CN115400766B - Pt 1 -CeO 2 /Co 3 O 4 Monoatomic catalyst and preparation method thereof - Google Patents
Pt 1 -CeO 2 /Co 3 O 4 Monoatomic catalyst and preparation method thereof Download PDFInfo
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- CN115400766B CN115400766B CN202211233149.5A CN202211233149A CN115400766B CN 115400766 B CN115400766 B CN 115400766B CN 202211233149 A CN202211233149 A CN 202211233149A CN 115400766 B CN115400766 B CN 115400766B
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
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Abstract
Pt 1 ‑CeO 2 /Co 3 O 4 Monoatomic catalyst and preparation method thereof. The preparation method comprises the following steps: with Co (CH) 3 COO) 2 ·4H 2 O、CeCl 3 ·7H 2 O、H 2 PtCl 6 ·6H 2 O、Na 2 CO 3 And ethylene glycol as raw materials to prepare monoatomic Pt 1 ‑CeO 2 /Co 3 O 4 Under the condition of introducing nitrogen in the whole process, co (CH) 3 COO) 2 ·4H 2 O、CeCl 3 ·7H 2 Mixing O with ethylene glycol to form a mixed salt solution; then will be mixed with H 2 PtCl 6 ·6H 2 Na of O 2 CO 3 The solution was added to the mixed salt solution and the reaction produced a precipitate. Finally, pyrolyzing the collected precipitate in air atmosphere, collecting the obtained powder to obtain target Pt 1 ‑CeO 2 /Co 3 O 4 Monoatomic catalysts. The invention adopts a one-step coprecipitation method to prepare the monoatomic Pt loadIn CeO 2 /Co 3 O 4 Pt on composite metal oxide support 1 ‑CeO 2 /Co 3 O 4 The monoatomic catalyst is used for obtaining the toluene degradation catalyst with excellent performance.
Description
Technical Field
The invention relates to monoatomic Pt for toluene degradation 1 -CeO 2 /Co 3 O 4 Composite metal oxide catalyst products.
Background
Volatile Organic Compounds (VOCs) are key intermediates for secondary organic aerosols and photochemical smog, which pose serious threats to the atmospheric environment and human health. The noble metal supported catalyst is considered as a promising method for removing VOC in industrial waste gas because of the advantages of high oxidation activity, low operating temperature, strong regeneration capability and the like. However, since noble metals are costly and scarce, it is necessary to further reduce the loading while improving the catalytic performance of noble metal-supported catalysts to achieve cost effectiveness and wider applicability.
Disclosure of Invention
The invention aims to provide a single-atom Pt-loaded Pt which can be used for degrading toluene 1 -CeO 2 /Co 3 O 4 The composite oxide catalyst can maximally improve the utilization rate of atoms and reduce the cost.
According to a first aspect of the present invention, there is provided a Pt 1 -CeO 2 /Co 3 O 4 A method for preparing a monoatomic catalyst comprising:
co (CH) 3 COO) 2 ·4H 2 O and CeCl 3 ·7H 2 O is dissolved in glycol to form a mixed salt solution, wherein Co (CH 3 COO) 2 ·4H 2 O and CeCl 3 ·7H 2 The mass ratio of O is 3:1-15:1;
providing a mixture of H 2 PtCl 6 ·6H 2 Na of O 2 CO 3 An aqueous solution;
will be mixed with H 2 PtCl 6 ·6H 2 Na of O 2 CO 3 Adding the aqueous solution into the mixed salt solution to form a reaction solution, so that the pH value of the reaction solution is 9-11;
heating the reaction solution to 140-180 ℃ under the protective atmosphere, and keeping the reaction time to 1-3 h;
calcining (pyrolyzing) the precipitate obtained by the reaction in air atmosphere to obtain Pt 1 -CeO 2 /Co 3 O 4 The single-atom catalyst has calcination temperature of 300-450 deg.c and calcination time of 3-5 hr, and the platinum load of the catalyst is 0.03-0.11 wt% (ICP measurement result).
The invention prepares the Pt with ultralow Pt load by a one-step coprecipitation method 1 -CeO 2 /Co 3 O 4 Monoatomic catalysts. This particular ternary structure allows monoatomic Pt and CeO 2 /Co 3 O 4 Enhanced strong metal-to-carrier interactions (SMSI) between carriers can induce more Pt 0 And Ce (Ce) 3+ For adsorption and activation of oxygen, more Co 3+ For the activation of toluene. Furthermore, ceO 2 The oxygen vacancies of the surface can induce the generation of a number of active oxygen species, which can migrate efficiently to the active sites (Pt 1 -Co 3 O 4 To) replace surface-consumed oxygen, thereby improving the stability of the catalyst.
According to the preparation method of the invention, the mass ratio of Co salt to Ce salt in the mixed salt solution is preferably 13:1. The amount of ethylene glycol used as the solvent is not limited as long as it can ensure uniform mixing of the metal salts in the solution.
According to the preparation method of the present invention, the temperature of the mixed salt solution is preferably about 50 ℃. The mixed salt solution is preferably formed under a nitrogen atmosphere.
According to the preparation method of the present invention, the pH of the reaction solution is preferably 10. By adjusting Na 2 CO 3 The pH value of the reaction solution can be controlled.
According to the preparation method of the present invention, the reaction temperature of the reaction solution is preferably 160℃and the reaction time is preferably 2 hours. In addition, nitrogen atmosphere is preferably used in the reaction.
According to the preparation method of the invention, the calcination temperature is preferably 350 ℃; the calcination time is preferably kept at 4 hours.
According to the inventionThe noble metal (platinum) loading of the resulting catalyst was preferably 0.06wt% (ICP measurement). By adjusting Na 2 CO 3 H mixed in aqueous solution 2 PtCl 6 ·6H 2 The amount of O can realize the control of the platinum loading.
The monoatomic catalyst prepared by the method is uniform in distribution, low in load capacity, simple in operation and easy to prepare.
According to another aspect of the present invention there is also provided a catalyst product prepared according to the above process.
The catalyst product is particularly suitable for being used as a toluene degradation catalyst for catalytic oxidation of toluene.
The special ternary structure of the invention ensures that single-atom Pt and CeO 2 /Co 3 O 4 Enhanced strong metal-to-carrier interactions (SMSI) between carriers can induce more Pt 0 And Ce (Ce) 3+ For adsorption and activation of oxygen, more Co 3+ For the activation of toluene. Furthermore, ceO 2 The oxygen vacancies of the surface can induce the generation of a number of active oxygen species, which can migrate efficiently to the active sites (Pt 1 -Co 3 O 4 And (3) the surface-consumed oxygen is replaced, thereby improving the stability of the catalyst and the toluene degradation activity.
As described above, the catalyst product of the invention is prepared by adopting a one-step coprecipitation method, and has the advantages of simple process, mild condition, rapid deposition, good controllability of product morphology and size, good dispersity of monoatomic Pt, and good dispersity of Pt and CeO 2 /Co 3 O 4 The carriers can have strong interaction, have good repeatability and low price, and are particularly suitable for catalyzing and oxidizing toluene.
Drawings
FIG. 1 is a Pt loading of 0.06wt% Pt 1 -CeO 2 /Co 3 O 4 XRD pattern of the monoatomic catalyst;
FIG. 2 is 0.06Pt 1 -CeO 2 /Co 3 O 4 High angle annular dark field scanning transmission electron microscope (HAADF-STEM) images of the monoatomic catalyst; and
FIG. 3 is a schematic view ofPt supported at 0.06wt% Pt 1 -CeO 2 /Co 3 O 4 Toluene conversion and CO over monoatomic catalyst 2 Mineralization rate plot.
Detailed Description
The invention is further described below in connection with examples and figures, which should be understood by those skilled in the art that the examples and figures are for the purpose of better understanding of the invention and are not intended to be limiting in any way.
1 2 3 4 One-step coprecipitation method for preparing single-atom Pt-supported Pt-CeO/CoO catalyst for catalytic oxidation of toluene
(1) 2.865g of Co (CH) was charged into a three-necked flask under a nitrogen atmosphere 3 COO) 2 ·4H 2 O、0.222g CeCl 3 ·7H 2 O and 30mL of ethylene glycol were stirred at 50deg.C for 10min to form a mixed salt solution.
(2) Will be mixed with 265uL H 2 PtCl 6 ·6H 2 Na of O 2 CO 3 Aqueous solution (Na) 2 CO 3 1 mol/L) was added dropwise to the above mixed salt solution to form a reaction solution having a pH of 10.
(3) The reaction temperature was raised to 160℃and stirring was continued for 2h at constant temperature under nitrogen atmosphere.
(4) Washing the obtained precipitate with water for 3 times, washing with alcohol for 3 times, and oven drying at 60deg.C in vacuum oven overnight.
(5) Placing the dried powder in a muffle furnace, and calcining at 350 ℃ for 4 hours to obtain Pt 1 -CeO 2 /Co 3 O 4 A catalyst in which the loading of noble metal was 0.06wt% (ICP measurement).
1 2 3 4 XRD pattern analysis of Pt-CeO/CoO monoatomic catalyst
FIG. 1 is a Pt loading of 0.06wt% Pt 1 -CeO 2 /Co 3 O 4 XRD pattern of the monoatomic catalyst. As can be seen from FIG. 1, the samples had significant diffraction peaks at 19.0 °, 31.3 °, 36.9 °, 44.8 °, 59.4 ° and 65.2 °, which are comparable to spinel Co 3 O 4 (JCPDS No. 42-1467) are related to the (111), (220), (311), (400), (511) and (440) crystal planes. Weak peaks at 28.6 °, 33.1 °, 47.5 ° and 56.3 °, respectively, correspond to CeO 2 The (111), (200), (220) and (311) crystal planes of fluorite structure (JCPDS No. 34-0349). No diffraction peak corresponding to Pt or PtOx was observed in XRD, which means Pt at 10Ce-Co 3 O 4 The carrier is highly dispersed and/or has a low loading content.
1 2 3 4 HAADF-STEM image analysis of Pt-CeO/CoO monoatomic catalyst
FIG. 2 is 0.06Pt 1 -CeO 2 /Co 3 O 4 HAADF-STEM image of monoatomic catalyst; to understand that Pt is 0.06Pt 1 -CeO 2 /Co 3 O 4 The dispersion on the catalyst was tested using a high angle annular dark field scanning transmission electron microscope (HAADF-STEM). Can clearly observe that a large number of bright spots (red circles) are dispersed in CeO 2 /Co 3 O 4 On the support, it was shown that Pt was atomically dispersed on the catalyst surface.
1 2 3 4 Toluene catalytic combustion performance test of Pt-CeO/CoO monoatomic catalyst
0.1g Pt was used 1 -CeO 2 /Co 3 O 4 The catalyst was mixed with 0.3g of quartz sand and the toluene catalytic combustion test was performed in a continuous flow fixed bed quartz microreactor (i.e., =6 mm). As shown in FIG. 3, the catalyst reached a 90% conversion at a temperature of 169℃at 1000ppm and 20,000mL/g h test conditions (T) 90 )，CO 2 The mineralization rate is 171 ℃, which is superior to a plurality of single-atom catalysts and nanoparticle composite catalysts reported at present. The reasons may be: 1. the special ternary structure enables monoatomic Pt and CeO 2 /Co 3 O 4 Enhanced strong metal-to-carrier interactions (SMSI) between carriers can induce more Pt 0 And Ce (Ce) 3+ For adsorption and activation of oxygen, more Co 3+ For activation of toluene; 2. CeO (CeO) 2 Oxygen vacancies at the surface can induce the formation of a number of reactive oxygen speciesActive oxygen can migrate to active sites (Pt 1 -Co 3 O 4 And (3) the surface-consumed oxygen is replaced, thereby improving the stability of the catalyst and the toluene degradation activity.
Claims (6)
1. Pt (platinum) 1 -CeO 2 /Co 3 O 4 A method for preparing a monoatomic catalyst comprising:
co (CH) 3 COO) 2 ·4H 2 O and CeCl 3 ·7H 2 O is dissolved in glycol to form a mixed salt solution, wherein Co (CH 3 COO) 2 ·4H 2 O and CeCl 3 ·7H 2 The mass ratio of O is 3:1-15:1;
providing a mixture of H 2 PtCl 6 ·6H 2 Na of O 2 CO 3 An aqueous solution;
will be mixed with H 2 PtCl 6 ·6H 2 Na of O 2 CO 3 Adding the aqueous solution into the mixed salt solution to form a reaction solution, so that the pH value of the reaction solution is 9-11;
heating the reaction solution to 140-180 ℃ in a protective atmosphere, and keeping the reaction time to be 1-3 h;
calcining the precipitate obtained by the reaction in the air atmosphere to obtain Pt 1 -CeO 2 /Co 3 O 4 The catalyst is a monoatomic catalyst, wherein the calcination temperature is 300-450 ℃, the calcination time is 3-5 h, and the platinum loading of the catalyst is 0.03-0.11 wt%.
2. The preparation method according to claim 1, wherein the protective atmosphere is nitrogen.
3. The preparation method according to claim 1, wherein the mixed salt solution is formed by stirring at 30-80 ℃ under the condition of a protective atmosphere.
4. The process according to claim 1, wherein H is incorporated 2 PtCl 6 ·6H 2 Na of O 2 CO 3 Is added dropwise to the mixed salt solution to form a reaction solution.
5. Pt (platinum) 1 -CeO 2 /Co 3 O 4 Monoatomic catalysts prepared by the process according to any of claims 1 to 4.
6. The catalyst according to claim 5 for the catalytic oxidation of toluene.
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| US11766663B2 (en) * | 2019-07-19 | 2023-09-26 | Arizona Board Of Regents On Behalf Of Arizona State University | Functional nanoscale metal oxides for stable metal single atom and cluster catalysts |
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