CN104475096B - A kind of TiO of Au Nanoparticle Modifieds2The preparation method of nano wire photochemical catalyst - Google Patents
A kind of TiO of Au Nanoparticle Modifieds2The preparation method of nano wire photochemical catalyst Download PDFInfo
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Abstract
The invention discloses a kind of TiO of Au Nanoparticle Modifieds2The preparation method of nano wire photochemical catalyst, step is as follows:Titanium sheet is cleaned to the greasy dirt and oxide layer that surface is removed with pickling by ethanol respectively, surface is polished until uniform and smooth, and oxidation processes are carried out to it by anodizing, the method boosted using ladder, anodized, calcined in atmosphere after oxidation processes;Using the method for absorption photo-reduction to TiO2Nano wire carries out Au Nanoparticle Modifieds, TiO2Nano wire is immersed in chlorauric acid solution, and UV illumination is carried out under stirring, and deionized water rinsing, drying are used after processing.The present invention has higher photocatalytic activity under simulation solar radiation, improves the utilization to visible ray, and preparation method is simple, and control is easy in reaction;As the photochemical catalyst of immobilization, it is easy to be separated from the water, it is to avoid produce new pollution, removal Organic Pollutants In Water has good stability and repeatable usability.
Description
Technical field
The present invention relates to a kind of preparation method of photochemical catalyst, more particularly to a kind of TiO of Au Nanoparticle Modifieds2Nanometer
The preparation method of linear light catalyst.
Background technology
Because semiconductor light-catalyst has some superior performances in field of environment pollution control, therefore, nearly tens
Year has attracted the interest of researcher.TiO2Photochemical catalyst has perfect photocatalysis performance, stable chemical nature, and no poison
Property, it is considered to be a kind of more satisfactory material for producing clean energy resource and environmental improvement.TiO2Nanostructured, such as,
Nanotube, nano wire, quantum dot and nanofiber, due to having special performance in terms of photocatalytic applications, are caused big
Quantifier elimination interest.TiO2The geometrical morphology of photochemical catalyst plays vital effect to its photocatalysis performance, with perfection
The photochemical catalyst of pattern can increase accessible surface product, improve the accessibility to object, and then improve the drop to pollutant
Solution efficiency.
But, TiO2The band gap of photochemical catalyst is 3.2eV, can only absorb ultraviolet light, and ultraviolet light only accounts for daylight light
The 3% of spectrum, therefore, limit it and be widely applied.Additionally, previous most of TiO2Photochemical catalyst is all the shape using powder
Formula, has catalyst and is difficult to reclaim or even can cause the problem of nanometer pollutes.
The content of the invention
It is an object of the invention to solve deficiency of the prior art, there is provided a kind of TiO of Au Nanoparticle Modifieds2Nanometer
Line (Au/TiO2Nano wire) photochemical catalyst preparation method, the Au/TiO of preparation2Nano wire photochemical catalyst can be effectively with water
Organic pollution haptoreaction in body, Au nano-particles are uniformly supported on TiO2Nanowire surface, particle diameter is nanoscale, tool
There is visible light photocatalysis active and good stability, and be easy to reuse.
To achieve these goals, the technical solution of use is the present invention:A kind of Au/TiO2Nano wire photochemical catalyst
Preparation method, step is as follows:
First, TiO2It is prepared by nano wire:Titanium sheet is cleaned to the greasy dirt and oxide layer that surface is removed with pickling by ethanol respectively,
Then the surface of titanium sheet is polished with the sand paper of 1000 mesh, until surface is uniform and smooth, using anodizing to it
Oxidation processes are carried out, electrolyte is the ethylene glycol solution of water, and the content of water is 3.5~4.5% (v/v), and ammonium fluoride content is 0.4
~0.5wt%, the method boosted using ladder, the rate of rise is to raise 1 volt in every 2 seconds, and ceiling voltage is at 60V, anodic oxidation
The reason time be 2.5h, after oxidation processes in atmosphere 450~490 DEG C calcining 1~2h;
2nd, Au Nanoparticle Modifieds:Using the method for absorption-photo-reduction to TiO2Nano wire carries out Au nano-particles and repaiied
Decorations, Jin Yuan is chlorauric acid solution, and concentration is 1~2mmolL-1, the TiO that anodized is crossed2Nano wire is immersed in gold chloride
In solution, power is used under stirring for 12W 1~2h of UV illumination, deionized water rinsing, drying system are used after processing
Standby Au/TiO2Nano wire photochemical catalyst.
Further, the photochemical catalyst obtained in the step 2, simulation solar radiation decline solution methyl orange solution with
Its photocatalysis performance is evaluated, methyl orange solution concentration is 5mg/L, the light application time 2h under 35W xenon lamps.In degradation process every
30min is sampled, and detects the change in concentration of methyl orange.
Further, the titanium sheet is purity 99.8%.
Further, the titanium sheet is length 10cm, width 1cm rectangle.
Further, pickle used is HF: HNO in the pickling3∶H2O is mixed according to 1~2: 4~5: 8~10 volume ratios
Conjunction is formed.
The beneficial effects of the invention are as follows:The Au/TiO prepared by above-mentioned technique2Nano wire photochemical catalyst is in simulation daylight
Irradiation is lower to have higher photocatalytic activity, improves the utilization to visible ray, and preparation method is simple, and control is easy in reaction;
The Au/TiO of preparation2Nano wire photochemical catalyst is the photochemical catalyst of immobilization, be easy to be separated from water, it is to avoid to water body
New pollution is produced, and with good stability and repeatable usability, the removal available for Organic Pollutants In Water.
Brief description of the drawings
The invention will be further elaborated with reference to the accompanying drawings and examples.
Fig. 1 is Au/TiO prepared by embodiment 22The stereoscan photograph of nano wire.
Fig. 2 is Au/TiO prepared by embodiment 22The light absorbs spectrogram of nano wire, and with pure TiO2Nano wire compares.
Fig. 3 is Au/TiO prepared by embodiment 22The EDX spectrograms of nano wire.
Fig. 4 is Au/TiO prepared by embodiment 22The clearance and light of nano wire photocatalytic degradation 5mg/L methyl orange solutions
According to time chart, and with pure TiO2Nano wire compares.
Specific embodiment
Embodiment 1
A kind of Au/TiO2The preparation method of nano wire photochemical catalyst, step is as follows:
First, TiO2It is prepared by nano wire:Titanium sheet is cleaned to the greasy dirt and oxide layer that surface is removed with pickling by ethanol respectively,
Then the surface of titanium sheet is polished with the sand paper of 1000 mesh, until surface is uniform and smooth, using anodizing to it
Oxidation processes are carried out, electrolyte is the ethylene glycol solution of water, and the content of water is 3.5% (v/v), and ammonium fluoride content is 0.4wt%,
The method boosted using ladder, the rate of rise is to raise 1 volt in every 2 seconds, and ceiling voltage is 60V, and the anodized time is
2.5h, after oxidation processes in atmosphere 450 DEG C calcining 1h;
2nd, Au Nanoparticle Modifieds:Using the method for absorption-photo-reduction to TiO2Nano wire carries out Au nano-particles and repaiied
Decorations, Jin Yuan is chlorauric acid solution, and concentration is 1mmolL-1, the TiO that anodized is crossed2It is molten that nano wire is immersed in gold chloride
In liquid, it is the UV illumination 1h of 12W, the sample deionized water rinsing after treatment, drying that power is used under stirring
Prepare Au/TiO2Nano wire photochemical catalyst.
The photochemical catalyst obtained in the step 2, declines solution methyl orange solution and is urged with evaluating its light in simulation solar radiation
Change performance, methyl orange solution concentration is 5mg/L, the light application time 2h under 35W xenon lamps.Sampled every 30min in degradation process, inspection
Survey the change in concentration of methyl orange.
The titanium sheet is purity 99.8%.The titanium sheet is length 10cm, the rectangle of width 1cm.
Pickle used is HF: HNO in the pickling3∶H2O is mixed according to 1: 4: 10 volume ratio.
Embodiment 2
A kind of Au/TiO2The preparation method of nano wire photochemical catalyst, step is as follows:
First, TiO2It is prepared by nano wire:Titanium sheet is cleaned to the greasy dirt and oxide layer that surface is removed with pickling by ethanol respectively,
Then the surface of titanium sheet is polished with the sand paper of 1000 mesh, until surface is uniform and smooth, using anodizing to it
Oxidation processes are carried out, electrolyte is the ethylene glycol solution of water, and the content of water is 4% (v/v), and ammonium fluoride content is 0.45wt%,
The method boosted using ladder, the rate of rise is to raise 1 volt in every 2 seconds, and ceiling voltage is 60V, and the anodized time is
2.5h, after oxidation processes in atmosphere 450 DEG C calcining 2h;
2nd, Au Nanoparticle Modifieds:Using the method for absorption-photo-reduction to TiO2Nano wire carries out Au nano-particles and repaiies
Decorations, Jin Yuan is chlorauric acid solution, and concentration is 1mmolL-1, the TiO that anodized is crossed2It is molten that nano wire is immersed in gold chloride
In liquid, power is used under stirring for 12W UV illumination 1.5h, the sample deionized water rinsing after processing dries
Drying standby Au/TiO2Nano wire photochemical catalyst.
The photochemical catalyst obtained in the step 2, declines solution methyl orange solution in simulation solar radiation and is urged with evaluating its light
Change performance, methyl orange solution concentration is 5mg/L, the light application time 2h under 35W xenon lamps.Sampled every 30min in degradation process, inspection
Survey the change in concentration of methyl orange.
The titanium sheet is purity 99.8%.The titanium sheet is length 10cm, width 1cm rectangle.
Pickle used is HF: HNO in the pickling3∶H2O is mixed according to 1: 4: 10 volume ratio.
Embodiment 3
A kind of Au/TiO2The preparation method of nano wire photochemical catalyst, step is as follows:
First, TiO2It is prepared by nano wire:Titanium sheet is cleaned to the greasy dirt and oxide layer that surface is removed with pickling by ethanol respectively,
Then the surface of titanium sheet is polished with the sand paper of 1000 mesh, until surface is uniform and smooth, using anodizing to it
Oxidation processes are carried out, electrolyte is the ethylene glycol solution of water, and the content of water is 4.5% (v/v), and ammonium fluoride content is 0.5wt%,
The method boosted using ladder, the rate of rise is to raise 1 volt in every 2 seconds, and ceiling voltage is 60V, and the anodized time is
2.5h, after oxidation processes in atmosphere 490 DEG C calcining 1h;
2nd, Au Nanoparticle Modifieds:Using the method for absorption-photo-reduction to TiO2Nano wire carries out Au nano-particles and repaiied
Decorations, Jin Yuan is chlorauric acid solution, and concentration is 2mmolL-1, the TiO that anodized is crossed2It is molten that nano wire is immersed in gold chloride
In liquid, it is the UV illumination 1h of 12W, the sample deionized water rinsing after treatment, drying that power is used under stirring
Prepare Au/TiO2Nano wire photochemical catalyst.
The photochemical catalyst obtained in the step 2, declines solution methyl orange solution in simulation solar radiation and is urged with evaluating its light
Change performance, methyl orange solution concentration is 5mg/L, the light application time 2h under 35W xenon lamps.Sampled every 30min in degradation process, inspection
Survey the change in concentration of methyl orange.
The titanium sheet is purity 99.8%.The titanium sheet is length 10cm, the rectangle of width 1cm.
Pickle used is HF: HNO in the pickling3∶H2O is mixed according to 1: 4: 10 volume ratio.
The Au/TiO prepared by above-mentioned technique2Nano wire photochemical catalyst under simulation solar radiation there is higher light to urge
Change activity, improve the utilization to visible ray, and preparation method is simple, control is easy in reaction;The Au/TiO of preparation2Nano wire
Photochemical catalyst is the photochemical catalyst of immobilization, be easy to be separated from water, it is to avoid new pollution is produced to water body, and is had
There are good stability and repeatable usability, the removal available for Organic Pollutants In Water.
Described above is not limitation of the present invention, and the present invention is also not limited to the example above, the art
Change, remodeling, addition or replacement that technical staff is made in the essential scope of the present invention, should also belong to the protection of the present invention
Scope.
Claims (5)
1. a kind of TiO of Au Nanoparticle Modifieds2The preparation method of nano wire photochemical catalyst, it is characterised in that step is as follows:
First, TiO2It is prepared by nano wire:Titanium sheet is cleaned into greasy dirt and oxide layer that surface is removed with pickling by ethanol respectively, then
The surface of titanium sheet is polished with the sand paper of 1000 mesh, until surface is uniform and smooth, it is carried out using anodizing
Oxidation processes, electrolyte is the ethylene glycol solution of water, and the content of water is 3.5~4.5% (v/v), ammonium fluoride content is 0.4~
0.5wt%, the method boosted using ladder, the rate of rise is to raise 1 volt in every 2 seconds, and ceiling voltage is 60V, anodized
Time is 450~490 DEG C of 1~2h of calcining in atmosphere after 2.5h, oxidation processes;
2nd, Au Nanoparticle Modifieds:Using the method for absorption-photo-reduction to TiO2Nano wire carries out Au Nanoparticle Modifieds, Jin Yuan
For chlorauric acid solution, concentration is 1~2 mmolL-1, the TiO that anodized is crossed2Nano wire is immersed in chlorauric acid solution
In, power is used under stirring for 12W 1~2h of UV illumination, with deionized water rinsing, drying after processing, is prepared
The TiO of Au Nanoparticle Modifieds2Nano wire photochemical catalyst.
2. the TiO of Au Nanoparticle Modifieds according to claim 12The preparation method of nano wire photochemical catalyst, its feature exists
In:The photochemical catalyst obtained in the step 2, declines solution methyl orange solution to evaluate its photocatalytic in simulation solar radiation
Can, methyl orange solution concentration is 5mg/L, the light application time 2h under 35W xenon lamps;Sampled every 30min in degradation process, detect first
The change in concentration of base orange.
3. the TiO of Au Nanoparticle Modifieds according to claim 12The preparation method of nano wire photochemical catalyst, its feature exists
In:The titanium sheet is purity 99.8%.
4. the TiO of Au Nanoparticle Modifieds according to claim 12The preparation method of nano wire photochemical catalyst, its feature exists
In:The titanium sheet is length 10cm, the rectangle of width 1cm.
5. the TiO of Au Nanoparticle Modifieds according to claim 12The preparation method of nano wire photochemical catalyst, its feature exists
In:Pickle used is HF: HNO in the pickling3∶H2O is mixed according to 1~2: 4~5: 8~10 volume ratios.
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CN108479771B (en) * | 2016-05-16 | 2019-07-30 | 南通大学 | Au/TiO2The liquid-phase synthesis process of composite nanometer particle and hetero-junctions |
CN106622225A (en) * | 2016-12-29 | 2017-05-10 | 天津大学 | Photochemical preparation method of single atom Au for catalytic degradation of VOCs |
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CN108816253A (en) * | 2018-05-31 | 2018-11-16 | 宁夏大学 | A kind of Au/Bi24O31Br10Composite photo-catalyst and preparation method thereof |
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CN112044432B (en) * | 2020-09-07 | 2021-12-17 | 南京大学 | Rapid preparation method of titanium dioxide supported gold nanoparticles at normal temperature |
CN114749173A (en) * | 2022-04-24 | 2022-07-15 | 长春工业大学 | Ag-TiO2Composite photocatalytic material and preparation method thereof |
CN115814785B (en) * | 2022-11-18 | 2024-04-26 | 同济大学 | TiO (TiO) with visible light response nano Au modified crystal face heterojunction2Photoelectrode, construction and application thereof |
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