CN114682252A - Manganese catalyst, preparation method and application thereof - Google Patents
Manganese catalyst, preparation method and application thereof Download PDFInfo
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- CN114682252A CN114682252A CN202210430593.XA CN202210430593A CN114682252A CN 114682252 A CN114682252 A CN 114682252A CN 202210430593 A CN202210430593 A CN 202210430593A CN 114682252 A CN114682252 A CN 114682252A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 45
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 33
- 239000011572 manganese Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 32
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000000693 micelle Substances 0.000 claims abstract description 10
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000004094 surface-active agent Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 4
- 238000003421 catalytic decomposition reaction Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 30
- 230000000593 degrading effect Effects 0.000 abstract description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 16
- 238000001514 detection method Methods 0.000 description 9
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000012935 Averaging Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229960000502 poloxamer Drugs 0.000 description 1
- 229920001983 poloxamer Polymers 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
- B01J23/16—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
-
- 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
- B01D53/8678—Removing components of undefined structure
- B01D53/8687—Organic components
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- 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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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention belongs to the field of catalysts, and discloses a manganese-based catalyst and a preparation method and application thereof, wherein the preparation method of the manganese-based catalyst comprises the following steps: step 1: adding a surfactant which can easily form micelle balls in water into deionized water, and uniformly stirring to prepare a micelle ball solution with the concentration of 0.1-2 g/L; step 2: adding a potassium permanganate solution into the micellar solution prepared in the step (1), and uniformly stirring to obtain a mixed solution, wherein the mass-volume ratio of the addition amount of the potassium permanganate to the micellar solution is 1-2 g/L; and step 3: dropwise adding n-butanol into the mixed solution obtained in the step 2, and stirring and reacting at normal temperature to obtain a reaction solution; and 4, step 4: and (3) standing the reaction solution obtained in the step (3), filtering, taking a precipitate, washing the precipitate, and drying, calcining and grinding to obtain the manganese catalyst powder. The manganese catalyst prepared by the invention has excellent performance of catalyzing and degrading toluene.
Description
Technical Field
The invention belongs to the field of catalysts, and particularly relates to a manganese catalyst, and a preparation method and application thereof.
Background
So far, the catalysts used for the catalytic oxidation of volatile organic gases (VOCs) and studied at home and abroad are roughly classified into two types: one class is noble metal catalysts, such as platinum and palladium, which are highly efficient, expensive and subject to deactivation. Another class is non-noble metal oxide catalysts such as manganese, copper, cerium, iron, cobalt, and the like. Among them, manganese oxides have been widely studied and paid attention to because of their low price, excellent catalytic performance and environmental friendliness. And in the last decade, the manganese oxides have been found to be comparable to the activity of noble metal catalysts in the catalytic oxidation of toluene-like VOCs gases in some cases. However, the manganese-based catalysts on the market at present have the problems of insufficient activity, easy agglomeration, poor conductivity and the like, and the defects directly obstruct the commercial application of the manganese-based catalysts.
Disclosure of Invention
In order to solve the above-mentioned problems, an object of the present invention is to provide a method for producing a manganese-based catalyst, which is simple and inexpensive.
In order to achieve the purpose, the technical scheme of the invention is as follows: the preparation method of the manganese catalyst comprises the following steps:
step 1: adding a surfactant which can easily form micelle balls in water into deionized water, and uniformly stirring to prepare a micelle ball solution with the concentration of 0.1-2 g/L;
step 2: adding a potassium permanganate solution into the micellar solution prepared in the step (1), and uniformly stirring to obtain a mixed solution, wherein the mass-volume ratio of the addition amount of the potassium permanganate to the micellar solution is 1-2 g/L;
and step 3: dropwise adding n-butanol into the mixed solution obtained in the step 2, and stirring and reacting at normal temperature to obtain a reaction solution, wherein the mass ratio of the addition amount of the n-butanol to the addition amount of the potassium permanganate is not less than 4.68;
and 4, step 4: and (3) standing the reaction solution obtained in the step (3), filtering, taking a precipitate, washing the precipitate with water, drying, calcining in an air environment, and grinding to obtain manganese catalyst powder.
In the technical scheme, the surfactant in the step 1 is cetyl trimethyl ammonium bromide or F127.
The concentration of the micellar solution in the step 1 in the technical scheme is 0.4 g/L.
In the technical scheme, the mass-to-volume ratio of the addition amount of the potassium permanganate to the micellar solution in the step 2 is 1.5-1.6 g/L.
In the technical scheme, the normal-temperature reaction time in the step 3 is 24 hours.
In the technical scheme, the standing time in the step 4 is 1h, the calcining temperature is 300-700 ℃, and the calcining time is 2h, wherein the calcining temperature rise rate is 2 ℃/min.
The second object of the present invention is to provide a manganese-based catalyst prepared by the above-mentioned preparation method.
The second purpose of the present invention is to provide an application of the manganese-based catalyst in catalytic decomposition of organic volatile gases.
The invention has the advantages that: in the manganese catalyst prepared by the soft mold method, the surfactant forms a large number of micelle spheres (as a soft template) in the solution to provide a large number of sites for the nucleation growth of manganese oxide (manganese oxide is obtained by reducing potassium permanganate with n-butyl alcohol), the micelle spheres are completely decomposed, only a small amount of conductive carbon black is left to be combined with the manganese oxide, the conductivity of the manganese oxide is improved, in addition, the existence of the soft template greatly improves the dispersity of the manganese oxide, reduces the grain size, ensures that the grain size is uniform, improves the specific surface area and the active site of the manganese oxide, thereby improving the performance of the manganese oxide catalyst, because of the unique nano structure, the prepared manganese catalyst has excellent performance of degrading and catalyzing toluene, and because the use of a noble metal catalyst is avoided, the preparation cost is greatly reduced, and the method is favorable for industrial application.
Drawings
FIG. 1 is a flow chart of the preparation of the manganese-based catalyst of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
As shown in figure 1, the invention discloses a preparation method of a manganese catalyst, which comprises the following steps:
step 1: adding a surfactant which can easily form micelle balls in water into deionized water, fully stirring and uniformly dispersing by ultrasonic to prepare a micelle ball solution with the concentration of 0.1-2 g/L;
step 2: adding a potassium permanganate solution into the micellar solution prepared in the step (1), and uniformly stirring to obtain a mixed solution, wherein the mass-volume ratio of the addition amount of the potassium permanganate to the micellar solution is 1-2 g/L;
and step 3: dropwise adding n-butyl alcohol into the mixed solution obtained in the step 2, stirring and ultrasonically dispersing uniformly, and then placing at normal temperature for reaction to obtain a reaction solution, wherein the mass ratio of the addition amount of the n-butyl alcohol to the addition amount of the potassium permanganate is not lower than 4.68;
and 4, step 4: and (3) standing the reaction solution obtained in the step (3), filtering, taking a precipitate, washing the precipitate with water, drying, calcining in an air environment, and grinding to obtain manganese catalyst powder.
Example 1
Adding 100mg CTAB (cetyl trimethyl ammonium bromide) into 500mL deionized water, ultrasonically stirring for 1h, adding 0.5g potassium permanganate, continuously stirring for 0.5h, and ultrasonically dispersing for 0.5 h. Adding 4mL of n-butanol (analytically pure) into the solution, stirring at room temperature for 24 hours, aging for 1 hour, filtering to obtain a precipitate, washing the precipitate with deionized water for 3 times, and drying. Calcining at 300 ℃ for 2h, and grinding to obtain the manganese catalyst. Get100mg of prepared manganese catalyst is added into a detection device under the detection conditions of toluene concentration of 1000ppm, clean air carrier gas (without interference of impurities, water vapor and the like) and space velocity of 60000h-1And (3) raising the reaction temperature from 150 ℃ to 400 ℃, keeping the temperature for 1h at the temperature of 25 ℃ every time, detecting for three times (taking values after each reading is stable), and averaging. The manganese catalyst can decompose over 50 percent of toluene at about 235 ℃ and completely decompose toluene (over 99 percent) at about 275 ℃ through detection.
Example 2
Adding 1000mg CTAB into 500mL deionized water, ultrasonically stirring for 1h, adding 0.5g potassium permanganate, continuously stirring for 0.5h, and ultrasonically dispersing for 0.5 h. Adding 4mL of n-butanol into the solution, stirring at room temperature for 24 hours, aging for 1 hour, filtering to obtain a precipitate, washing the precipitate with deionized water for 3 times, and drying. Calcining at 500 ℃ for 2h, and grinding to obtain the manganese catalyst. 100mg of prepared catalyst is added into a detection device, and the detection conditions are that the concentration of toluene is 1000ppm, clean air carrier gas (without interference of impurities, water vapor and the like) and space velocity is 60000h-1The reaction temperature is increased from 150 ℃ to 400 ℃, the temperature is kept for 1h at the temperature of 25 ℃ every time the temperature is increased, the temperature is detected for three times (after each reading is stable), and the average value is taken. The detection shows that the catalyst can decompose over 50 percent of toluene at about 255 ℃ and completely decompose the toluene (over 99 percent) at about 300 ℃.
Example 3
Adding 200mg of F127 (poloxamer) into 500mL of deionized water, ultrasonically stirring for 1h, adding 0.5g of potassium permanganate, continuously stirring for 0.5h, and ultrasonically stirring for 0.5 h. Adding 4mL of n-butanol into the solution, stirring at room temperature for 24 hours, aging for 1 hour, filtering to obtain a precipitate, washing the precipitate with deionized water for 3 times, and drying. Calcining for 2h at 700 ℃, and grinding to obtain the manganese catalyst. 100mg of prepared catalyst is added into a detection device, and the detection conditions are that the concentration of toluene is 1000ppm, clean air carrier gas (without interference of impurities, water vapor and the like) and space velocity is 60000h-1And (3) raising the reaction temperature from 150 ℃ to 400 ℃, keeping the temperature for 1h at the temperature of 25 ℃ every time, detecting for three times (taking values after each reading is stable), and averaging. The catalyst can decompose over 50 percent of toluene at the temperature of about 270 ℃ and completely decompose (over 99 percent) at the temperature of about 325 ℃ through detection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The preparation method of the manganese catalyst is characterized by comprising the following steps of:
step 1: adding a surfactant which can easily form micelle balls in water into deionized water, and uniformly stirring to prepare a micelle ball solution with the concentration of 0.1-2 g/L;
step 2: adding a potassium permanganate solution into the micellar solution prepared in the step (1), and uniformly stirring to obtain a mixed solution, wherein the mass-volume ratio of the addition amount of the potassium permanganate to the micellar solution is 1-2 g/L;
and step 3: dropwise adding n-butanol into the mixed solution obtained in the step 2, and stirring and reacting at normal temperature to obtain a reaction solution, wherein the mass ratio of the addition amount of the n-butanol to the addition amount of the potassium permanganate is not less than 4.68;
and 4, step 4: and (3) standing the reaction solution obtained in the step (3), filtering, taking a precipitate, washing the precipitate with water, drying, calcining in an air environment, and grinding to obtain manganese catalyst powder.
2. The method for preparing a manganese-based catalyst according to claim 1, wherein said surfactant in step 1 is cetyltrimethylammonium bromide or F127.
3. The method for preparing a manganese-based catalyst according to claim 1, wherein the concentration of the micellar solution in step 1 is 0.4 g/L.
4. The manganese-based catalyst preparation method according to claim 1, wherein the mass-to-volume ratio of the amount of potassium permanganate added to the micellar solution in step 2 is 1.5 to 1.6 g/L.
5. The method for preparing a manganese-based catalyst according to claim 1, wherein the reaction time at normal temperature in step 3 is 24 hours.
6. The method for preparing manganese-based catalyst according to claim 1, wherein the standing time in step 4 is 1h, the calcination temperature is 300-700 ℃, and the calcination time is 2h, wherein the temperature rise rate of calcination is 2 ℃/min.
7. A manganese-based catalyst, characterized by being produced by the production method according to any one of claims 1 to 6.
8. Use of a manganese-based catalyst according to claim 7 for the catalytic decomposition of organic volatile gases.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116212856A (en) * | 2023-03-07 | 2023-06-06 | 北京清新环境技术股份有限公司 | Method for preparing cerium-manganese catalyst for high-performance catalytic oxidation of toluene by hydrothermal method, obtained catalyst and application |
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| CN110102290A (en) * | 2019-04-24 | 2019-08-09 | 华南理工大学 | A kind of K doped alpha-MnO2/Mn3O4Efficiency light thermocatalyst and preparation method and application |
| CN112357905A (en) * | 2020-10-12 | 2021-02-12 | 广东药科大学 | Nitrogen-doped mesoporous carbon nanosphere material and preparation method and application thereof |
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| CN102502848A (en) * | 2011-10-27 | 2012-06-20 | 湖南科技大学 | Solvothermal preparation method for alkali manganese oxide nanowires |
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| CN109482175A (en) * | 2018-11-23 | 2019-03-19 | 华南理工大学 | A kind of yolk-shell structure cryptomelane-type manganese dioxide-catalyst and the preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116212856A (en) * | 2023-03-07 | 2023-06-06 | 北京清新环境技术股份有限公司 | Method for preparing cerium-manganese catalyst for high-performance catalytic oxidation of toluene by hydrothermal method, obtained catalyst and application |
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