CN114433074A - Petal-shaped manganese-cerium composite oxide denitration catalyst and preparation method thereof - Google Patents
Petal-shaped manganese-cerium composite oxide denitration catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 46
- WYCDUUBJSAUXFS-UHFFFAOYSA-N [Mn].[Ce] Chemical compound [Mn].[Ce] WYCDUUBJSAUXFS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 9
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- KQJQGYQIHVYKTF-UHFFFAOYSA-N cerium(3+);trinitrate;hydrate Chemical compound O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KQJQGYQIHVYKTF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001816 cooling Methods 0.000 claims abstract description 5
- HBTFASPVVFSRRI-UHFFFAOYSA-N manganese(2+);dinitrate;hydrate Chemical compound O.[Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O HBTFASPVVFSRRI-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 3
- 239000003546 flue gas Substances 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 235000013842 nitrous oxide Nutrition 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 229910000420 cerium oxide Inorganic materials 0.000 description 2
- 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 2
- 238000011161 development Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- ALIMWUQMDCBYFM-UHFFFAOYSA-N manganese(2+);dinitrate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ALIMWUQMDCBYFM-UHFFFAOYSA-N 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- 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
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- 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
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/613—10-100 m2/g
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Abstract
The invention relates to a petal-shaped manganese-cerium composite oxide denitration catalyst and a preparation method thereof, belonging to the field of catalyst technology and environmental protection. The catalyst has a petal-shaped structure and is composed of a manganese-cerium composite oxide. The preparation method of the catalyst comprises the following steps: (1) dissolving potassium permanganate, manganese nitrate hydrate and cerium nitrate hydrate in deionized water, uniformly stirring, adding into a hydrothermal reaction kettle, reacting at the temperature of 130-160 ℃ for 10-15 hours, and cooling; (2) washing and centrifuging the suspension obtained in the step (1), and then drying; (3) and (3) roasting the product obtained in the step (2) in an air atmosphere to obtain the manganese-cerium composite oxide denitration catalyst. The manganese-cerium composite oxide denitration catalyst prepared by a hydrothermal method has rich active sites and acid sites, has a petal-shaped structure, and is beneficial to providing more active sites so as to promote the adsorption of gas.
Description
Technical Field
The invention relates to a petal-shaped manganese-cerium composite oxide denitration catalyst and a preparation method thereof, belonging to the field of catalyst technology and environmental protection.
Background
At present, nitrogen oxides discharged by ships using diesel engines as engines cause a series of pollution to the environment and cause serious harm to human health, so that the reduction of the discharge of the nitrogen oxides has important significance for environmental protection. The marine diesel engine can treat 50 percent of NO by means of an internal purification technologyxAnd the increasingly strict emission requirements cannot be met, so that the external purification technology gradually becomes the development direction of the future. Wherein NH3The SCR technology is widely used in the denitration direction of ship exhaust gas because of its high denitration efficiency, mature technology and convenient operation, and its technical core is the creation of catalyst.
At present, the technical requirements for the denitration catalyst are that the denitration catalyst has good SCR activity, nitrogen selectivity, sulfur resistance, water resistance and the like in a wide temperature range under a high space velocity condition. Therefore, the development of the denitration catalyst with a novel structure has important practical significance for the denitration treatment of the ship exhaust.
Disclosure of Invention
The invention aims to provide a manganese-cerium composite oxide denitration catalyst and a preparation method thereof.
In order to realize the purpose, the technical scheme of the invention is as follows:
the invention provides a manganese-cerium composite oxide denitration catalyst, which has a petal-shaped structure and is composed of a manganese-cerium composite oxide.
In the technical scheme, furthermore, the specific surface area of the catalyst is 50-80 m2The molar ratio of manganese dioxide to cerium dioxide in the catalyst is 5: 1-1: 1.
The invention also provides a preparation method of the petal-shaped manganese-cerium composite oxide denitration catalyst, which comprises the following steps:
(1) dissolving potassium permanganate, manganese nitrate hydrate and cerium nitrate hydrate in deionized water, uniformly stirring, adding into a hydrothermal reaction kettle, reacting at the temperature of 130-160 ℃ for 10-15 hours, and cooling;
(2) washing and centrifuging the suspension obtained in the step (1), and then drying;
(3) and (3) roasting the product obtained in the step (2) in an air atmosphere to obtain the manganese-cerium composite oxide denitration catalyst.
In the above technical scheme, further, in the step (1), the mass ratio of potassium permanganate, manganese nitrate hydrate, cerium nitrate hydrate to deionized water is 5: (1-4): (1-4): 180.
in the above technical scheme, further, in the step (1), the stirring speed is 100-300 rpm/min, and the stirring time is 1-2 hours.
In the above technical scheme, further, in the step (2), the drying time is 8-16 h.
In the technical scheme, furthermore, in the step (3), the roasting temperature is 500-700 ℃, and the roasting time is 5-9 hours.
In the above technical scheme, further, in the step (3), the air flow rate in the air atmosphere is 50-300 ml/min, and the temperature is programmed to be 500-700 ℃ at a temperature rise rate of 10-20 ℃/min in the air atmosphere.
Compared with the prior art, the invention has the beneficial effects that:
(1) the manganese-cerium composite oxide denitration catalyst prepared by a hydrothermal method has rich active sites and acid sites, has a petal-shaped structure, and is beneficial to providing more active sites so as to promote the adsorption of gas;
(2) under the action of catalyst, 80% of nitrogen oxide can be converted into N at low temperature (90℃)2。
Drawings
FIG. 1 is an SEM photograph of the catalyst prepared in example 1;
FIG. 2 is a diagram of a test system architecture;
FIG. 3 is a graph of the conversion of nitrogen oxides for the catalysts prepared in examples 1 and 2;
fig. 4 is a graph of nitrogen oxide conversion for the catalyst of comparative example 1.
1、N2；2、NH3/N2；3、NO/N2；4、O2；5、SO2/N2(ii) a 6. A gas mixing tank; 7. a steam bottle; 8. a tubular heating furnace and a reaction tube; 9. a flue gas analyzer; 10. laughing gas detector.
Detailed Description
The following describes embodiments of the present invention in detail. The following embodiments are described as examples and are intended to illustrate the invention, but not to limit the invention.
The denitration catalyst of the invention is prepared by using a hydrothermal method to prepare Mn (NO) as a manganese cerium metal precursor3)3·4H2O、Ce(NO3)3·6H2O、KMnO4Uniformly dispersing, synthesizing a catalyst by a hydrothermal method, and then heating and oxidizing in an air atmosphere to form a petal-shaped structure. Details of the operation of the synthesis catalyst are shown in examples 1-2; the denitration reaction was used as a catalyst to evaluate the reaction, and is shown in example 3.
Example 1
The catalyst prepared in example 1 had a molar ratio of manganese dioxide to cerium oxide of 1:1 and was prepared by the following steps:
(1) mixing 0.4g of manganese nitrate tetrahydrate, 0.4g of cerium nitrate hexahydrate, 1g of potassium permanganate and 36ml of deionized water under a stirring state, wherein the stirring speed is 300rpm/min, and the stirring time is 1.5h, then transferring the mixed solution into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 12h at 140 ℃;
(2) cooling to obtain a suspension, washing the suspension with deionized water for about 5-10 times, and then centrifugally drying the suspension for 12 hours;
(3) then the temperature was raised to 500 ℃ in an air atmosphere and held for 6 hours.
The SEM image of the catalyst obtained in example 1 is shown in fig. 1, and it can be seen from fig. 1 that the catalyst shows a petal-like structure after calcination.
Example 2
The catalyst prepared in example 2 had a molar ratio of manganese dioxide to cerium oxide of 5:1 and was prepared by the following steps:
(1) mixing 0.63g of manganese nitrate tetrahydrate, 0.17g of cerium nitrate hexahydrate, 1g of potassium permanganate and 36ml of deionized water under a stirring state, wherein the stirring speed is 300rpm/min, and the stirring time is 1.5h, then transferring the mixed solution into a hydrothermal reaction kettle, and carrying out hydrothermal reaction for 12h at 140 ℃;
(2) cooling to obtain a suspension, washing the suspension with deionized water for about 5-10 times, and then centrifugally drying the suspension for 12 hours;
(3) then the temperature was raised to 500 ℃ in an air atmosphere and held for 6 hours.
Example 3
Filling the catalysts prepared in the embodiments 1 and 2 into a self-made quartz reaction tube, introducing mixed gas, and adjusting GHSV to 100000-130000 h-1Increasing the temperature during the test to test the activity; the NO concentration is detected by a flue gas analyzer at each temperature point, and the N is detected by a laughing gas detector2The amount of O produced.
The test system structure is shown in fig. 2.
Fig. 3 shows NO catalytic activities of manganese cerium composite oxides at different ratios.
Comparative example 1
Performing performance test comparison on the catalyst with the shell-core structure prepared from the same elements as in example 1, filling the catalyst into a self-made quartz reaction tube, introducing mixed gas, and adjusting the GHSV to 100000-130000 h-1Increasing the temperature during the test to test the activity; the NO concentration is detected by a flue gas analyzer at each temperature point, and the N is detected by a laughing gas detector2The amount of O produced.
The test system structure is shown in fig. 2.
FIG. 4 shows the results of NO catalytic activity test of manganese-cerium composite oxide of comparative example 1, and it was found from comparison of FIG. 3 with FIG. 4 that Mn was produced by hydrothermal methodxCeyThe performance of the catalyst is obviously improved under the low temperature condition, and the catalyst can reach 80 DEG CConversion rate of more than 80%, NO conversion rate of more than 80% in a wide temperature range of 80-360 ℃, compared with CeO in comparative example 12@MnO2The catalyst reached 80% NO conversion at 330 ℃ and the 80% NO conversion temperature interval was only 50 ℃. It can be seen that Mn is produced according to the present inventionxCeyThe catalyst has excellent low-temperature activity.
The above examples are merely preferred embodiments of the present invention, and are not intended to limit the embodiments. The protection scope of the present invention shall be subject to the scope defined by the claims. Other variations and modifications may be made on the basis of the above description. Obvious variations or modifications of this invention are within the scope of the invention.
Claims (8)
1. The denitration catalyst is characterized by having a petal-shaped structure and consisting of manganese-cerium composite oxides.
2. The catalyst according to claim 1, wherein the specific surface area of the catalyst is 50 to 80m2The molar ratio of manganese dioxide to cerium dioxide in the catalyst is 5: 1-1: 1.
3. A preparation method of a petal-shaped manganese-cerium composite oxide denitration catalyst is characterized by comprising the following steps:
(1) dissolving potassium permanganate, manganese nitrate hydrate and cerium nitrate hydrate in deionized water, uniformly stirring, adding into a hydrothermal reaction kettle, reacting at the temperature of 130-160 ℃ for 10-15 hours, and cooling;
(2) washing and centrifuging the suspension obtained in the step (1), and then drying;
(3) and (3) roasting the product obtained in the step (2) in an air atmosphere to obtain the manganese-cerium composite oxide denitration catalyst.
4. The preparation method according to claim 3, wherein in the step (1), the mass ratio of potassium permanganate, manganese nitrate hydrate, cerium nitrate hydrate to deionized water is 5: (1-4): (1-4): 180.
5. the preparation method according to claim 3, wherein in the step (1), the stirring speed is 100-300 rpm/min, and the stirring time is 1-2 h.
6. The preparation method according to claim 3, wherein in the step (2), the drying time is 8-16 h.
7. The preparation method according to claim 3, wherein in the step (3), the roasting temperature is 500-700 ℃ and the roasting time is 5-9 h.
8. The method according to claim 3, wherein in the step (3), the air flow rate in the air atmosphere is 50-300 ml/min, and the temperature is programmed to be 500-700 ℃ at a temperature rise rate of 10-20 ℃/min in the air atmosphere.
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Cited By (3)
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| CN114984944A (en) * | 2022-06-24 | 2022-09-02 | 河北工业大学 | Preparation method of high-sulfur-resistance low-temperature SCR catalyst |
| CN115430417A (en) * | 2022-08-31 | 2022-12-06 | 兰润环保技术(烟台)有限公司 | Flue gas denitration catalyst and preparation method thereof |
| CN116251585A (en) * | 2023-02-27 | 2023-06-13 | 武汉科技大学 | Cerium-manganese catalyst for catalytic oxidation of toluene and preparation method thereof |
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