaim out with after light-catalyzed reaction, being difficult to from reactant mixture, separate because the grain diameter of powder photocatalyst is less.The one dimension TiO of the present invention's preparation
2Its length of photochemical catalyst is in the micron order scope, thereby behind photocatalysis degradation organic contaminant, is easy to separate from reaction solution and enter recycling next time.Simultaneously, its wall shell of prepared in this way photochemical catalyst has meso-hole structure, and the interior organic reactant of shell and the product of degraded are effectively transmitted by the mesopore orbit between hole wall, thereby increases the efficient of light-catalyzed reaction.
Embodiment 2:
For the concentration of checking titanium tetrafluoride to one dimension TiO
2The influence of hollow-core construction pattern, except that the concentration difference of titanium tetrafluoride, other reaction condition as: the pH value of reaction solution, the reaction temperature of solution, the reaction time of solution etc. are all identical with embodiment 1.The result shows, when the concentration of titanium tetrafluoride is higher than 0.1 mol, because prepared TiO
2The shell of hollow-core construction is very thick, is difficult to find out its hollow-core construction with TEM; When the concentration of titanium tetrafluoride is lower than 0.001 mol, because TiO in the system
2Content less, vanadium oxide nanometer belt surface can not be coated fully, causes uneven hollow-core construction, simultaneously, the reduction of titanium tetrafluoride concentration causes vanadium oxide nanometer band template not dissolved by HF fully.The concentration of best titanium tetrafluoride is the 0.005-0.05 mol.
Embodiment 3:
For the pH value of checking reaction solution to one dimension TiO
2The influence of hollow-core construction pattern, except that the pH value difference of reaction solution, other reaction condition as: the reaction time of the concentration of reaction solution, the reaction temperature of solution, solution etc. are all identical with embodiment 1.The result shows that when the pH of reaction solution value was higher than 6, tangible white precipitate appearred in solution, and this precipitation is deposited on container bottom and does not deposit to template surface, is difficult to obtain one dimension TiO
2Hollow-core construction, simultaneously because the increase of titanium tetrafluoride hydrolysis rate causes the crystallization degree of titanium dioxide granule to reduce; H when reaction solution
+When ion is very high (pH＜0), because H
+The existence of ion can suppress the hydrolysis of titanium tetrafluoride, thereby needs the longer processing time.The pH value of optimum response solution is 1-3.
Embodiment 4:
For the reaction temperature of test solution to one dimension TiO
2The influence of hollow-core construction pattern, except that the reaction temperature difference of solution, other reaction condition as: the pH value of the concentration of titanium tetrafluoride, reaction solution, the reaction time of solution etc. are all identical with embodiment 1.The result shows that when the reaction temperature of solution was lower than 30 ± 2 ℃, the hydrolysis reaction of titanium tetrafluoride was too slow, and the sedimentation rate of titanium dioxide granule is too low, needs the very long reaction time of experience; When reaction temperature was higher than 90 ± 2 ℃, the hydrolysis reaction of titanium tetrafluoride was too fast, and titanium dioxide directly forms powder deposition in container bottom, influenced the deposition quantity of the particle of vanadium oxide nanometer band template surface.The optimal reaction temperature of reaction solution is 50-70 ℃.
Embodiment 5:
For reaction time of test solution to one dimension TiO
2The influence of hollow-core construction pattern, except that the reaction time difference of solution, other reaction condition as: the pH value of the concentration of titanium tetrafluoride, reaction solution, the reaction temperature of solution etc. are all identical with embodiment 1.The result shows that titanium tetrafluoride did not have complete hydrolysis and formed titanium dioxide granule and be deposited on vanadium oxide nanometer band template surface, can cause the waste of raw material when being less than 8 hours the reaction time of solution, and simultaneous oxidation vanadium nanometer band template can not be removed fully; When reaction time during greater than 20 hours, to one dimension TiO
2The pattern influence of hollow-core construction is very little, considers from energy-conservation angle, can cause the waste of the energy.The optimum reacting time of reaction solution is 10-15 hour.
Claims (8)
1, a kind of is that template prepares one dimension TiO with vanadium oxide nanometer band
2The method of hollow structured photocatalyst is characterized in that method step is followed successively by:
1st, the vanadium oxide nanometer band with Hydrothermal Preparation is a template, and the length of template is the 10-400 micron, and width is the 100-300 nanometer, and thickness is the 20-50 nanometer;
2nd, titanium tetrafluoride being dissolved in deionized water for stirring and evenly forming reaction solution, is 0-6 with the pH value of 1 mol hydrochloric acid and 1 mol NaOH conditioned reaction solution, and wherein the molar concentration of titanium tetrafluoride is the 0.001-0.1 mol;
3rd, 0.001 gram vanadium oxide nanometer band of step 1 preparation is immersed in 60 milliliters of reaction solutions of step 2 preparation, puts into temperature after the sealing and be 30-90 ℃ baking oven insulation and handled 8-20 hour, must contain white depositions solution;
4th, take out the reaction solution that insulation is handled through step 3, white depositions is filtered, and wash respectively with deionized water and absolute ethyl alcohol, vacuum drying in 50-80 ℃ at last promptly obtains one dimension TiO
2Hollow structured photocatalyst.
2, preparation one dimension TiO as claimed in claim 1
2The method of hollow structured photocatalyst, the molar concentration that it is characterized in that titanium tetrafluoride in the reaction solution is the 0.005-0.05 mol.
3, preparation one dimension TiO as claimed in claim 1
2The method of hollow structured photocatalyst is characterized in that the pH value of reaction solution is 1-3.
4, preparation one dimension TiO as claimed in claim 1
2The method of hollow structured photocatalyst, the reaction temperature that it is characterized in that reaction solution is 50-70 ℃.
5, preparation one dimension TiO as claimed in claim 1
2The method of hollow structured photocatalyst, the reaction time that it is characterized in that reaction solution is 10-15 hour.
6, preparation one dimension TiO as claimed in claim 1
2The method of hollow structured photocatalyst is characterized in that the white reaction product that obtains washes 3-5 time respectively with deionized water and absolute ethyl alcohol.
7, preparation one dimension TiO as claimed in claim 1
2The method of hollow structured photocatalyst is characterized in that vacuum drying temperature is 50-80 ℃; The vacuum drying time is 4-10 hour.
8, the hydrothermal preparing process of the used vanadium oxide nanometer band of claim 1 is characterized in that the preparation method step is:
1st, the ammonium metavanadate of 0.01-0.1 gram and the PEG400 of 0.1-0.5 gram are joined in 30 ml deionized water, stir;
2nd, the pH with 1 mol hydrochloric acid and 1 mol NaOH regulating step, 1 gained solution is 2-4;
3rd, the resulting reaction solution of step 2 is put into 50 milliliters water heating kettle, be incubated 20-30 hour down, generate vanadium oxide nanometer band precipitation at 180-200 ℃;
4th, with behind the resulting sedimentation and filtration of step 3, wash 3-5 time respectively, at 50-80 ℃ of following vacuum drying 4-10 hour, promptly obtain vanadium oxide nanometer band then with deionized water and absolute ethyl alcohol.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920513A (en) * | 2014-04-29 | 2014-07-16 | 山东大学 | Ti<3+>:TiO2/TiF3 composite semiconductor photocatalyst and preparation method thereof |
| CN104773757A (en) * | 2015-05-04 | 2015-07-15 | 哈尔滨工业大学 | Method for preparing hollow nanostructure constructed by TiO2 nanorods |
| CN105692625A (en) * | 2014-11-24 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Preparation method of oxide nanotube and nanobelt |
| CN107779905A (en) * | 2017-09-19 | 2018-03-09 | 同济大学 | A kind of preparation method of vanadium oxide nanobelt |
| CN114180620A (en) * | 2021-11-30 | 2022-03-15 | 陕西科技大学 | Preparation method for preparing titanium dioxide/carbon cathode by taking polypyrrole as template |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4486400A (en) * | 1983-05-25 | 1984-12-04 | Combustion Engineering, Inc. | Vanadium oxide synthesis |
| US5718878A (en) * | 1996-07-12 | 1998-02-17 | Akzo Nobel N.V. | Mesoporous titania and process for its preparation |
| CN100515556C (en) * | 2004-12-29 | 2009-07-22 | 上海杰事杰新材料股份有限公司 | Nano hollow microsphere of composite titania / inorganic carbon, preparation method and application |
| CN1699644A (en) * | 2005-04-29 | 2005-11-23 | 中国科学院青海盐湖研究所 | Titanium dioxide hollow fiber with high length-diameter ratio and high specific surface area and preparation method thereof |
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2006
- 2006-12-19 CN CNB2006101255200A patent/CN100453166C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103920513A (en) * | 2014-04-29 | 2014-07-16 | 山东大学 | Ti<3+>:TiO2/TiF3 composite semiconductor photocatalyst and preparation method thereof |
| CN105692625A (en) * | 2014-11-24 | 2016-06-22 | 中国科学院上海硅酸盐研究所 | Preparation method of oxide nanotube and nanobelt |
| CN104773757A (en) * | 2015-05-04 | 2015-07-15 | 哈尔滨工业大学 | Method for preparing hollow nanostructure constructed by TiO2 nanorods |
| CN107779905A (en) * | 2017-09-19 | 2018-03-09 | 同济大学 | A kind of preparation method of vanadium oxide nanobelt |
| CN114180620A (en) * | 2021-11-30 | 2022-03-15 | 陕西科技大学 | Preparation method for preparing titanium dioxide/carbon cathode by taking polypyrrole as template |
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