CN114515573A - Alkali metal modified single-atom platinum-cerium catalyst and preparation method and application thereof - Google Patents
Alkali metal modified single-atom platinum-cerium catalyst and preparation method and application thereof Download PDFInfo
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- CN114515573A CN114515573A CN202210240542.0A CN202210240542A CN114515573A CN 114515573 A CN114515573 A CN 114515573A CN 202210240542 A CN202210240542 A CN 202210240542A CN 114515573 A CN114515573 A CN 114515573A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 76
- FFNYNHKYVBPMQP-UHFFFAOYSA-N cerium platinum Chemical compound [Ce].[Pt] FFNYNHKYVBPMQP-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052783 alkali metal Inorganic materials 0.000 title claims abstract description 43
- 150000001340 alkali metals Chemical class 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 13
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000011068 loading method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 14
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 12
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 229910001963 alkali metal nitrate Inorganic materials 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 7
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 235000010344 sodium nitrate Nutrition 0.000 claims description 3
- 239000004317 sodium nitrate Substances 0.000 claims description 3
- 230000010718 Oxidation Activity Effects 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000003379 elimination reaction Methods 0.000 abstract 1
- 238000003878 thermal aging Methods 0.000 abstract 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 12
- 239000011591 potassium Substances 0.000 description 12
- 230000003197 catalytic effect Effects 0.000 description 10
- 229910052700 potassium Inorganic materials 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 239000007789 gas Substances 0.000 description 7
- 229910001413 alkali metal ion Inorganic materials 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000969 carrier Substances 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000000192 extended X-ray absorption fine structure spectroscopy Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 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 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- -1 alkali metal modified platinum cerium oxide Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
-
- B01J35/23—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/088—Decomposition of a metal salt
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/50—Carbon oxides
- B01D2257/502—Carbon monoxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention discloses an alkali metal modified monatomic platinum cerium catalyst, and a preparation method and application thereof, and belongs to the technical field of motor vehicle exhaust catalysis. The catalyst takes cerium oxide as a carrier, and Pt and alkali metal are loaded on the surface of the cerium oxide, wherein the loading mass fraction of Pt is 1%, and the quantity loading ratio of the alkali metal to the substance of Pt is 1: 1-10: 1. The motor vehicle tail gas catalyst of the invention can show higher CO oxidation activity at lower temperature, broaden the active temperature window, has higher thermal aging resistance, and can be widely applied to the elimination reaction of CO in tail gas of gasoline vehicles and diesel vehicles.
Description
Technical Field
The invention belongs to the technical field of motor vehicle exhaust catalysis, and particularly relates to an alkali metal modified monatomic platinum cerium catalyst, and a preparation method and application thereof.
Background
With the increasing quantity of the current motor vehicles, the problem of pollution and emission of the tail gas of the motor vehicles is also increased. In order to reduce the emission concentration of pollutants in the tail gas, the tail gas catalyst arranged at the rear part of the automobile can catalyze and eliminate pollutants such as CO in the tail gas. Cerium oxide has excellent redox ability and electron transfer ability, and is a very important catalyst carrier component in the current exhaust gas catalyst. Platinum group noble metals, however, have excellent catalytic properties and are widely used as active components of catalysts in the current field of automotive catalysis.
The price of precious metals is high, which puts a great cost pressure on their industrial application. If the catalyst can be dispersed on the surface of cerium oxide in a highly dispersed form, the atom utilization rate can be greatly improved, thereby effectively reducing the industrial production cost of the catalyst. However, the monatomic platinum catalyst is not satisfactory in catalytic activity because of the strong interaction between metal carriers and the poisoning effect of CO and other substances. The traditional means for improving the activity of the catalyst comprise reducing atmosphere treatment, construction of carriers with different morphologies and other means, but the prepared catalyst has poor stability and cannot meet the requirement of long service life of industrial application. Therefore, a method is needed to ensure that the performance of the catalyst for catalytic oxidation of exhaust pollutants is improved while the monoatomic stable structure of the catalyst is maintained.
Disclosure of Invention
In view of the problems in the prior art, one technical problem to be solved by the present invention is to provide an alkali metal modified monatomic platinum cerium catalyst. Another technical problem to be solved by the present invention is to provide a method for preparing an alkali metal modified monatomic platinum cerium catalyst. The method utilizes alkali metal as a modification auxiliary agent to regulate and control the electronic structure and the geometric structure of platinum species on the surface, and simultaneously stabilizes the monoatomic structure of the platinum species; the catalyst is modified by alkali metal, so that the catalytic activity of the catalyst is effectively improved, and the catalyst shows very good thermal stability; the reaction raw materials are simple and easy to obtain, the preparation method is simple and convenient, and the promotion effect is obvious; the problem that the monatomic platinum-cerium catalyst is easy to inactivate in a high-temperature tail gas atmosphere is solved.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of a platinum cerium catalyst modified by alkali metal comprises the following steps:
1) the cerium nitrate was calcined at 300 ℃ for 3 hours so that the cerium nitrate could be completely decomposed. Fully grinding the cerium oxide obtained after the reaction into fine and uniform powder as a catalyst carrier; the particle size of the powder is 20-50 nm;
2) dissolving tetraammineplatinum nitrate and alkali metal nitrate in aqueous solution to respectively obtain aqueous solution of platinum and alkali metal; wherein the concentration of the aqueous solution of the tetraammineplatinum nitrate is 0.05mmol/mL, and the concentration of alkali metal ions in the aqueous solution of alkali metal is 0.15 mmol/mL;
3) loading tetraammineplatinum nitrate and alkali metal nitrate on the surface of cerium oxide by using an incipient wetness impregnation method; and drying the loaded powder at 60 ℃ for 12 hours, and then calcining the powder at 800 ℃ for 10 hours to obtain the alkali metal modified monatomic platinum-cerium catalyst.
According to the preparation method of the alkali metal modified monatomic platinum cerium catalyst, the alkali metal nitrate is any one of lithium nitrate, sodium nitrate or potassium nitrate.
According to the preparation method of the alkali metal modified monatomic platinum cerium catalyst, the mass fraction of platinum loaded on each gram of cerium oxide carrier is 1%.
According to the preparation method of the alkali metal modified monatomic platinum-cerium catalyst, the amount ratio of the supported alkali metal to the platinum substance is 1: 1-10: 1, and preferably 5: 1.
The alkali metal modified single-atom platinum cerium catalyst prepared by the method.
The alkali metal modified single-atom platinum-cerium catalyst can effectively catalyze CO oxidation and H2Application in reduction.
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) produced by the inventionCompared with the unmodified platinum cerium catalyst, the method for modifying the platinum cerium catalyst by using the alkali metal has excellent catalytic CO oxidation activity, and can completely convert CO into CO at lower temperature2. Compared with H2The modified platinum cerium catalyst has good thermal stability and good reaction stability, and after multiple reaction cycle tests, the activity of alkali metal on the platinum cerium catalyst is obviously improved, and the platinum cerium catalyst has good stability.
(2) The modification method adopted by the invention has the advantages of low cost of reaction raw materials, simple production process, environmental protection and large-scale production.
Drawings
FIG. 1 is a graph showing the results of CO oxidation activities of platinum cerium catalysts supporting different alkali metals;
FIG. 2 is a graph showing the results of CO oxidation activity of platinum cerium catalysts loaded with different amounts of potassium;
FIG. 3 is H of platinum cerium catalyst loaded with different contents of potassium2Temperature programmed reduction (H)2-TPR) results graph;
FIG. 4 shows an alkali metal supported platinum cerium catalyst and catalyst using H2A CO oxidation activity cycle result chart of the platinum cerium catalyst prepared by reduction;
fig. 5 is a graph of results of geometric characterization of the platinum cerium catalyst by EXAFS on surface Pt species before and after loading with alkali metal.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
A preparation method of a platinum cerium catalyst modified by alkali metal comprises the following steps:
1) roasting cerium nitrate at 300 ℃ for 3 hours to completely decompose the cerium nitrate, and fully grinding cerium oxide obtained after reaction into fine and uniform powder with the particle size of 20-50nm to be used as a catalyst carrier;
2) dissolving tetrammine platinum nitrate and alkali metal nitrate (lithium nitrate, sodium nitrate and potassium nitrate) in an aqueous solution to respectively obtain aqueous solutions of platinum and alkali metal, wherein the concentration of the aqueous solution of the tetrammine platinum nitrate is 0.05mmol/mL, and the concentration of alkali metal ions in the aqueous solution of the alkali metal is 0.15 mmol/mL;
3) Loading tetraammineplatinum nitrate and alkali metal nitrate on the surface of cerium oxide by using an incipient wetness impregnation method; drying the loaded powder at 60 ℃ for 12 hours, and then calcining the powder at 800 ℃ for 10 hours to obtain the alkali metal modified platinum cerium oxide catalyst, wherein the mass fraction of platinum loaded on the cerium oxide carrier per gram in the catalyst is 1%, and the mass concentration ratio of alkali metal ions to Pt substances is 3: 1.
The results of CO oxidation activity of the platinum cerium catalysts supporting different alkali metals are shown in fig. 1. For activity test, 10mg of sample was placed in a fixed bed at 1% CO + 1% O2+ 98% He atmosphere, 150,000h-1The activity test was performed at a gas hourly space velocity of (a). It can be found that the catalytic activity of the platinum cerium catalyst is obviously improved after the alkali metal is doped, and the sequence of the alkali metal for improving the catalytic activity is K>Na>Li。
Example 2
And (3) loading potassium with different contents on the surface of the catalyst by controlling the volume of the dropwise added potassium nitrate solution by adopting an initial wet impregnation method to prepare the platinum cerium catalyst loaded with potassium with different contents. Fig. 2 is a graph showing the results of CO oxidation activities of platinum cerium catalysts loaded with different amounts of potassium. It can be concluded from fig. 2 that the addition of potassium to the platinum-cerium catalyst can significantly improve the catalytic activity of the catalyst, and the improvement of the catalytic activity of the platinum-cerium catalyst is most significant when the amount ratio of the supported potassium to the platinum material reaches 5: 1.
Example 3
And (3) loading potassium with different contents on the surface of the catalyst by controlling the volume of the dropwise added potassium nitrate solution by adopting an initial wet impregnation method to prepare the platinum cerium catalyst loaded with potassium with different contents. FIG. 3 is H of platinum cerium catalyst loaded with different contents of potassium2Temperature programmed reduction (H)2TPR) results. H2Catalyst before TPR test at N2The treatment was carried out at 200 ℃ for 1 hour under an atmosphere. Then each catalyst was at 7% H2In an Ar atmosphere at 10 deg.CThe temperature rise rate/min increased from room temperature to 750 ℃ and the signal was detected and recorded by the TCD detector. From FIG. 3 it can be seen that the H of the catalyst increases with the potassium content of the support2The reduction peak temperature gradually decreases, i.e., the stronger its redox ability, the strongest the redox ability of the catalyst when the potassium to platinum ratio is 5: 1.
Example 4
Fig. 4 is a graph showing the cycle results of CO temperature-rising oxidation activity of the platinum cerium catalyst modified with an alkali metal and reduced with hydrogen. The alkali metal-modified catalyst shows stable and excellent catalytic activity in an activity cycle test after the reaction, while using H2After one cycle of the catalyst obtained by reduction, the activity is obviously reduced. This shows that the alkali metal modification method not only improves the reaction activity of the catalyst, but also has better reaction stability.
Example 5
Fig. 5 is an analysis of the surface geometry of surface Pt species by EXAFS characterization of the alkali metal-loaded and pre-loaded platinum cerium catalysts. The Pt on the surface of the platinum cerium catalyst has no obvious change before and after loading the alkali metal, and proves that the Pt is better loaded on CeO in the form of single atom2The surface, and the improvement of the reactivity comes from the action of alkali metal on the surface.
Claims (6)
1. A preparation method of an alkali metal modified monatomic platinum cerium catalyst is characterized by comprising the following steps:
1) roasting the cerium nitrate at 300 ℃ for 3 hours to enable the cerium nitrate to be completely decomposed; fully grinding the cerium oxide obtained after the reaction into fine and uniform powder as a catalyst carrier;
2) dissolving tetraammineplatinum nitrate and alkali metal nitrate in aqueous solution to respectively obtain aqueous solution of platinum and alkali metal;
3) loading tetraammineplatinum nitrate and alkali metal nitrate on the surface of cerium oxide by using an incipient wetness impregnation method; and drying and calcining the loaded powder to obtain the alkali metal modified monatomic platinum-cerium catalyst.
2. The method for preparing an alkali metal-modified monatomic platinum-cerium catalyst as claimed in claim 1, wherein the alkali metal nitrate is any one of lithium nitrate, sodium nitrate, or potassium nitrate.
3. The method for preparing an alkali metal-modified monatomic platinum-cerium catalyst as recited in claim 1, wherein the mass fraction of platinum supported per gram of the cerium oxide support is 1%.
4. The method for preparing the alkali metal modified monatomic platinum-cerium catalyst according to claim 1, characterized in that the amount ratio of the supported alkali metal and the platinum substance is 1:1 to 10: 1.
5. An alkali metal-modified monatomic platinum-cerium catalyst obtained by the method as recited in any one of claims 1 to 4.
6. The alkali metal modified single-atom platinum-cerium catalyst as claimed in claim 5 for efficiently catalyzing CO oxidation and H2Application in reduction.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114950412A (en) * | 2022-07-12 | 2022-08-30 | 清华大学 | Method for preparing monatomic and nanocluster cooperative supported catalyst through atom reconstruction |
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