CN111889100A - Cryptomelane type mixed manganese oxide catalyst for removing soot of diesel vehicle through oxidation - Google Patents
Cryptomelane type mixed manganese oxide catalyst for removing soot of diesel vehicle through oxidation Download PDFInfo
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- CN111889100A CN111889100A CN202010769835.9A CN202010769835A CN111889100A CN 111889100 A CN111889100 A CN 111889100A CN 202010769835 A CN202010769835 A CN 202010769835A CN 111889100 A CN111889100 A CN 111889100A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 57
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 40
- 239000004071 soot Substances 0.000 title claims abstract description 31
- 230000003647 oxidation Effects 0.000 title claims abstract description 18
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 7
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 239000000779 smoke Substances 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000033116 oxidation-reduction process Effects 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 description 14
- 239000000243 solution Substances 0.000 description 10
- 229910052783 alkali metal Inorganic materials 0.000 description 7
- 150000001340 alkali metals Chemical class 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 6
- 239000011572 manganese Substances 0.000 description 5
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000002149 hierarchical pore Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 206010058467 Lung neoplasm malignant Diseases 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910016978 MnOx Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 206010006451 bronchitis Diseases 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 229940029329 intrinsic factor Drugs 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 201000005202 lung cancer Diseases 0.000 description 1
- 208000020816 lung neoplasm Diseases 0.000 description 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D49/00—Separating dispersed particles from gases, air or vapours by other methods
-
- 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
-
- B01J35/613—
-
- B01J35/633—
-
- B01J35/647—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
- B01D2258/012—Diesel engines and lean burn gasoline engines
Abstract
The invention relates to a cryptomelane type mixed manganese oxide catalyst for removing soot of a diesel vehicle by oxidation, wherein the chemical structural formula of the catalyst is KMnOx. The catalyst is prepared by taking potassium permanganate, manganese acetate and acetic acid as raw materials through precipitation reaction and calcination. The raw materials used in the invention are cheap and easily available, the conditions are mild, the preparation process is simple, and the method has important scientific significance and good application prospect. Prepared KMnOxThe catalyst has large specific surface area and pore volume, and has the characteristics of a multi-stage pore structure and good oxidation-reduction capability. The catalyst can be used for efficiently catalyzing and oxidizing soot particles of a diesel vehicle.
Description
Technical Field
The invention relates to a preparation method of a cryptomelane type mixed manganese oxide catalyst for removing soot of a diesel vehicle by oxidation and application of the cryptomelane type mixed manganese oxide catalyst in removing soot particles of the diesel vehicle by catalytic oxidation, belonging to the field of preparation and catalytic application of nano materials.
Background
Diesel engines are widely used due to low oil consumption, high power, high durability and high efficiency, however, particulate matter (PM, mainly soot) in diesel vehicle exhaust can enter the respiratory system of the human body, causing diseases such as lung cancer and bronchitis, and causing great harm to human health. Therefore, an efficient tail gas aftertreatment process is imperative. Among diesel aftertreatment technologies, particulate filters (DPF) are one of the most widely used technologies today. A particulate filter (DPF) is used to collect soot particles in the exhaust gases of diesel vehicles, which can be oxidized by oxygen at higher temperatures (> 600 ℃). However, the exhaust temperature of diesel vehicles is generally lower than 400 ℃, it is difficult to sufficiently burn soot particles at a low temperature, and the particulate filter is deactivated after long-term use. Therefore, it is an urgent task to develop a high efficiency catalyst to realize low temperature catalytic oxidation of soot.
At present, the catalysts for catalytic purification of automobile exhaust used at home and abroad can be classified into noble metal catalysts, transition metal catalysts and alkali metal catalysts according to different active components. Among them, noble metal catalysts have the advantages of better catalytic activity, thermal stability and selectivity, etc., but the noble metal resources are in short supply, the sulfur resistance is poor, and the high-temperature stability is poor, which limits the popularization and application of the noble metal catalysts. Transition metals generally have multiple valence states and stronger redox performance, and compared with alkali metals, transition metal catalysts have better thermal stability but low catalytic activity. The alkali metal catalyst has excellent catalytic activity and lower use cost, and meanwhile, the alkali metal with low melting point is easy to melt at high temperature, so that the alkali metal has fluidity, the contact area between the catalyst and the carbon smoke particles is greatly increased, and the catalytic oxidation of the carbon smoke particles is promoted. However, the characteristics of low melting point and strong alkalinity of the alkali metal catalyst also cause the defects of poor stability, corrosion of the ceramic DPF and the like.
Soot combustion catalysts of the K-doped type have proven to be excellent catalytic soot combustion catalysts. Compared with other alkali metal elements, the K-containing material can increase the content of chemisorbed oxygen, form low-melting-point compounds and carbonate intermediates, and show higher catalytic performance. Rich in the valence state of manganese element, MnOxThe characteristics of environmental friendliness, low toxicity, diversified morphological structures and low cost make the compound enzyme popular in various research fields. The existence of the mixed valence state of K and Mn in the cryptomelane type manganese oxide (OMS-2) catalyst enables the catalyst to have excellent ion exchange performance and good oxidation reduction performance. Loaded in 3DOM SiO2The K-OMS-2 improves the catalytic performance of the catalyst through the macroporous effect, the microporous effect and the synergistic effect between K and Mn, and the valence change of Mn species and the existence of K play a role in catalyzing soot combustion.
For the reasons, the research and development of the cryptomelane type mixed manganese oxide catalyst for removing soot of the diesel vehicle through oxidation has important economic and practical significance.
Disclosure of Invention
The invention aims to provide a cryptomelane type mixed manganese oxide catalyst for removing soot of a diesel vehicle by oxidation.
The cryptomelane type mixed manganese oxide catalyst for oxidizing and removing soot of a diesel vehicle comprises the following preparation steps:
(1) weighing appropriate amount of potassium permanganate (KMnO)4) Dissolving in 75 mL of deionized water, and marking as a solution I;
(2) weighing appropriate amount of manganese acetate (MnC)4H6O4·4H2O) is dissolved in 20 mL of deionized water and is marked as solution II;
(3) mixing the solution II with 42 mL of acetic acid solution (6 wt.%) under stirring, and then adding the solution I dropwise;
(4) and (4) heating, refluxing, washing, drying and calcining the mixed product obtained in the step (3) at a certain temperature. And cooling to room temperature, and taking out to obtain a sample, namely the cryptomelane type mixed manganese oxide catalyst.
The synthesized catalyst is a cryptomelane type mixed manganese oxide catalyst for removing soot of a diesel vehicle by oxidation.
KMnO synthesized by the inventionxThe catalyst has the characteristics of large specific surface area, large pore volume and a hierarchical pore structure.
The invention has the function of removing soot particles of the diesel vehicle by catalytic oxidation.
The method is simple and easy to implement, mild in preparation conditions, cheap and easily available in raw materials, and free of toxic reaction raw materials, so that the catalyst is an environment-friendly green synthetic catalyst.
Drawings
FIG. 1 shows KMnO prepared according to the present inventionxXRD pattern of catalyst.
FIG. 2 shows KMnO prepared according to the present inventionxN of catalyst2Adsorption and desorption and a pore size distribution curve map.
FIG. 3 shows KMnO prepared according to the present inventionxEDS profile of the catalyst.
FIG. 4 shows KMnOx catalyst in O prepared by the present invention2And NO + O2Soot particle catalytic oxidation pattern under atmosphere.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example one
(1) 3.25g of potassium permanganate (KMnO) is weighed4) Dissolving in 75 mL of deionized water, and marking as a solution I; 5.5g of manganese acetate (MnC) were weighed4H6O4·4H2O) is dissolved in 20 mL of deionized water and is marked as solution II;
(2) mixing the solution II with 42 mL of acetic acid solution (6 wt.%) under stirring, and then adding the solution I dropwise;
(3) and (3) heating and refluxing the mixed solution obtained in the step (2) at 50 ℃ while stirring for 36 hours. Washed with absolute ethanol and deionized water sequentially, dried at 80 ℃ overnight, and finally calcined at 550 ℃ for 5 h. And cooling to room temperature, and taking out to obtain a sample, namely the cryptomelane type mixed manganese oxide catalyst, which is called KMnOx for short.
Example two
Fig. 1 is an XRD spectrum of the prepared sample. XRD analysis found that the KMnO preparedxIs prepared from cryptomelane (K)2-xMn8O16) And Mn2O3The formed mixed manganese oxide.
Example three
The specific surface area, pore size distribution and pore volume of the catalyst were measured on a fully automated specific surface area and porosity analyzer, model ASAP 2460, manufactured by Micromeritics, usa. KMnOxN of the sample2The adsorption-desorption curve follows the type II isotherm in IUPAC, is accompanied by a type H3 hysteresis loop in the relatively high pressure region, and is at P/P0No adsorption limitation occurred near 1, indicating the presence of a slit-shaped macroporous structure in the sample. Specific surface area (S) of sampleBET) Pore volume (V)p) And average pore diameter (D)p) Are respectively 42.6 m2/g、0.21 cm3G and 35.6 nm. As can be seen from the pore size distribution curve (fig. 2), the sample has a hierarchical pore structure having micropores, mesopores, and macropores, and the proportions thereof are 2%, 55%, and 43%, respectively.
Example four
To obtain elemental information for the catalyst, the amount of surfacial elements in the sample was determined by EDS. FIG. 3 demonstrates the presence of Mn, O and K components in the sample.
Practice five
The cryptomelane type mixed manganese oxide catalysts prepared in the above embodiments are respectively taken to simulate the exhaust gas atmosphere of a diesel vehicle, Printex-U carbon black of Degussa company of Germany is used for replacing soot particles discharged by a diesel engine, and the soot catalytic combustion activity of the catalysts is evaluated by adopting a temperature programming oxidation technology. As shown in FIG. 4, at O2Under the atmosphere, measuring the ignition temperature of soot combustion on the catalyst according to the soot combustion reaction conversion rate curveThe temperature is generally 400-430 ℃ to generate CO2The selectivity of the catalyst reaches 100 percent, and CO is not generated. In NO + O2In the atmosphere, the ignition temperature for catalyzing soot combustion on the catalyst is reduced to 300-330 ℃ to generate CO2The selectivity of the catalyst also reaches 100 percent, and no CO is generated. The catalyst prepared by the method has good catalytic activity and high selectivity, and the external factor is KMnOxThe multistage pore structure, especially the macroporous structure, is favorable for the contact of the catalyst and the soot. One aspect of the intrinsic factor is KMnOxStrong oxidation-reduction capability of the catalyst; on the other hand, the promoting effect of the basic metal K.
Claims (8)
1. A preparation method of cryptomelane type mixed manganese oxide catalyst for removing soot of diesel vehicles by oxidation is characterized by comprising the following steps:
(1) weighing a certain amount of potassium permanganate (KMnO)4) Dissolved in deionized water and stirred until completely dissolved, and is marked as solution I.
2. (2) weighing a certain amount of manganese acetate (MnC)4H6O4·4H2O) is dissolved in deionized water and stirred until completely dissolved, and is marked as solution II.
3, (3) first, the solution II is mixed with acetic acid solution (CH)3COOH), stirring continuously, and then adding the solution i dropwise.
4, (4) heating and refluxing the mixed product obtained in the step (3) at a certain temperature, and stirring simultaneously; then washing with absolute ethyl alcohol and deionized water, drying and calcining at high temperature to finally obtain the cryptomelane type mixed manganese oxide catalyst for oxidizing the carbon smoke particles of the diesel vehicle.
5. The preparation method of the cryptomelane type mixed manganese oxide catalyst for removing soot of the diesel vehicle by oxidation according to claim 1, is characterized in that: the concentration of the potassium permanganate solution is 1.0-2.0 mol/L.
6. The method for preparing the cryptomelane type mixed manganese oxide catalyst for removing soot from diesel vehicles by oxidation according to claim 1, wherein in the step (4), the washed precipitated product is dried at 60-100 ℃ for 48h while the precipitated product is dried; in calcining the precipitated product, the dried precipitated product is calcined at 500-600 ℃ for at least 3 hours.
7. The preparation method of the cryptomelane type mixed manganese oxide catalyst for removing soot of the diesel vehicle by oxidation according to claim 1, is characterized in that: the molar ratio of potassium permanganate to manganese acetate is 1-2.
8. The preparation method of the cryptomelane type mixed manganese oxide catalyst for removing soot of the diesel vehicle by oxidation according to claim 1, is characterized in that: the prepared catalyst has the function of catalyzing and oxidizing the soot of the diesel vehicle with high activity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112371121A (en) * | 2020-12-01 | 2021-02-19 | 吉林大学 | Catalyst for eliminating formaldehyde and carbon monoxide at room temperature and preparation method thereof |
| CN114733514A (en) * | 2022-03-01 | 2022-07-12 | 沈阳师范大学 | Monolithic catalyst containing cryptomelane type potassium-manganese composite oxides with different morphologies as well as preparation method and application of monolithic catalyst |
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| CN109589968A (en) * | 2018-12-19 | 2019-04-09 | 沈阳师范大学 | Three-dimensional ordered macroporous-meso titanium silica the composite oxide carrier of one kind supports K-OMS-2 catalyst and preparation method thereof |
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2020
- 2020-08-04 CN CN202010769835.9A patent/CN111889100A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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Application publication date: 20201106 |