CN114682252B - Manganese catalyst and preparation method and application thereof - Google Patents
Manganese catalyst and preparation method and application thereof Download PDFInfo
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- CN114682252B CN114682252B CN202210430593.XA CN202210430593A CN114682252B CN 114682252 B CN114682252 B CN 114682252B CN 202210430593 A CN202210430593 A CN 202210430593A CN 114682252 B CN114682252 B CN 114682252B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 28
- 239000011572 manganese Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 15
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 14
- 238000001354 calcination 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
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 4
- 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
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000000967 suction filtration Methods 0.000 claims description 2
- 230000032683 aging Effects 0.000 claims 1
- 238000001132 ultrasonic dispersion Methods 0.000 claims 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 abstract description 30
- 239000000243 solution Substances 0.000 abstract description 21
- 239000000693 micelle Substances 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 239000011259 mixed solution Substances 0.000 abstract description 6
- 239000004094 surface-active agent Substances 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000012295 chemical reaction liquid Substances 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 3
- 238000005406 washing Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 15
- 238000001514 detection method Methods 0.000 description 9
- 239000013049 sediment Substances 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 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
- 239000000203 mixture Substances 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
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental 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
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical class [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 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
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 230000035484 reaction time Effects 0.000 description 1
Classifications
-
- 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
-
- 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
Abstract
The invention belongs to the field of catalysts, and discloses a manganese catalyst, a preparation method and application thereof, wherein the preparation method of the manganese catalyst comprises the following steps: step 1: adding a surfactant which is easy to form micelle balls in water into deionized water, and uniformly stirring to prepare micelle ball solution with the concentration of 0.1-2 g/L; step 2: adding a potassium permanganate solution into the micelle ball solution prepared in the step 1, and uniformly stirring to obtain a mixed solution, wherein the mass volume ratio of the added amount of the potassium permanganate to the micelle ball solution is 1-2g/L; step 3: dropwise adding n-butanol into the mixed solution obtained in the step 2, and stirring at normal temperature to react to obtain a reaction solution; step 4: and (3) standing the reaction liquid obtained in the step (3), filtering, taking a precipitate, washing the precipitate with water, and drying, calcining and grinding to obtain manganese catalyst powder. The manganese catalyst prepared by the invention has excellent toluene catalytic degradation performance.
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, catalysts used in the catalytic oxidation technology of volatile organic gases (VOCs) applied at home and abroad are largely classified into two types: one class is noble metal catalysts, such as platinum and palladium, which are highly effective, 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-based oxides are widely studied and paid attention to because of their low price, excellent catalytic performance and environmental friendliness. And in the last decade, manganese oxides have been found to be comparable to noble metal catalysts in terms of catalytic oxidation of toluene-based 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 disadvantages can directly prevent the commercialization of the manganese-based catalysts.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a preparation method of a manganese catalyst, which is simple and convenient in preparation method and low in cost.
In order to achieve the above object, the technical scheme of the present invention is as follows: a preparation method of a manganese catalyst comprises the following steps:
step 1: adding a surfactant which is easy to form micelle balls in water into deionized water, and uniformly stirring to prepare micelle ball solution with the concentration of 0.1-2 g/L;
step 2: adding a potassium permanganate solution into the micelle ball solution prepared in the step 1, and uniformly stirring to obtain a mixed solution, wherein the mass volume ratio of the added amount of the potassium permanganate to the micelle ball solution is 1-2g/L;
step 3: dropwise adding n-butanol into the mixed solution obtained in the step 2, and stirring at normal temperature to react and 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 lower than 4.68;
step 4: and (3) standing the reaction liquid 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.
The surfactant in the step 1 in the technical scheme is cetyl trimethyl ammonium bromide or F127.
The concentration of the micelle solution in the step 1 in the technical scheme is 0.4g/L.
In the technical scheme, the mass volume ratio of the addition amount of the potassium permanganate in the step 2 to the micellar solution is 1.5-1.6g/L.
In the technical scheme, the reaction time at normal temperature in the step 3 is 24 hours.
In the technical scheme, in the step 4, standing time is 1h, calcining temperature is 300-700 ℃ and calcining time is 2h, wherein calcining heating rate is 2 ℃/min.
The second object of the present invention is to provide a manganese-based catalyst produced by the above production method.
The second object of the 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 adopting the soft mold method, a large number of micelle balls (serving as a soft mold plate) are formed by the surfactant in the solution, a large number of sites are provided for nucleation growth of manganese oxide (the manganese oxide is obtained by reducing potassium permanganate by n-butyl alcohol), meanwhile, in the calcination stage, the micelle balls are all decomposed, only a small amount of conductive carbon black is remained to be combined with the manganese oxide, so that the conductivity of the manganese oxide is improved, in addition, the existence of the soft mold plate greatly improves the dispersibility of the manganese oxide, reduces the grain size, ensures that the grain size is uniform, and improves the specific surface area and the active site of the manganese oxide, thereby improving the performance of the manganese oxide catalyst.
Drawings
FIG. 1 is a flow chart of the preparation of the manganese-based catalyst according to the present invention.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
As shown in fig. 1, the invention discloses a preparation method of a manganese catalyst, which comprises the following steps:
step 1: adding a surfactant which is easy to form micelle balls in water into deionized water, fully stirring and uniformly dispersing by ultrasonic to prepare micelle ball solution with the concentration of 0.1-2 g/L;
step 2: adding a potassium permanganate solution into the micelle ball solution prepared in the step 1, and uniformly stirring to obtain a mixed solution, wherein the mass volume ratio of the added amount of the potassium permanganate to the micelle ball solution is 1-2g/L;
step 3: dropwise adding n-butanol into the mixed solution obtained in the step 2, stirring and uniformly dispersing by ultrasonic, and then standing at normal temperature for reaction to obtain a reaction solution, wherein the mass ratio of the addition of the n-butanol to the addition of the potassium permanganate is not lower than 4.68;
step 4: and (3) standing the reaction liquid 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
100mg of CTAB (cetyltrimethylammonium bromide) was added to 500mL of deionized water, stirred ultrasonically for 1h, 0.5g of potassium permanganate was added, stirring was continued for 0.5h, and dispersed ultrasonically for 0.5h. 4mL of n-butanol (analytically pure) was added to the solution, stirred at room temperature for 24 hours, aged for 1 hour, the precipitate was collected by suction filtration, and the precipitate was washed 3 times with deionized water and dried. Calcining at 300 ℃ for 2 hours, and grinding to obtain the manganese catalyst. Adding 100mg of prepared manganese catalyst into a detection device under the detection condition of toluene concentration of 1000ppm and clean air carrier gas (without interference of impurities, water vapor and the like), and space velocity of 60000h -1 The reaction temperature is raised from 150 ℃ to 400 ℃, the temperature is kept for 1h at 25 ℃ when the temperature is raised, and the reaction is detected three times (the value is obtained after each indication is stable), and the average value is obtained. As proved by detection, the manganese catalyst can decompose more than 50% of toluene at about 235 ℃ and completely decompose more than 99% of toluene at about 275 ℃.
Example 2
1000mg of CTAB was added to 500mL of deionized water, stirred ultrasonically for 1h, 0.5g of potassium permanganate was added, stirring was continued for 0.5h, and dispersed ultrasonically for 0.5h. 4mL of n-butanol is added into the solution, the mixture is stirred for 24 hours at room temperature, aged for 1 hour, the sediment is filtered by suction, and the sediment is washed with deionized water for 3 times and dried. Calcining at 500 ℃ for 2 hours, and grinding to obtain the manganese catalyst. Adding 100mg of prepared catalyst into a detection device under the detection condition of toluene concentrationClean air carrier gas (without impurity, water vapor, etc. interference) at 1000ppm, airspeed 60000h -1 The reaction temperature is raised from 150 ℃ to 400 ℃, the temperature is kept for 1h at 25 ℃ when the temperature is raised, and the reaction is detected three times (the value is obtained after each indication is stable), and the average value is obtained. Through detection, the catalyst can decompose more than 50% of toluene at about 255 ℃, and can completely decompose more than 99% of toluene at about 300 ℃.
Example 3
200mg of F127 (poloxamer) is added to 500mL of deionized water, stirred ultrasonically for 1h, 0.5g of potassium permanganate is added, stirring is continued for 0.5h, and sonicated for 0.5h. 4mL of n-butanol is added into the solution, the mixture is stirred for 24 hours at room temperature, aged for 1 hour, the sediment is filtered by suction, and the sediment is washed with deionized water for 3 times and dried. Calcining at 700 ℃ for 2 hours, and grinding to obtain the manganese catalyst. Adding 100mg of the prepared catalyst into a detection device under the detection condition of toluene concentration of 1000ppm and clean air carrier gas (without interference of impurities, water vapor and the like) and space velocity of 60000h -1 The reaction temperature is raised from 150 ℃ to 400 ℃, the temperature is kept for 1h at 25 ℃ when the temperature is raised, and the reaction is detected three times (the value is obtained after each indication is stable), and the average value is obtained. The detection shows that the catalyst can decompose 50% or more of toluene at about 270 ℃ and can completely decompose (99% or more) at about 325 ℃.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (3)
1. The preparation method of the manganese catalyst is characterized by comprising the following steps:
100mg of cetyltrimethylammonium bromide is added into 500mL of deionized water, ultrasonic stirring is carried out for 1h, 0.5g of potassium permanganate is added, stirring is continued for 0.5h, ultrasonic dispersion is carried out for 0.5h, 4mL of n-butanol is added into the solution, stirring is carried out for 24h at room temperature, ageing is carried out for 1h, suction filtration is carried out to obtain precipitate, the precipitate is washed with deionized water for 3 times, drying is carried out, calcination is carried out for 2h at 300 ℃, the calcination heating rate is 2 ℃/min, and manganese-based catalyst is obtained after grinding.
2. A manganese-based catalyst, characterized by being produced by the production method according to claim 1.
3. Use of the manganese-based catalyst according to claim 2 for the catalytic decomposition of organic volatile gases.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210430593.XA CN114682252B (en) | 2022-04-22 | 2022-04-22 | Manganese catalyst and preparation method and application thereof |
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| CN202210430593.XA CN114682252B (en) | 2022-04-22 | 2022-04-22 | Manganese catalyst and preparation method and application thereof |
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| CN114682252A CN114682252A (en) | 2022-07-01 |
| CN114682252B true CN114682252B (en) | 2024-01-05 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502848A (en) * | 2011-10-27 | 2012-06-20 | 湖南科技大学 | Solvothermal preparation method for alkali manganese oxide nanowires |
| CN103754936A (en) * | 2014-01-23 | 2014-04-30 | 山东科技大学 | Method for synthesizing mesoporous manganese oxide |
| CN105618031A (en) * | 2016-01-05 | 2016-06-01 | 武汉理工大学 | Nanorod-like low-temperature denitration catalyst and preparation method thereof |
| 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 |
| 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 |
-
2022
- 2022-04-22 CN CN202210430593.XA patent/CN114682252B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502848A (en) * | 2011-10-27 | 2012-06-20 | 湖南科技大学 | Solvothermal preparation method for alkali manganese oxide nanowires |
| CN103754936A (en) * | 2014-01-23 | 2014-04-30 | 山东科技大学 | Method for synthesizing mesoporous manganese oxide |
| CN105618031A (en) * | 2016-01-05 | 2016-06-01 | 武汉理工大学 | Nanorod-like low-temperature denitration catalyst and preparation method thereof |
| 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 |
| 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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