CN104492431A - Preparation method of Au-Pd/TiO2 NBs photocatalyst - Google Patents
Preparation method of Au-Pd/TiO2 NBs photocatalyst Download PDFInfo
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- CN104492431A CN104492431A CN201410750904.6A CN201410750904A CN104492431A CN 104492431 A CN104492431 A CN 104492431A CN 201410750904 A CN201410750904 A CN 201410750904A CN 104492431 A CN104492431 A CN 104492431A
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Abstract
The invention discloses a preparation method of an Au-Pd/TiO2 NBs photocatalyst, which comprises the following steps: with a titanium sheet as a matrix, performing anodic oxidation treatment on the titanium sheet to prepare TiO2NBs; before anodic oxidation, performing ultrasonic cleaning of the titanium sheet in ethanol and acetone respectively, performing acid pickling, washing with deionized water and drying, wherein a two-electrode system is adopted for the anodic oxidation; calcining in air; modifying the TiO2NBs prepared in the step I with Au-Pd bimetallic nanoparticles; adopting a three-electrode system in which chloroauric acid and a palladium chloride aqueous solution are used as Au and Pd sources; and depositing Au and Pd in turn and drying. The photocatalyst prepared by the method disclosed by the invention is fixed on the titanium matrix, the water body pollution caused by non-thorough recovery is avoided, a contactable surface area is larger, the contact reaction between organic pollutant molecules and the photocatalyst is facilitated, the photocatalytic degradation property of the photocatalyst is remarkably promoted, reaction conditions are mild, and the process flow is simple and easy to control.
Description
Technical field
The present invention relates to a kind of preparation method of photochemical catalyst, particularly relate to a kind of Au-Pd/TiO
2the preparation method of NBs photochemical catalyst.
Background technology
TiO
2photochemical catalyst is stablized, is had no side effect and the feature such as with low cost due to its high photocatalytic activity, physicochemical properties, is considered to remove the most promising material of Organic Pollution in water body and air in environment.Research shows, TiO
2photochemical catalyst can be degraded most organic matter, and such as aromatic hydrocarbon, halogenated hydrocarbon, nitrogen-containing heterocycle compound etc., therefore, utilize TiO
2photocatalytic oxidation degraded water body and air in organic pollution become one of focus of domestic and international photocatalysis research field.But TiO
2the practical application of photochemical catalyst still has many obstacles, therefore, the photochemical catalyst preparing a kind of highly effective be a kind of in the urgent need to.
TiO
2the geometrical morphology of photochemical catalyst plays vital effect to its photocatalysis performance, and the photochemical catalyst with perfect pattern can increase can contact surface area, improves the accessibility to object, and then improves the degradation efficiency to pollutant.Anatase TiO
2the energy gap of photochemical catalyst is 3.2ev, the ultraviolet portion that sunshine medium wavelength is less than 387.5nm can only be absorbed, and ultraviolet portion only accounts for about 4% of whole solar spectral, therefore develop the important directions that visible light-responded photochemical catalyst is photocatalysis field.In addition, previous most of TiO
2photochemical catalyst is all the form adopting powder, there is catalyst and is difficult to reclaim the problem that nanometer even can be caused to pollute.
Summary of the invention
The object of the invention is to solve deficiency of the prior art, a kind of Au-Pd/TiO is provided
2nBs (the TiO that Au-Pd bimetal nano particles is modified
2nanobelt) preparation method of photochemical catalyst, adopt Au-Pd/TiO prepared by the method
2nBs photochemical catalyst have larger can contact surface sum visible light activity, and overcome the defect being unfavorable for being separated from water, Au-Pd bimetal nano particles is evenly distributed, and particle diameter is little.
To achieve these goals, the technical solution of employing is in the present invention: a kind of Au-Pd/TiO
2the preparation method of NBs photochemical catalyst, step is as follows:
One, TiO
2prepared by NBs: using titanium sheet as matrix, carry out anodized prepare TiO to titanium sheet
2nBs, electrolyte is that ethylene glycol adds water 18 ~ 20: 1 (v/v), and ammonium fluoride content is 0.4 ~ 0.6wt%, and applied voltage is 55 ~ 65V, oxidization time is 2.5 ~ 3.5h, before anodic oxidation, titanium sheet is ultrasonic cleaning 8 ~ 12min in ethanol and acetone respectively, then pickling 28 ~ 35s, then use deionized water rinsing, and in 100 ~ 110 DEG C of air dryings, anodic oxidation adopts two electrode systems, 540 ~ 555 DEG C of calcining 1.5 ~ 3h in atmosphere;
Two, Au-Pd bimetal nano particles is modified: the TiO prepared step one
2nBs carries out the modification of Au-Pd bimetal nano particles, adopts three-electrode system, TiO
2nBs is negative electrode, and platinized platinum is anode, and SCE electrode is reference electrode, the gold chloride of 0.1mM and palladium chloride aqueous solution are Au and Pd source, and deposition potential is-0.2 ~-0.15V, and sedimentation time is 5 ~ 10s, deposit Pd after first depositing Au, dry in 100 ~ 110 DEG C of baking ovens after deposition.
Further, the Au-Pd/TiO obtained in described step 2
2nBs photochemical catalyst, its performance is evaluated by photocatalytic degradation rhodamine B, rhodamine B solution concentration is 5mg/L, degradation time is 2h, adopt 35W xenon lamp simulating nature light, light source and catalyst distance are 3cm, get a sample, measure the change of its absorbance with T6 spectrophotometric in degradation process every 30min.
Further, described titanium sheet is of a size of 9mm × 40mm × 0.5mm.
Further, in described pickling, pickle used is HF: HNO
3: H
2o mixes according to 1 ~ 2: 4 ~ 5: 5 ~ 6 volume ratios.
The invention has the beneficial effects as follows: the Au-Pd/TiO of preparation
2nBs photochemical catalyst is fixed on Ti matrix, the defect be not easily separated from water after overcoming Powdered photocatalyst applications, is conducive to the recycling of catalyst, and avoids because reclaiming the not thoroughly water pollution caused.Experiment proves, with TiO
2nanotube is compared, and is fixed on the TiO on matrix
2nBs have larger can contact surface area, be convenient to organic pollutant molecule haptoreaction with it.After adopting Au-Pd bimetal nano particles to modify, reduce Charger transfer electromotive force, facilitate the fast transfer of light induced electron, improve effective separation of photo-generate electron-hole, in addition, Au-Pd bimetal nano particles can also improve TiO
2nBs, to the absorption of visible ray, improves the utilization rate of light, therefore, facilitates TiO greatly
2the Photocatalytic Degradation Property of NBs.This preparation method's reaction condition is gentle, and technological process is simple, and reaction is easy to control.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further elaborated.
Fig. 1 is Au-Pd/TiO prepared by embodiment 1
2the stereoscan photograph of NBs.
Fig. 2 is Au-Pd/TiO prepared by embodiment 1
2the transmission electron microscope photo of NBs.
Fig. 3 is Au-Pd/TiO prepared by embodiment 1
2the EDX spectrogram of NBs
Fig. 4 is Au-Pd/TiO prepared by embodiment 1
2the clearance of NBs photocatalytic degradation 5mg/L rhodamine B solution and light application time graph of a relation, and with pure TiO
2nBs compares.
Detailed description of the invention
Embodiment 1
A kind of Au-Pd/TiO
2the preparation method of NBs photochemical catalyst, step is as follows:
One, TiO
2prepared by NBs: using titanium sheet as matrix, carry out anodized prepare TiO to titanium sheet
2nBs, electrolyte is that ethylene glycol adds water 19: 1 (v/v), and ammonium fluoride content is 0.5wt%, and applied voltage is 60V, oxidization time is 3h, before anodic oxidation, titanium sheet is ultrasonic cleaning 10min in ethanol and acetone respectively, then pickling 30s, then use deionized water rinsing, and in 100 DEG C of air dryings, anodic oxidation adopts two electrode systems, 540 DEG C of calcining 1h in atmosphere;
Two, Au-Pd bimetal nano particles is modified: the TiO prepared step one
2nBs carries out the modification of Au-Pd bimetal nano particles, adopts three-electrode system, TiO
2nBs is negative electrode, and platinized platinum is anode, and SCE electrode is reference electrode, the gold chloride of 0.1mM and palladium chloride aqueous solution are Au and Pd source, and deposition potential is-0.2V, Au sedimentation time is 10s, Pd sedimentation time is 5s, deposits Pd, dry after deposition in 100 DEG C of baking ovens after first depositing Au.
The Au-Pd/TiO obtained in described step 2
2nBs photochemical catalyst, its performance is evaluated by photocatalytic degradation rhodamine B, rhodamine B solution concentration is 5mg/L, degradation time is 2h, adopt 35W xenon lamp simulating nature light, light source and catalyst distance are 3cm, get a sample, measure the change of its absorbance with T6 spectrophotometric in degradation process every 30min.
In described pickling, pickle used is HF: HNO
3: H
2o mixes according to 1: 4: 5 volume ratio.
Embodiment 2
A kind of Au-Pd/TiO
2the preparation method of NBs photochemical catalyst, step is as follows:
One, TiO
2prepared by NBs: carry out anodized to the titanium sheet of 9mm × 40mm × 0.5mm and prepare TiO
2nBs, electrolyte is that ethylene glycol adds water (19: 1v/v), and ammonium fluoride content is 0.4wt%, and applied voltage is 60V, and oxidization time is 4h.Before anodic oxidation, titanium sheet is ultrasonic cleaning 10min in ethanol and acetone respectively, then pickling 30s (HF: HNO
3: H
2o=1: 4: 5), then deionized water rinsing is used, and in 105 DEG C of air dryings.Anodic oxidation adopts two electrode systems.Sample 550 DEG C of calcining 2h in atmosphere of preparation.
Two, Au-Pd bimetal nano particles is modified: to the TiO of preparation
2nBs carries out the modification of Au-Pd bimetal nano particles, adopts three-electrode system, TiO
2nBs is negative electrode, and platinized platinum is anode, and SCE electrode is reference electrode, the gold chloride of 0.1mM and palladium chloride aqueous solution are Au and Pd source, and deposition potential is-0.15V, Au sedimentation time is 10s, Pd sedimentation time is 5s, and deposit Pd after first depositing Au, post-depositional sample is dried in 105 DEG C of baking ovens.
The Au-Pd/TiO obtained in described step 2
2nBs photochemical catalyst, its performance is evaluated by photocatalytic degradation rhodamine B, rhodamine B solution concentration is 5mg/L, degradation time is 2h, adopt 35W xenon lamp simulating nature light, light source and catalyst distance are 3cm, get a sample, measure the change of its absorbance with T6 spectrophotometric in degradation process every 30min.
Utilize noble metal to TiO
2photochemical catalyst is modified, and can improve the utilization to visible region, improves photocatalysis efficiency.Compared to pure TiO
2photochemical catalyst, TiO
2hetero-junctions light abstraction width can be expanded to visible region and improve separation and the transmission of electric charge, therefore, it is possible to improve photocatalysis efficiency.At TiO
2area load noble metal can improve TiO from following two aspects
2photocatalysis performance.On the one hand, the noble metal of load can promote electron capture, strengthens the separation of electron hole pair, improves TiO
2quantum efficiency.On the other hand, the coherent resonance of the collective of the noble metal nano structure free electron caused by visible light exposure, i.e. surface plasma body resonant vibration (SPR), the local electric field around metallic can be strengthened, local electric field causes forming electron hole pair fast at the nearly surf zone of semiconductor with the interaction of contiguous semiconductor, expand the light abstraction width of wide band gap semiconducter, improve the utilization rate to visible ray, thus improve its photocatalytic degradation efficiency.
Light absorption affects TiO
2a key factor of properties of catalyst, the power of light absorption directly determines the generation of the photo-generated carrier causing contaminant degradation.Make Au nano particle can produce response to visible ray by the resonate localized surface plasmons resonance (SPR) that causes of surface electronic.The SPR of Au nano particle can strengthen the internal field of particle surface, and produce Raman scattering and the INFRARED ABSORPTION effect of surface enhanced, the strong local electric field that SPR produces can strengthen TiO
2the catalytic activity of photochemical catalyst.In addition, Au nano particle and TiO
2the compound that the hetero-junctions formed can suppress photo-generate electron-hole right, improves TiO
2photochemical catalyst quantum efficiency.
Pd load not only can promote TiO
2photocatalysis performance and enhancing O
2catching light induced electron, and the inactivation that greatly can also suppress photochemical catalyst.The TiO that Pd modifies
2photochemical catalyst has successfully been applied in gas-phase photocatalysis reaction and sewage disposal.As compared to monometallic Au with Pd, the composite table of two kinds of metals reveals obvious cooperative effect, and further can strengthen the catalytic activity of catalyst and selective.The special electronics that bimetal nano particles can have that monometallic do not have, optics, catalysis or photocatalysis performance.Analyzing reason is because the two load of Au-Pd facilitates effective separation and the H of photo-generated carrier
2o
2synthesis.If light induced electron is fixed on TiO
2the Au-Pd core-shell structure nanometer particle on surface is caught, and is limited in Au core, so due to the uneven distribution TiO of electronics
2photocatalytic activity will be enhanced.
Above-mentioned explanation is not limitation of the present invention, and the present invention is also not limited in above-mentioned citing, and the change that those skilled in the art make in essential scope of the present invention, remodeling, interpolation or replacement also should belong to protection scope of the present invention.
Claims (4)
1. an Au-Pd/TiO
2the preparation method of NBs photochemical catalyst, is characterized in that, step is as follows:
One, TiO
2prepared by NBs: using titanium sheet as matrix, carry out anodized prepare TiO to titanium sheet
2nBs, electrolyte is that ethylene glycol adds water 18 ~ 20: 1 (v/v), and ammonium fluoride content is 0.4 ~ 0.6wt%, and applied voltage is 55 ~ 65V, oxidization time is 2.5 ~ 3.5h, before anodic oxidation, titanium sheet is ultrasonic cleaning 8 ~ 12min in ethanol and acetone respectively, then pickling 28 ~ 35s, then use deionized water rinsing, and in 100 ~ 110 DEG C of air dryings, anodic oxidation adopts two electrode systems, 540 ~ 555 DEG C of calcining 1.5 ~ 3h in atmosphere;
Two, Au-Pd bimetal nano particles is modified: the TiO prepared step one
2nBs carries out the modification of Au-Pd bimetal nano particles, adopts three-electrode system, TiO
2nBs is negative electrode, and platinized platinum is anode, and SCE electrode is reference electrode, the gold chloride of 0.1mM and palladium chloride aqueous solution are Au and Pd source, and deposition potential is-0.2 ~-0.15V, and sedimentation time is 5 ~ 10s, deposit Pd after first depositing Au, dry in 100 ~ 110 DEG C of baking ovens after deposition.
2. Au-Pd/TiO according to claim 1
2the preparation method of NBs photochemical catalyst, is characterized in that: the Au-Pd/TiO obtained in described step 2
2nBs photochemical catalyst, its performance is evaluated by photocatalytic degradation rhodamine B, rhodamine B solution concentration is 5mg/L, degradation time is 2h, adopt 35W xenon lamp simulating nature light, light source and catalyst distance are 3cm, get a sample, measure the change of its absorbance with T6 spectrophotometric in degradation process every 30min.
3. Au-Pd/TiO according to claim 1
2the preparation method of NBs photochemical catalyst, is characterized in that: described titanium sheet is of a size of 9mm × 40mm × 0.5mm.
4. Au-Pd/TiO according to claim 1
2the preparation method of NBs photochemical catalyst, is characterized in that: in described pickling, pickle used is HF: HNO
3: H
2o mixes according to 1 ~ 2: 4 ~ 5: 5 ~ 6 volume ratios.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104815648A (en) * | 2015-04-23 | 2015-08-05 | 周小燕 | Platinum doped titanium dioxide film sol preparation method |
| CN106622318A (en) * | 2016-11-08 | 2017-05-10 | 河南理工大学 | Layered composite photocatalyst using bimetallic nanoparticles as heterojunctions and preparation method thereof |
| CN106622322A (en) * | 2016-11-08 | 2017-05-10 | 河南理工大学 | Two-dimensional nanosheet composite photocatalyst with bimetallic nanoparticles as heterojunction and preparation method thereof |
| CN109603820A (en) * | 2019-01-09 | 2019-04-12 | 天津大学 | The monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition |
| CN110228839A (en) * | 2019-06-21 | 2019-09-13 | 同济大学 | A kind of efficient Atrazine photoelectrocatalysis reduction minimizing technology |
| CN110270327A (en) * | 2018-09-28 | 2019-09-24 | 南昌航空大学 | A kind of catalyst and preparation method of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis |
-
2014
- 2014-12-10 CN CN201410750904.6A patent/CN104492431B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| QINGHUA CHEN ET AL.,: ""Coupling immobilized TiO2 nanobelts and Au nanoparticles for enhanced photocatalytic and photoelectrocatalytic activity and mechanism insights"", 《CHEMICAL ENGINEERING JOURNAL》 * |
| REN SU ET AL.,: ""Promotion of Phenol photodecomposition over TiO2 using Au, Pd, and Au-Pd nanoparticles"", 《ACSNANO》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104815648A (en) * | 2015-04-23 | 2015-08-05 | 周小燕 | Platinum doped titanium dioxide film sol preparation method |
| CN106622318A (en) * | 2016-11-08 | 2017-05-10 | 河南理工大学 | Layered composite photocatalyst using bimetallic nanoparticles as heterojunctions and preparation method thereof |
| CN106622322A (en) * | 2016-11-08 | 2017-05-10 | 河南理工大学 | Two-dimensional nanosheet composite photocatalyst with bimetallic nanoparticles as heterojunction and preparation method thereof |
| CN106622322B (en) * | 2016-11-08 | 2019-01-04 | 河南理工大学 | It is a kind of using bimetal nano particles as two-dimensional nano piece composite photo-catalyst of hetero-junctions and preparation method thereof |
| CN106622318B (en) * | 2016-11-08 | 2019-04-02 | 河南理工大学 | It is a kind of using bimetal nano particles as lamellar composite photochemical catalyst of hetero-junctions and preparation method thereof |
| CN110270327A (en) * | 2018-09-28 | 2019-09-24 | 南昌航空大学 | A kind of catalyst and preparation method of the quick dealuminated USY cataluyst Florfenicol of photoelectrocatalysis |
| CN109603820A (en) * | 2019-01-09 | 2019-04-12 | 天津大学 | The monatomic method for preparing catalyst of room temperature degradation of formaldehyde under a kind of Oxygen Condition |
| CN110228839A (en) * | 2019-06-21 | 2019-09-13 | 同济大学 | A kind of efficient Atrazine photoelectrocatalysis reduction minimizing technology |
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