CN116273007A - Pt NPs/Fe 2 O 3 Preparation method and application of hexagon catalyst - Google Patents
Pt NPs/Fe 2 O 3 Preparation method and application of hexagon catalyst Download PDFInfo
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- CN116273007A CN116273007A CN202310260430.6A CN202310260430A CN116273007A CN 116273007 A CN116273007 A CN 116273007A CN 202310260430 A CN202310260430 A CN 202310260430A CN 116273007 A CN116273007 A CN 116273007A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 10
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 10
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 6
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims abstract description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000013598 vector Substances 0.000 claims abstract description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 150000004687 hexahydrates Chemical class 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000007254 oxidation reaction Methods 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 239000012855 volatile organic compound Substances 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 6
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 description 8
- 229910000510 noble metal Inorganic materials 0.000 description 5
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/864—Removing carbon monoxide or hydrocarbons
-
- 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
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- 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
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Abstract
The invention discloses a Pt NPs/Fe 2 O 3 The preparation method and application of the hexagon catalyst comprise the following steps: (1) Ultrasonically dissolving ferric trichloride hexahydrate in absolute ethyl alcohol to prepare ferric trichloride solution, adding deionized water and anhydrous sodium acetate, and uniformly stirring to perform hydrothermal reaction; (2) Centrifuging and drying the material obtained in the step (1), and calcining in an air atmosphere to obtain Fe 2 O 3 hexagon vector; (3) Dissolving hexahydrated chloroplatinic acid in deionized water to obtain chloroplatinic acid solution, and addingInto the Fe 2 O 3 Stirring and dispersing the hexagon carrier, adding sodium borohydride solution, and stirring and reacting at room temperature; (4) And (3) centrifuging and drying the material obtained in the step (3), and calcining in an air atmosphere to obtain the material. The invention does not involve complex reactions and operation steps and is easy to operate and repeat.
Description
Technical Field
The invention belongs to the technical field of new material preparation, and in particular relates to Pt NPs/Fe 2 O 3 A method for preparing hexagon catalyst and application thereof.
Background
Supported noble metal catalysts have excellent catalytic activity and stability compared to other transition metal oxide catalysts and have been widely studied in the industry. For supported noble metal catalysts, the active sites in the metallic state are capable of effecting electron transfer between the active sites, which can significantly reduce the reaction energy barrier of the catalytic reaction. Therefore, the highly dispersed supported noble metal catalyst with metallic nature generally has better catalytic activity than a nonmetallic catalyst, and can be applied to the fields of catalytic oxidation for removing indoor Volatile Organic Compounds (VOCs) and carbon monoxide (CO) and the like. However, the preparation method of the supported noble metal catalyst in the prior art has high cost, so that the application of the supported noble metal catalyst in actual working conditions is limited.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a Pt NPs/Fe 2 O 3 A method for preparing hexagon catalyst.
Another object of the present invention is to provide Pt NPs/Fe prepared by the above preparation method 2 O 3 Application of hexagon catalyst.
The technical scheme of the invention is as follows:
pt NPs/Fe 2 O 3 A method for preparing a hexagon catalyst comprising the steps of:
(1) Ultrasonically dissolving ferric trichloride hexahydrate in absolute ethyl alcohol to prepare ferric trichloride solution, adding deionized water and anhydrous sodium acetate, and uniformly stirring to perform hydrothermal reaction;
(2) Centrifuging and drying the material obtained in the step (1), and calcining in an air atmosphere to obtain Fe with exposed {001} crystal face 2 O 3 hexagon vector;
(3) Dissolving hexahydrated chloroplatinic acid in deionized water to obtain chloroplatinic acid solution, and adding Fe 2 O 3 Stirring and dispersing the hexagon carrier, adding sodium borohydride solution, and stirring and reacting at room temperature;
(4) Centrifuging and drying the material obtained in the step (3), and calcining in an air atmosphere to obtain the Pt NPs/Fe 2 O 3 hexagon catalyst wherein the loading of Pt is 0.2wt%.
In a preferred embodiment of the present invention, in the step (1), the ratio of ferric trichloride hexahydrate, absolute ethanol, deionized water and anhydrous sodium acetate is 13.12g:480mL:33.6mL:38.4g.
Further preferably, the hydrothermal reaction is carried out at 160-200 ℃ for 10-14h.
Still more preferably, in the step (2), the calcination temperature is 400 ℃ and the time is 4 hours.
Still more preferably, in the step (2), the temperature of drying is 80 ℃.
In a preferred embodiment of the present invention, in the step (3), the mass ratio of the chloroplatinic acid hexahydrate to the sodium borohydride in the sodium borohydride solution is 27:1, and the mass ratio of the chloroplatinic acid hexahydrate to the ferric trichloride hexahydrate is 0.0054:13.13.
Further preferably, in the step (4), the calcination temperature is 200 ℃ and the time is 2 hours.
Further preferably, in the step (4), the drying temperature is 120 ℃.
Pt NPs/Fe prepared by the preparation method 2 O 3 Use of a hexagon catalyst for removal of VOCs in a room.
Pt NPs/Fe prepared by the preparation method 2 O 3 Use of a hexagon catalyst in the catalytic oxidation of CO.
The beneficial effects of the invention are as follows:
1. the invention does not involve complex reactions and operation steps and is easy to operate and repeat.
2. The invention uses Fe 2 O 3 The abundant cationic defect sites on hexagon can anchor Pt atoms better, so that Pt can exist stably in a highly dispersed form on the carrier.
3. Pt NPs/Fe prepared by the invention 2 O 3 The hexagon catalyst has excellent catalytic performance, and the conversion rate of benzene reaches 90% at 165 ℃.
Drawings
FIG. 1 shows Fe of the high-exposure {001} crystal plane obtained in example 1 of the present invention 2 O 3 high resolution transmission electron microscopy of hexagonal vectors.
FIG. 2 shows the Pt NPs/Fe prepared in example 1 of this invention 2 O 3 Infrared CO adsorption experimental patterns for hexagon catalyst and comparative catalyst prepared in example 2.
FIG. 3 shows the Pt NPs/Fe prepared in example 1 of this invention 2 O 3 X-ray powder diffraction patterns for the hexagon catalyst and the comparative catalyst prepared in example 2.
FIG. 4 shows the Pt NPs/Fe prepared in example 1 of this invention 2 O 3 Activity profile of the hexagon catalyst and the comparative catalyst prepared in example 2 on the catalytic oxidation of benzene.
Detailed Description
The technical scheme of the invention is further illustrated and described below by the specific embodiments in combination with the accompanying drawings.
Example 1
Pt NPs/Fe 2 O 3 A method for preparing a hexagon catalyst comprising the steps of:
(1) Dissolving 13.12g of ferric trichloride hexahydrate in 480mL of absolute ethyl alcohol by ultrasonic to prepare ferric trichloride solution, adding 33.4mL of deionized water and 38.4g of anhydrous sodium acetate, magnetically stirring uniformly, and performing hydrothermal reaction at 180 ℃ for 12h;
(2) Centrifuging and drying the material obtained in the step (1) at 80 ℃, and calcining for 4 hours at 400 ℃ under an air atmosphere to obtain Fe with exposed {001} crystal face as shown in figure 1 2 O 3 hexagon vector;
(3) 0.0054g of chloroplatinic acid hexahydrate was dissolved in deionized water to prepare a chloroplatinic acid solution, and then the above-mentioned Fe was added thereto 2 O 3 The hexagon carrier is stirred and dispersed, then sodium borohydride solution (containing 0.002g of sodium borohydride and deionized water as solvent) is added, and magnetic stirring reaction is carried out at room temperature;
(4) Centrifuging the material obtained in the step (3) and drying at 120 ℃, placing the material in an air atmosphere, and calcining at 200 ℃ for 2 hours to obtain the Pt NPs/Fe 2 O 3 hexagon catalyst wherein the loading of Pt is 0.2wt%.
Example 2
Unlike example 1, a comparative catalyst (Pt) was obtained without adding a sodium borohydride solution in step (3) ox /Fe 2 O 3 hexagon catalyst).
Example 3
Pt NPs/Fe prepared in example 1 2 O 3 The hexagon catalyst and the comparative catalyst prepared in example 2 were respectively subjected to infrared CO adsorption experimental analysis, and the comparative results are shown in fig. 2. As can be seen from FIG. 2, the Pt NPs/Fe prepared in example 1 2 O 3 In the hexagon catalyst, the vibration frequency of CO linear adsorption on metallic Pt is 2085cm -1 Below 2090cm in the nonmetallic state -1 And it can be observed from the partial enlarged view that the vibration frequency of CO linearly adsorbed on the metallic Pt gradually red-shifts as the CO coverage decreases, which is thatThe characteristic phenomenon in the metallic state does not occur in the nonmetallic Pt of the comparative catalyst in example 2.
Example 4
To verify the success of the catalyst prepared and the Pt state of its surface, the Pt NPs/Fe prepared in example 1 2 O 3 The hexagon catalyst and the comparative catalyst prepared in example 2 were each subjected to X-ray powder diffraction analysis, and the results are shown in fig. 3.
It can be seen from FIG. 3 that all diffraction peaks of the catalyst sample are attributed to Fe 2 O 3 And no diffraction peak associated with Pt appears in the spectrum, indicating that Pt is highly dispersed as fine particles on the surface of the support in the prepared catalyst.
Example 5
Pt NPs/Fe prepared in example 1 2 O 3 The hexagon catalyst and the comparative catalyst prepared in example 2 were each pressed through a 40-60 mesh sieve, followed by taking 0.1g each in a quartz tube having an inner diameter of 0.6 mm. 0.05vol% benzene, 20vol% O are introduced 2 Balance gas N 2 Is mixed with the gas at a total flow rate of 100mL min -1 . And (3) programming the reactor to 350 ℃, and allowing the reacted gas to enter gas chromatography to analyze the catalytic performance of the catalyst. The performance of the catalyst is shown in figure 4.
As can be seen from FIG. 4, the Pt NPs/Fe supported by the Pt in the metallic state compared to the comparative catalyst supported by the Pt in the non-metallic state 2 O 3 The hexagon catalyst has better benzene catalytic oxidation performance, wherein the conversion rate of benzene reaches 90% at 165 ℃.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, i.e., the invention is not to be limited to the details of the invention.
Claims (10)
1. Pt NPs/Fe 2 O 3 A process for preparing a hexagon catalyst characterized by: the method comprises the following steps:
(1) Ultrasonically dissolving ferric trichloride hexahydrate in absolute ethyl alcohol to prepare ferric trichloride solution, adding deionized water and anhydrous sodium acetate, and uniformly stirring to perform hydrothermal reaction;
(2) Centrifuging and drying the material obtained in the step (1), and calcining in an air atmosphere to obtain Fe with exposed {001} crystal face 2 O 3 hexagon vector;
(3) Dissolving hexahydrated chloroplatinic acid in deionized water to obtain chloroplatinic acid solution, and adding Fe 2 O 3 Stirring and dispersing the hexagon carrier, adding sodium borohydride solution, and stirring and reacting at room temperature;
(4) Centrifuging and drying the material obtained in the step (3), and calcining in an air atmosphere to obtain the Pt NPs/Fe 2 O 3 hexagon catalyst wherein the loading of Pt is 0.2wt%.
2. The method of manufacturing according to claim 1, wherein: in the step (1), the ratio of the ferric trichloride hexahydrate, the absolute ethyl alcohol, the deionized water and the anhydrous sodium acetate is 13.12g:480mL:33.6mL:38.4g.
3. The method of manufacturing as claimed in claim 2, wherein: the hydrothermal reaction is carried out at 160-200 ℃ for 10-14h.
4. A method of preparation as claimed in claim 3, wherein: in the step (2), the calcination temperature is 400 ℃ and the time is 4 hours.
5. A method of preparation as claimed in claim 3, wherein: in the step (2), the drying temperature is 80 ℃.
6. The method of manufacturing according to claim 1, wherein: in the step (3), the mass ratio of the chloroplatinic acid hexahydrate to the sodium borohydride in the sodium borohydride solution is 27:1, and the mass ratio of the chloroplatinic acid hexahydrate to the ferric trichloride hexahydrate is 0.0054:13.13.
7. The method of manufacturing according to claim 6, wherein: in the step (4), the calcination temperature is 200 ℃ and the time is 2 hours.
8. The method of manufacturing according to claim 6, wherein: in the step (4), the drying temperature is 120 ℃.
9. Pt NPs/Fe prepared by the preparation method as claimed in any one of claims 1 to 8 2 O 3 Use of a hexagon catalyst for removal of VOCs in a room.
10. Pt NPs/Fe prepared by the preparation method as claimed in any one of claims 1 to 8 2 O 3 Use of a hexagon catalyst in the catalytic oxidation of CO.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310260430.6A CN116273007A (en) | 2023-03-17 | 2023-03-17 | Pt NPs/Fe 2 O 3 Preparation method and application of hexagon catalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310260430.6A CN116273007A (en) | 2023-03-17 | 2023-03-17 | Pt NPs/Fe 2 O 3 Preparation method and application of hexagon catalyst |
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| CN116273007A true CN116273007A (en) | 2023-06-23 |
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- 2023-03-17 CN CN202310260430.6A patent/CN116273007A/en active Pending
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