CN114425330A - Double-noble-metal-loaded nano titanium dioxide and preparation method and application thereof - Google Patents
Double-noble-metal-loaded nano titanium dioxide and preparation method and application thereof Download PDFInfo
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 40
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 67
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 13
- 229910021650 platinized titanium dioxide Inorganic materials 0.000 claims abstract description 13
- 229910002696 Ag-Au Inorganic materials 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000002244 precipitate Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
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- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- 150000003839 salts Chemical class 0.000 claims description 10
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
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- 238000001354 calcination Methods 0.000 claims description 7
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- 229910002621 H2PtCl6 Inorganic materials 0.000 claims description 3
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
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- 239000000463 material Substances 0.000 abstract description 9
- 238000011068 loading method Methods 0.000 abstract description 8
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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Abstract
The invention discloses a preparation method and application of noble metal supported nano titanium dioxide, wherein the base material of the catalyst is nano TiO2And loading double noble metal particles Au-Pt, Ag-Pt and Ag-Au on the surface of the substrate material. Firstly, synthesizing nano TiO by thermal decomposition method2As a carrier, and then obtaining a product Au-Pt/TiO by a photoreduction supporting mode2、Ag‑Pt/TiO2And Ag-Au/TiO2. The preparation method is simple and feasible to operate, and the synthesized A-B/TiO2The (A, B ═ Au, Ag, Pt) nano-particles have strong photocatalytic activity andstability and excellent performance in the aspect of degrading formaldehyde by photocatalysis.
Description
Technical Field
The invention belongs to the technical field of new energy and photocatalytic materials, and particularly relates to double-noble-metal-loaded nano titanium dioxide and a preparation method and application thereof.
Background
The nano semiconductor photocatalysis technology is a new emerging technology for eliminating environmental pollutants, and draws more and more attention of people, and the nano semiconductor photocatalysis technology is a most effective method for eliminating indoor pollutants by photolysis of the pollutants fundamentally by utilizing the principle of photocatalysis. Among the numerous visible light responsive photocatalytic materials, TiO2It is widely used as the best catalyst for photocatalytic reaction, and has wide source, low cost, easy preparation, no toxicity, high photocatalytic activity and high stability. Under illumination conditions, TiO2Can convert pollutant formaldehyde into CO2And H2And O. But TiO 22The bulk still has the problems of slow photon-generated carrier migration rate and fast recombination rate, so that further modification is still needed, and one of the problems is to load a high-efficiency noble metal promoter. In recent years, people belong to TiO by loading single noble metal2The method achieves certain achievements in the aspect of formaldehyde degradation, but the loaded double noble metal cocatalyst is used for nano TiO2The effect of degradation has been rarely studied.
Disclosure of Invention
Aiming at the problems, the invention provides a double-noble-metal-loaded photocatalytic material A-B/TiO2(a, B ═ Au, Ag, Pt), which has excellent activity in photocatalytic degradation of formaldehyde.
The technical scheme of the invention is as follows:
a preparation method of double-noble-metal-loaded nano titanium dioxide comprises the following steps:
(1) firstly, the mixture of Ti (SO)4Dissolving in deionized water, uniformly stirring, carrying out vacuum filtration, taking a lower-layer clear solution, and then slowly dropwise adding ammonia water until the maximum precipitate is generated; respectively centrifugally washing the precipitate with high-purity water and ethanol until the supernatant is turbid, and finally calcining the obtained precipitate in a muffle furnace to obtain white nano TiO2Powder;
(2) adding TiO into the mixture2Dispersing the powder in the mixed solution of deionized water and methanol, performing ultrasonic treatment to completely disperse the powder, adding two noble metal salts, performing ultrasonic treatment, and respectively reducing the noble metal salts into noble metal nanoparticles under illumination and attaching the noble metal nanoparticles to TiO2And (3) obtaining the noble metal loaded nano titanium dioxide on the surface of the powder, washing the precipitate by using deionized water and ethanol, and drying the precipitate for later use.
Further, the Ti (SO)4And deionized water in a mass ratio of 5-20: 100, respectively;
further, in the step (1), the calcination temperature is 500-700 ℃; the calcination time is 1-4 h.
Further, the noble metal salt is HAuCl4·3H2O、H2PtCl6·6H2O and AgNO3Two kinds of (1).
Further, in the step (2), the volume ratio of the deionized water to the methanol is 4: 1;
further, after adding the noble metal salt, carrying out ultrasonic treatment for 10-30 min;
further, in the step (2), a noble metal salt and TiO2In an amount of 100mg TiO20.5-2mg of noble metal is loaded.
Further, in the step (2), the illumination condition is a 300W xenon lamp equipped with an AM1.5G filter.
The double-noble-metal-loaded nano titanium dioxide prepared by the preparation method comprises Au-Pt/TiO2、Ag-Pt/TiO2And/or Ag-Au/TiO2。
The noble metal loaded nano titanium dioxide is mainly applied to photocatalytic degradation of formaldehyde.
The invention has the following beneficial effects:
1. the single noble metal is loaded in the prior art and belongs to TiO2In the invention, the prepared Au-Pt/TiO2、Ag-Pt/TiO2And Ag-Au/TiO2The photocatalytic material shows excellent activity of degrading formaldehyde by photocatalysis, and the formaldehyde degrading speed can reach 3.28 g, 2.5 g and 2.66g respectively-1min-1. Experimental research shows that Au-Pt/TiO2、Ag-Pt/TiO2And Ag-Au/TiO2The photocatalyst shows good photocatalytic performance and can reach higher degradation amount under the irradiation of visible light. The formaldehyde photocatalytic explanation efficiency is TiO28.6, 6.6 and 7.0 times of the monomer.
2. The preparation and synthesis method of the photocatalytic material has simple conditions and higher commercial application prospect. Prepared by the method of the invention, TiO is loaded with double noble metals2The size of the noble metal is not changed too much, and the noble metal is loaded on TiO by small particles of 2-4nm2The obtained double noble metal loaded nano titanium dioxide has good dispersity, small size and uniformity.
3. A-B/TiO prepared by photoreduction loading method2The (A, B ═ Au, Ag and Pt) photocatalyst is used for degrading formaldehyde in a photocatalytic manner, and the catalyst has good photocatalytic stability through a cycle experiment. The three noble double metals can be used as good promoters for photocatalytic degradation of formaldehyde.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure, illustrate embodiments of the disclosure and together with the description serve to explain the disclosure and are not to limit the disclosure.
Embodiments of the present disclosure are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is an X-ray powder diffraction pattern of a sample and a standard card made according to the present invention;
FIG. 2 is a light absorption spectrum of a sample prepared according to the present invention;
FIG. 3 shows HRTEM (high resolution transmission electron microscope) spectra and EDS (X-ray energy spectra) of samples prepared according to the present invention;
FIG. 4 shows a sample and TiO prepared according to the present invention2The monomer is used for photocatalytic degradation of formaldehyde activity comparison curve chart;
FIG. 5 shows a sample prepared according to the present invention and TiO2The monomer is used for photocatalytic degradation of formaldehyde activity and is compared with a histogram;
FIG. 6 shows a sample prepared according to the present invention and TiO2The monomer is used for photocatalytic degradation of formaldehyde stability comparison chart.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention is further illustrated by the following description in conjunction with the figures and the examples.
The invention relates to TiO loaded by noble double metal A-B (A, B ═ Au, Ag, Pt)2The composite photocatalytic material has A-B (Au, Ag or Pt) supported by photoreduction to obtain A-B/TiO2The (A, B ═ Au, Ag and Pt) composite photocatalyst has the advantages of small particle size (5-10nm), uniform dispersion, excellent performance, good chemical stability and the like.
Example 1:
(1) firstly, adopting thermal decomposition method to prepare nano TiO2：
First, 100ml of water is measured in a measuring cylinder and poured into a 150ml beaker, 11.5200g of Ti (SO) are weighed4And (3) putting the mixture into the beaker filled with water, stirring the mixture into a uniform aqueous solution, carrying out suction filtration under reduced pressure to obtain a lower-layer clear solution, and then slowly dripping ammonia water at the speed of 20d/min until the maximum precipitate is generated. Centrifuging with high-purity water and ethanol, washing the precipitate for 3-4 times until the upper layer solution is clear, calcining the precipitate in a muffle furnace at 600 deg.C for 3h (heating rate of 5 deg.C/min) to obtain white nanometer TiO2And (3) powder.
(2) Secondly, preparing the nanometer TiO loaded by the double noble metals2Photocatalyst:
Au-Pt/TiO2is prepared by photoreduction supporting. 40ml of deionized water and 10ml of methanol are weighed, poured into a beaker, and 100mg of TiO is added2Dispersing the powder in the solution by ultrasonic treatment, adding 2.0mg HAuCl under stirring4·3H2O and 2.7mgH2PtCl6·6H2And O, performing ultrasonic treatment for 20min, and stirring for 15min under the illumination of a 300W xenon lamp with an AM1.5G optical filter. And after stirring, centrifugally washing the precipitate by using deionized water and ethanol, and drying the precipitate for later use.
Ag-Pt/TiO2And Ag-Au/TiO2All prepared by the same photoreduction load, except that the metal precursor is changed into AgNO3And H2PtCl6·6H2O、AgNO3And HAuCl4·3H2O。
The photocatalytic activity test method for the prepared material in example 1 is as follows:
the photocatalytic degradation of formaldehyde test was carried out in a formaldehyde detection reactor (volume: 250ml) system (atmospheric pressure) closed with circulating cooling water (25 ℃). The light source for top irradiation is 300W xenon lamp equipped with AM1.5G filter, and the relative concentration (C/C) of formaldehyde in the system is used0) The photocatalytic activity of the samples was evaluated. 50mg of the sample was weighed, dispersed in a petri dish and placed on a reactor fixed bed. Before the photocatalytic reaction test, air in the reactor is removed by argon gas, 50 microliters of formaldehyde solution is dripped into the reactor, the reactor is sealed, the infrared photo-generated chromatograph is preheated, the temperature is stabilized at 50 +/-0.1 ℃ for about 4 hours, the formaldehyde solution is completely volatilized, and at the moment, the concentration of the formaldehyde gas in the reactor reaches a peak value. And (3) after the light is turned on, an automatic sampling switch of the instrument is turned on, the instrument automatically samples every 3 parts for 28 seconds to analyze the concentration of formaldehyde, and the testing instrument is an infrared photo-chromatograph. The stability of the prepared photocatalyst is carried out by a cycle test, and the specific method comprises the following steps: after degradation, argon is used again to exhaust the gas in the reactor, formaldehyde solution is dripped in the reactor, the reactor is sealed, and the formaldehyde solution is volatilized at the same temperatureAnd then the sample is illuminated again for testing. This cycle test was performed four times in total.
FIG. 1 shows TiO before and after loading obtained in example2X-ray diffraction pattern of (D) TiO synthesized, as can be seen from FIG. 12Is anatase pure phase, does not have peaks of other phases, and is loaded to obtain A-B/TiO2The (a, B ═ Au, Ag, Pt) product did not show a diffraction peak of a — B (a, B ═ Au, Ag, Pt) clearly, which may be caused by too small a loading amount and good dispersion of particles, and no hetero-peak of other substances was introduced.
FIG. 2 shows the UV-visible diffuse reflection absorption spectrum of the photocatalyst prepared in the example, from FIG. 2, pure TiO2Has an absorption edge at 387nm in the visible region, and a corresponding band gap of 3.2 eV. In TiO2After the noble double metals Au, Ag and Pt are loaded, the absorption of the catalyst at visible light can be obviously enhanced due to the specific plasma resonance effect of Au, Ag and Pt, and the promotion of light absorption is generally accompanied with the improvement of photocatalytic performance.
FIG. 3 shows the product A-B/TiO obtained in the example2HRTEM and EDS images of (A, B ═ Au, Ag, Pt), and the obtained TiO was found from HRTEM2TiO after loading double noble metal with the size of about 5-10nm2The size of the noble metal is not changed too much, and the noble metal is loaded on TiO by small particles of 2-4nm2Of (2) is provided. The presence of Ti, O, Ag, Au and Pt elements can be seen from the EDS diagram, which indicates that Ag, Au and Pt are loaded on TiO2Of (2) is provided.
FIGS. 4 and 5 show examples of A-B/TiO compounds prepared by a method of photoreduction supporting2Curves of (a, B ═ Au, Ag, Pt) photocatalyst for photocatalytic degradation of formaldehyde, as can be seen from fig. 4 and 5, TiO was observed under visible light2The average formaldehyde degradation rate per minute of the monomer was 0.38g-1And Au-Pt/TiO2、Ag-Pt/TiO2And Ag-Au/TiO2The average formaldehyde degrading rate of the photocatalyst is 3.28 g, 2.5 g and 2.66g per minute-1The activity of the photocatalyst after loading the double noble metal is obviously higher than that of TiO2The monomer is about 8.6 times, 6.6 times and 7.0 times of the monomer respectively.
FIG. 6 is a schematic diagram of an embodiment of a light passing filterA-B/TiO prepared by original loading method2Stability curves of (a, B ═ Au, Ag, Pt) photocatalysts for photocatalytic degradation of formaldehyde, as can be seen from fig. 6, a-B/TiO after four cycles2The activity of (a, B ═ Au, Ag, Pt) did not decay significantly after four cycles, indicating that the catalyst had good photocatalytic stability. These results all indicate that the three noble bimetallic metals can be used as good promoters for the photocatalytic degradation of formaldehyde.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the double-precious-metal-loaded nano titanium dioxide is characterized by comprising the following steps of:
(1) firstly, the ingredients are Ti (SO)4Dissolving in deionized water, uniformly stirring, carrying out vacuum filtration, taking a lower-layer clear solution, and then slowly dropwise adding ammonia water until the maximum precipitate is generated; respectively centrifugally washing the precipitate with high-purity water and ethanol until the supernatant is turbid, and finally calcining the obtained precipitate in a muffle furnace to obtain white nano TiO2Powder;
(2) mixing TiO with2Dispersing the powder in a mixed solution of deionized water and methanol, performing ultrasonic treatment to completely disperse the powder, adding two noble metal salts, performing ultrasonic treatment, respectively reducing the noble metal salts into noble metal nanoparticles under illumination, attaching the noble metal nanoparticles to the surface of TiO powder to obtain double noble metal-loaded nano titanium dioxide, washing the precipitate with deionized water and ethanol, and drying the precipitate for later use.
2. The method of claim 1, wherein the ti (so)4And deionized water in a mass ratio of 5-20: 100.
3. the method as claimed in claim 1, wherein the calcination temperature in step (1) is 500-700 ℃; the calcination time is 1-4 h.
4. The method according to claim 1, wherein the noble metal salt is HAuCl4·3H2O、H2PtCl6·6H2O and AgNO3Two kinds of (1).
5. The method according to claim 1, wherein in the step (2), the volume ratio of deionized water to methanol is 4: 1.
6. the method according to claim 1, wherein the ultrasonic treatment is carried out for 10 to 30min after the noble metal salt is added in the step (2).
7. The method according to claim 1, wherein in the step (2), the noble metal salt and TiO are added2In an amount of 100mg TiO20.5-2mg of noble metal is loaded.
8. The production method according to claim 1, wherein in the step (2), the illumination condition is a 300W xenon lamp equipped with an AM1.5G filter.
9. The double noble metal-loaded nano titanium dioxide prepared by the preparation method according to any one of the preceding claims, wherein the double noble metal-loaded nano titanium dioxide comprises Au-Pt/TiO2、Ag-Pt/TiO2And/or Ag-Au/TiO2。
10. The use of the noble metal-loaded nano-titania of claim 9 in the photocatalytic degradation of formaldehyde.
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| CN117299232B (en) * | 2023-09-26 | 2024-04-19 | 华北电力大学 | Method for synthesizing hydroxyaldehyde by catalyzing dihydric alcohol and preparing hydrogen by coupling |
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