CN115770570A - Cerium oxide loaded atomic-scale dispersed Pt catalyst and redispersion preparation method thereof - Google Patents
Cerium oxide loaded atomic-scale dispersed Pt catalyst and redispersion preparation method thereof Download PDFInfo
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- CN115770570A CN115770570A CN202211466009.2A CN202211466009A CN115770570A CN 115770570 A CN115770570 A CN 115770570A CN 202211466009 A CN202211466009 A CN 202211466009A CN 115770570 A CN115770570 A CN 115770570A
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 77
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000003054 catalyst Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
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- 238000011068 loading method Methods 0.000 claims abstract description 20
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 104
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
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- 239000007788 liquid Substances 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 150000003057 platinum Chemical class 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
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- 229910052697 platinum Inorganic materials 0.000 claims description 3
- -1 platinum salt Chemical class 0.000 claims description 3
- KLFRPGNCEJNEKU-FDGPNNRMSA-L (z)-4-oxopent-2-en-2-olate;platinum(2+) Chemical compound [Pt+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O KLFRPGNCEJNEKU-FDGPNNRMSA-L 0.000 claims description 2
- CTUFHBVSYAEMLM-UHFFFAOYSA-N acetic acid;platinum Chemical compound [Pt].CC(O)=O.CC(O)=O CTUFHBVSYAEMLM-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 239000010413 mother solution Substances 0.000 claims description 2
- HNKLPNDFOVJIFG-UHFFFAOYSA-N oxalic acid;platinum Chemical compound [Pt].OC(=O)C(O)=O HNKLPNDFOVJIFG-UHFFFAOYSA-N 0.000 claims description 2
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 2
- NWAHZABTSDUXMJ-UHFFFAOYSA-N platinum(2+);dinitrate Chemical compound [Pt+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O NWAHZABTSDUXMJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 2
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- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 1
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- LVWZTYCIRDMTEY-UHFFFAOYSA-N metamizole Chemical compound O=C1C(N(CS(O)(=O)=O)C)=C(C)N(C)N1C1=CC=CC=C1 LVWZTYCIRDMTEY-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a cerium oxide loaded atomic-scale dispersed Pt catalyst and a redispersion preparation method thereof, belonging to the technical field of supported metal catalysts. The preparation method comprises the following steps: firstly, ceO is prepared 2 Loading Pt nano particle catalyst, high-temp calcining in oxidizing atmosphere to obtain Pt nano particles in CeO 2 (100) Redispersion occurs on crystal faces, and the dispersion degree of Pt is regulated and controlled by regulating the load of Pt to ensure that the Pt achieves atomic-level dispersion, thus obtaining the CeO 2 And carrying the atomically dispersed Pt catalyst. The control of the grain diameter from single atom, multiple atoms to cluster can be realized through the regulation and control of Pt loading capacity, and the distance between the single atoms in CeO can be realized 2 And controlling the distribution of the surface. On one hand, the method provides a basis for the precise regulation and control of the structure and the controllable preparation of the atomic-level dispersed Pt catalyst, can realize the application to various catalytic systems, and on the other hand, provides a solution for the regeneration of the sintered catalyst.
Description
Technical Field
The invention relates to the technical field of supported metal catalysts, in particular to a cerium oxide supported atomic-scale dispersed Pt catalyst and a redispersion preparation method thereof.
Background
Cerium oxide is one of the most important rare earth compounds, and is also known for its unique oxidationThe original characteristics, thermal stability, abundant oxygen vacancies and high oxygen storage capacity are widely applied in various catalytic fields. Platinum-based catalysts have a high capacity to activate C-H and C-O bonds and high chemical and hydrothermal stability, while having low tolerance to poisoning by certain elements (e.g., chlorine). The two are often combined to prepare a high-activity supported metal catalyst applied to environmental catalysis science and technology, and relate to oxidation processes (CO oxidation, VOCs emission reduction, smoke oxidation, automobile exhaust combustion and the like), nitro-aromatic reduction, CO 2 Using (alkane dry reforming, CO) 2 Reduction, etc.) and photocatalytic reactions. High temperatures in catalytic reactions tend to cause sintering of the metal, while the size effect of the catalyst active component particles has a great influence on the catalytic reaction. Therefore, the preparation of the stable and efficient atomic-level dispersed catalyst with high atom utilization rate has important research value. The theoretical limit size of the active components of the catalyst is single atom, the single-atom catalyst has the characteristics of uniform active sites of a homogeneous catalyst and stable and easily-separated structure of a heterogeneous catalyst, the number of the active sites is maximized, and the highest metal atom utilization rate can be realized. However, the surface energy of the metal particles in the atomically dispersed catalyst increases with decreasing size, which results in the atomically dispersed catalyst being more prone to agglomerate into large metal particles during synthesis and application. Therefore, an efficient and stable atomic-scale dispersed metal catalyst needs to be synthesized by means of an effective strategy, and the existing preparation method generally has the problems of high cost, complex process and the like, so that the research and development of the preparation method of the atomic-scale catalyst, which is low in cost, simple, convenient, green, efficient, controllable in synthesis, has important significance.
Disclosure of Invention
The invention aims to provide a cerium oxide loaded atomic-scale dispersed Pt catalyst and a redispersion preparation method thereof, wherein pre-synthesized cerium oxide (CeO) 2 ) The Pt-carried nano-particle catalyst is roasted at high temperature in oxidizing atmosphere, and the Pt nano-particles are roasted in CeO 2 (100) Redispersion occurs on the crystal face, and the dispersion degree of Pt is regulated and controlled by regulating the load amount of Pt to ensure that the Pt is dispersed at the atomic level to obtain CeO 2 And carrying the atomically dispersed Pt catalyst. By Pt loadingThe regulation and control of the method can realize the control of the particle size from single atom, multiple atoms to cluster and the distance between the single atoms in CeO 2 And controlling the surface distribution. On one hand, the method provides a basis for accurate regulation and preparation of the atomic-level dispersed Pt catalyst, can be applied to various catalytic systems, and on the other hand, provides an idea for regeneration of a sintered catalyst.
The purpose of the invention is realized by the following technical scheme:
cerium oxide loaded atomic-level dispersed Pt catalyst is prepared by loading active component of metal Pt on cubic nanometer CeO 2 The active component of the metal Pt is dispersed in CeO atomically 2 (100) Crystal face; the loading amount of the metal Pt is 0.01-1.0 wt.%, and the loading amount of the metal Pt is preferably 0.05-0.8 wt.% of the carrier CeO 2 The exposed crystal plane is (100).
The redispersion method of the cerium oxide loaded atomic-scale dispersed Pt catalyst comprises the following steps: first of all, ceO is prepared 2 The Pt nanoparticle-loaded catalyst is characterized in that Pt nanoparticles are distributed in cubic nanometer CeO with exposed (100) crystal face 2 C, removing; then the Pt nano particles are roasted at high temperature in an oxidizing atmosphere to be processed in CeO 2 And carrying out redispersion on the surface to obtain the cerium oxide loaded atomic-level dispersed Pt catalyst.
The method comprises the following specific steps:
(1) Mixing cubic nanometer CeO 2 Dispersing in proper amount of solvent, ultrasonic stirring to disperse the solvent uniformly to obtain CeO 2 A dispersion liquid; then dropwise adding the Pt nano particle dispersion liquid or the platinum salt solution to the CeO under the stirring condition 2 In the dispersion liquid, ultrasonic stirring is carried out for 1 to 3 hours, and uniform mixing is ensured; filtering to remove solvent to obtain CeO 2 Pt-loaded nanoparticle composite material or CeO 2 Loading a platinum salt composite material;
(2) Putting the composite material obtained in the step (1) into an oven for drying treatment, wherein the drying temperature is 50-200 ℃, and the drying time is 1-24 hours;
(3) Carrying out low-temperature roasting treatment on the composite material treated in the step (2) in an oxidizing atmosphere to obtain a load typePt/CeO 2 Catalyst (CeO) 2 A supported Pt nanoparticle catalyst);
(4) Loading Pt/CeO obtained in the step (3) 2 The catalyst is roasted at high temperature in the oxidizing atmosphere and cooled to room temperature to obtain the redispersed supported Pt/CeO 2 The catalyst is the cerium oxide loaded atomic-scale dispersed Pt catalyst.
Regulating and controlling the content of Pt in the composite material obtained in the step (1) to regulate and control the redispersed supported Pt/CeO obtained in the step (4) 2 The Pt loading amount in the catalyst realizes the atomic-scale dispersion of Pt.
In the step (1), the solvent is water, ethanol or methanol; the size of the Pt nano particle is 1-100 nm; the platinum salt is selected from one or more of platinum acetylacetonate, chloroplatinic acid, platinum nitrate, platinum chloride, platinum acetate and platinum oxalate.
In the step (1), the Pt nanoparticles (or Pt in platinum salt) and the cubic nanometer CeO 2 The ratio of (c) is determined by the amount of load required.
In the step (3), the roasting treatment in the oxidizing atmosphere is carried out at the temperature of 200-500 ℃, the oxidizing atmosphere comprises oxygen and inert gas, and the treatment time is 1-24 hours, so as to obtain the supported Pt/CeO 2 A catalyst.
In the step (4), when the oxidizing atmosphere is subjected to high-temperature roasting treatment, the oxygen content in the oxidizing atmosphere is 0.1 to 100vol.%.
In the step (4), when the high-temperature roasting treatment is carried out in the oxidizing atmosphere, the treatment temperature is 501-1000 ℃, and the treatment time is 1-24 hours.
The invention has the following advantages:
1. the Pt nano particles are prepared into the atomic-scale dispersed catalyst by a redispersion method, so that the utilization efficiency of noble metal atoms is greatly improved.
2. Can realize Pt on CeO 2 The fine structure control of the surface from single atom, multiple atoms to cluster can be realized, and the distance between Pt single atoms in CeO can be realized 2 Control of the surface.
3. Compared with the conventional preparation method of the atomic-scale dispersed Pt catalyst, the redispersion method has the advantages of simplicity, convenience, controllable synthesis process, no pollution in the production process, low cost and the like, and has wide industrial application prospects.
Drawings
FIG. 1 shows cubic nano CeO 2 And Pt/CeO 2 Transmission Electron Microscopy (TEM) and high angle annular dark field-scanning transmission electron microscopy (HAADF-STEM) images of the catalyst, wherein: (a) Cubic nanometer CeO 2 TEM image, inserting image at upper right corner as CeO 2 The particle size distribution of the nanoparticles; (b) Pt/CeO 2 TEM image of the catalyst, and the insert image at the upper right corner is the particle size distribution of the Pt nanoparticles; (c) And (d) Pt/CeO with different magnification 2 HAADF-STEM diagram of monatomic catalyst.
FIG. 2 shows the Pt/CeO after redispersion at different loadings 2 TEM images of the catalyst; wherein: (a) And (d) is Pt/CeO 2 TEM images of the nanoparticle catalyst; (b) And (e) is Pt/CeO 2 A TEM image of the nanocluster catalyst; (c) And (f) is Pt/CeO 2 TEM image of monatomic catalyst.
Detailed Description
The invention utilizes a redispersion method to carry out atomic-level dispersion regulation and control on Pt nano particles, combines crystal face mediation, and prepares CeO by dipping and high-temperature roasting treatment in an oxidizing atmosphere 2 And carrying the atomically dispersed Pt catalyst. The method of the invention firstly obtains CeO 2 The Pt nanoparticle-loaded catalyst is characterized in that Pt nanoparticles are distributed in cubic nanometer CeO with exposed (100) crystal face 2 Then the Pt nano particles are roasted in CeO at high temperature in oxidizing atmosphere 2 The surface redispersion phenomenon occurs. Finally, the dispersion degree of Pt is regulated and controlled by regulating the load capacity of Pt to achieve atomic-level dispersion, and the CeO is obtained 2 And carrying the atomically dispersed Pt catalyst. The present invention will be further described with reference to the following examples and the accompanying drawings.
Example 1:
this example prepares CeO 2 The process of loading the atomic-scale dispersed Pt catalyst is as follows:
1. hydrothermal method for preparing cubic nano CeO 2 : 3.472 g of cerium nitrate hexahydrate (Ce (NO) 3 ) 3 ·6H 2 O) is dissolved in 40mL deionized water to obtain Ce (NO) 3 ) 3 ·6H 2 O solution, 48 g of NaOH is dissolved in 40ml of deionized water to obtain NaOH solution, and Ce (NO) is stirred 3 ) 3 ·6H 2 The O solution was added dropwise to the NaOH solution, and after stirring for 0.5 hour, the mixed solution was transferred to a 200 ml Teflon-lined stainless steel autoclave and hydrothermally treated at 155 ℃ for 24 hours. After cooling to room temperature, centrifuging, filtering, washing three times with deionized water, washing three times with ethanol, and drying in an oven at 80 ℃ overnight. Calcining the mixture for 2 hours at 400 ℃ in air to obtain cubic nano CeO 2 . The cubic nanometer CeO 2 The exposed surface is (100).
2. Preparing Pt nano particles: 10 ml of 3.0mMol/L chloroplatinic acid hexahydrate (H) 2 PtCl 6 ·6H 2 O) and 90 ml of a solution containing 66.5 mg of polyvinyl pyridone (PVP; mw = 55000) was mixed with an ethanol solution, and refluxed at 90 ℃ for 3 hours in a 100 ml flask to obtain a Pt nanoparticle mother liquor.
3. Impregnation and loading: 69.9 mg of cubic nanometer CeO 2 Dispersing in 30 ml of ethanol, ultrasonically stirring to uniformly disperse, then dropwise adding 3 ml of Pt nano particle mother liquor while stirring, ultrasonically stirring for 0.5 hour to ensure uniform mixing, then filtering to remove the solvent, washing with deionized water for three times, washing with absolute ethanol for three times, and finally drying in an oven at 80 ℃ overnight to obtain CeO 2 And (3) loading the Pt nano particle composite material.
4. Roasting the sample treated in the step 3 at low temperature in air atmosphere, heating to 400 ℃ at a heating rate of 10 ℃/min, carrying out constant temperature treatment for 2 hours, and cooling to room temperature to obtain the load type Pt/CeO 2 Catalyst, named 0.5Pt/CeO 2 -Cub-400。
5. The sample treated in the step 4 is further roasted at high temperature in the air atmosphere, the temperature is raised to 600 ℃ at the heating rate of 10 ℃/min and is treated at constant temperature for 2 hours, and the temperature is reduced to room temperature to obtain CeO 2 The loaded atomic-level dispersed Pt catalyst is named as 0.5Pt/CeO 2 -a Cub-600 catalyst.
CeO prepared in this example 2 Pt loading in a supported atomic-level dispersed Pt catalystAbout 0.5wt.%.
Comparative example 1:
the difference from the embodiment 1 is that: taking 57.9 mg of cubic nano CeO in step 3 2 5 ml of Pt nano particle mother liquor is added to prepare Pt/CeO with Pt loading of about 1.5 wt% 2 The nanocluster catalyst is named as 1.5Pt/CeO 2 -Cub-600。
Comparative example 2:
the difference from the embodiment 1 is that: in step 3, 37.8 mg of cubic nano CeO is taken 2 Adding 10 ml of Pt nano particle mother solution to prepare Pt/CeO with the Pt loading of about 3 wt% 2 The nano particle catalyst is named as 3Pt/CeO 2 -Cub-600。
0.5Pt/CeO prepared as described in example 1 above 2 High-angle annular dark-field scanning transmission electron microscopy images of the-Cub-600 catalyst are shown in FIG. 1, example 1 and comparative examples 1-2 for preparing Pt/CeO with different loading amounts 2 The transmission electron micrograph of the-Cub-600 catalyst is shown in FIG. 2.
The above description should not be taken as limiting the invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the invention should be included in the protection scope of the invention.
Claims (10)
1. A cerium oxide loaded atomic-level dispersed Pt catalyst is characterized in that: the catalyst is prepared by loading active components of metal Pt on cubic nanometer CeO 2 Formed on a carrier, and the active component of the metal Pt is dispersed in CeO at an atomic level 2 (100) On the crystal face; the loading amount of the metal Pt is 0.01-1.0 wt.%.
2. The cerium oxide supported atomically dispersed Pt catalyst of claim 1, wherein: the carrier CeO 2 The exposed crystal plane is (100).
3. The method for redispersing an atomically dispersed Pt catalyst supported on cerium oxide according to claim 1, wherein: the method firstly prepares CeO 2 Pt-nanoparticle-supported catalyst in which Pt nanoparticles are distributedCubic nanometer CeO exposed on (100) crystal face 2 C, removing; then the Pt nano particles are roasted at high temperature in the oxidizing atmosphere to be in CeO 2 Redispersion on occurs on the surface to obtain the CeO 2 And carrying the atomically dispersed Pt catalyst.
4. The method for preparing the cerium oxide supported atomic-scale dispersed Pt catalyst of claim 3, wherein: the method specifically comprises the following steps:
(1) Mixing cubic nanometer CeO 2 Dispersing in proper amount of solvent, ultrasonic stirring to disperse the solvent uniformly to obtain CeO 2 A dispersion liquid; then, the Pt nano particle mother solution or the platinum salt dispersion liquid is dropwise added to the CeO under the stirring condition 2 In the dispersion liquid, ultrasonic stirring is carried out for 1 to 3 hours, and uniform mixing is ensured; then filtering or rotary evaporating to remove solvent to obtain CeO 2 Pt-loaded nanoparticle composite material or CeO 2 Loading a platinum salt composite material;
(2) Putting the composite material obtained in the step (1) into an oven for drying treatment, wherein the drying temperature is 50-200 ℃, and the drying time is 1-24 hours;
(3) Carrying out low-temperature roasting treatment on the composite material treated in the step (2) in an oxidizing atmosphere to obtain the supported Pt/CeO 2 Catalyst (CeO) 2 A supported Pt nanoparticle catalyst);
(4) Loading Pt/CeO obtained in the step (3) 2 The catalyst is roasted at high temperature in the oxidizing atmosphere and cooled to room temperature to obtain the redispersed supported Pt/CeO 2 The catalyst is the cerium oxide loaded atomic-level dispersed Pt catalyst.
5. The redispersion preparation method of a cerium oxide-supported atomic-scale dispersed Pt catalyst according to claim 4, characterized in that: regulating and controlling the amount of Pt loaded in the composite material obtained in the step (1) to regulate and control the redispersed loaded Pt/CeO obtained in the step (4) 2 The dispersion degree of Pt in the catalyst realizes the atomic-level dispersion of Pt.
6. The redispersion preparation method of the cerium oxide supported atomic-scale dispersed Pt catalyst according to claim 4, characterized in that: in the step (1), the solvent is water, ethanol or methanol; the size of the Pt nano particle is 1-100 nm; the platinum salt is selected from one or more of platinum acetylacetonate, chloroplatinic acid, platinum nitrate, platinum chloride, platinum acetate and platinum oxalate.
7. The redispersion preparation method of the cerium oxide supported atomic-scale dispersed Pt catalyst according to claim 4, characterized in that: in the step (1), the Pt nano particles (or Pt in platinum salt) and cubic nano CeO 2 Is determined by the amount of load required.
8. The redispersion preparation method of a cerium oxide-supported atomic-scale dispersed Pt catalyst according to claim 4, characterized in that: in the step (3), during the roasting treatment in the oxidizing atmosphere, the treatment temperature is 200-500 ℃, the oxidizing atmosphere comprises oxygen and inert gas, and the treatment time is 1-24 hours, so that the supported catalyst is obtained.
9. The redispersion preparation method of the cerium oxide supported atomic-scale dispersed Pt catalyst according to claim 4, characterized in that: in the step (4), when the oxidizing atmosphere is subjected to high-temperature roasting treatment, the oxygen content in the oxidizing atmosphere is 0.1-100 vol.%.
10. The redispersion preparation method of the cerium oxide supported atomic-scale dispersed Pt catalyst according to claim 4, characterized in that: in the step (4), when the high-temperature roasting treatment is carried out in the oxidizing atmosphere, the treatment temperature is 501-1000 ℃, and the treatment time is 1-24 hours.
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| CN116651442A (en) * | 2023-06-15 | 2023-08-29 | 西北工业大学 | Surface-confined atomic-level dispersed Pt@SiO 2 -N catalyst, preparation method and application thereof |
| CN118231681A (en) * | 2024-05-24 | 2024-06-21 | 内蒙古科学技术研究院 | Preparation method and application of rare earth-based monoatomic catalyst |
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| CN109647399A (en) * | 2018-11-05 | 2019-04-19 | 天津大学 | The preparation method of the monatomic catalyst of room-temperature catalytic oxidation aromatics VOCs |
| CN112044434A (en) * | 2020-10-20 | 2020-12-08 | 北京单原子催化科技有限公司 | Single-atom noble metal/transition metal oxide composite material and preparation method and application thereof |
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| CN116651442A (en) * | 2023-06-15 | 2023-08-29 | 西北工业大学 | Surface-confined atomic-level dispersed Pt@SiO 2 -N catalyst, preparation method and application thereof |
| CN118231681A (en) * | 2024-05-24 | 2024-06-21 | 内蒙古科学技术研究院 | Preparation method and application of rare earth-based monoatomic catalyst |
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