CN109317145A - A kind of Mn oxide noble metal composite catalyst, preparation method and applications - Google Patents
A kind of Mn oxide noble metal composite catalyst, preparation method and applications Download PDFInfo
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- CN109317145A CN109317145A CN201811346739.2A CN201811346739A CN109317145A CN 109317145 A CN109317145 A CN 109317145A CN 201811346739 A CN201811346739 A CN 201811346739A CN 109317145 A CN109317145 A CN 109317145A
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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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/656—Manganese, technetium or rhenium
- B01J23/6562—Manganese
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G2209/00—Specific waste
- F23G2209/14—Gaseous waste or fumes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention belongs to air purification field, it is related to a kind of Mn oxide noble metal composite catalyst, preparation method and applications.The present invention provides a kind of preparation methods of Mn oxide noble metal composite catalyst, comprising the following steps: step 1: precious metal catalyst agent carrier first being impregnated in stannous chloride solution, then is impregnated in palladium chloride solution;Step 2: the precious metal catalyst agent carrier that step 1 obtains being put into Mn oxide precursor solution and carries out hydro-thermal reaction;Step 3: the precious metal catalyst agent carrier after hydro-thermal reaction is put into heating water bath, drying in palladium precursor solution;The Mn oxide precursor solution includes potassium permanganate;The palladium precursor solution includes palladium chloride solution.The present invention also provides a kind of Mn oxide noble metal composite catalyst and its application, the present invention solves the technical problem that can not keep catalyst superior VOCs low temperature purification activity while effectively reducing noble metal dosage in the prior art.
Description
Technical field
The invention belongs to air purification field, be related to a kind of Mn oxide noble metal composite catalyst, preparation method and
It is applied.
Background technique
In the method that volatile organic matter (VOCs) is effectively treated, catalytic oxidation combustion method is concerned, and has place
The advantages that VOCs type is extensive, purification rate is fast and treatment effeciency is high is managed, and final product is CO2And water, it not will cause secondary
Pollution.The core of this method is catalyst, wherein cellular integrated combustion catalyst due to, treating capacity low with pressure drop is big,
The features such as mechanical and thermal stability is high, current application is the most extensive.Different main points by active component type of integral catalyzer
For two class of noble metal monolithic catalyst and base metal integral catalyzer.Noble metal monolithic catalyst possesses initiation temperature
The low and high-efficient advantage of low-temperature catalytic oxidation, but it is expensive, how noble metal is reduced on the basis of keeping catalytic activity use
Amount is always the research emphasis of such catalyst.Base metal integral catalyzer has cheap and thermodynamic property good
Advantage, especially manganese oxide catalyst, since its intracell has a large amount of variable valence manganese ions, so also having superior
Oxygen uptake and for oxygen characteristic.But the low-temperature catalytic oxidation activity of base metal integral catalyzer is poor, again limits it in VOCs
The popularization and application of field of purification.Therefore, catalyst can not be kept excellent while effectively reducing noble metal dosage in the prior art
VOCs low temperature purification activity more becomes those skilled in the art's technical problem urgently to be resolved.
Summary of the invention
The present invention provides a kind of Mn oxide noble metal composite catalyst, preparation method and applications, solve existing
Catalyst superior VOCs low temperature purification active technology can not be kept while effectively reducing noble metal dosage by having in technology
Problem.
The present invention provides a kind of preparation methods of Mn oxide noble metal composite catalyst, comprising the following steps:
Step 1: catalyst carrier first being impregnated in stannous chloride solution, then is impregnated in palladium chloride solution;
Step 2: the catalyst carrier that step 1 is obtained is put into Mn oxide precursor solution and carries out hydro-thermal reaction;
Step 3: the catalyst carrier after hydro-thermal reaction is put into heating water bath, drying in palladium precursor solution;
The Mn oxide precursor solution includes potassium permanganate;
The palladium precursor solution includes palladium chloride solution.
It should be noted that the solvent of the Mn oxide precursor solution and palladium precursor solution is water.
Preferably, the catalyst carrier is ceramic honey comb or cellular activated carbon.
Preferably, the concentration of the stannous chloride solution is 8-12g/L.
It is furthermore preferred that the time impregnated in the stannous chloride solution is 5-15min.
Preferably, the concentration of palladium chloride solution described in step 1 is 0.02-0.05g/L.
It is furthermore preferred that the time impregnated in the palladium chloride solution in step 1 is 5-15min.
Preferably, the temperature of hydro-thermal reaction described in step 2 is 90-120 DEG C.
It is furthermore preferred that the time of hydro-thermal reaction described in step 2 is 12-24h.
It is furthermore preferred that the temperature of heating water bath described in step 3 is 50-80 DEG C.
It is furthermore preferred that the time of heating water bath described in step 3 is 2-4h.
Preferably, the concentration of the liquor potassic permanganate is 0.05-0.15mol/L.
It is furthermore preferred that the Mn oxide precursor solution further includes acetic acid.
It is furthermore preferred that the concentration of the acetum is 0-0.3mol/L.
Preferably, the concentration of palladium chloride solution described in step 3 is 0.02-0.04g/L.
It is furthermore preferred that the palladium precursor solution further includes sodium hypophosphite, ammonium chloride and ammonium hydroxide.
It is furthermore preferred that the concentration of the ortho phosphorous acid sodium solution is 5.0g/L, the concentration of the ammonium chloride solution is
13.5g/L。
The present invention also provides a kind of Mn oxide noble metal composite catalysts, compound by above-mentioned Mn oxide noble metal
The preparation method of type catalyst is made.
The present invention also provides a kind of Mn oxide noble metal composite catalysts as the net of volatile organic contaminant
The application of agent.
Catalyst made from the preparation method of Mn oxide noble metal composite catalyst provided by the invention, can make expensive
Two kinds of active components of Metal Palladium and Mn oxide are uniformly interspersed in the regular carrier surface of honeycomb, are urged using the collaboration of the two
Change effect, in the catalyst under the conditions of palladium content very low (0.06-0.10wt.%), that is, it is low-temperature catalyzed to show superior VOCs
Burning purifying property: in 160-226 DEG C of ignition, reach at 236-270 DEG C and be fully cleaned up.And preparation method provided by the invention
Easy to operate, gained catalyst prod is cheap and the active height of catalytic purification, has good market application value and popularization
Prospect.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is the EDS surface-element analysis chart of 1 gained catalyst sample of the embodiment of the present invention;
Fig. 2 is the SEM surface topography map of 1 gained catalyst sample of the embodiment of the present invention;
Fig. 3 is the EDS surface-element analysis chart of 4 gained catalyst sample of the embodiment of the present invention;
Fig. 4 is the SEM surface topography map of 4 gained catalyst sample of the embodiment of the present invention.
Specific embodiment
The embodiment of the invention provides a kind of Mn oxide noble metal composite catalyst, preparation method and applications, solutions
Catalyst superior VOCs low temperature purification activity can not be kept while effectively reducing noble metal dosage in the prior art by having determined
The technical issues of.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention
Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below
Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field
Those of ordinary skill's all other embodiment obtained without making creative work, belongs to protection of the present invention
Range.
In order to further illustrate the present invention, following embodiment is enumerated, but is not intended to limit the scope of the invention.
Embodiment 1
By the regular substrate of the ceramic honey comb of 5 × 5 × 24mm of 0.37g, first room temperature is soaked in the stannous chloride solution of 10g/L
Stain 10min, then the room temperature immersion 10min in the palladium chloride solution of 0.03g/L then take out and are rinsed with water completely;It will pretreatment
Regular substrate afterwards is put into Mn oxide precursor solution (by the preparation of 0.10mol/L potassium permanganate, 0.1mol/L acetic acid and water
At), and be transferred in hydrothermal reaction kettle together, in 100 DEG C of sustained response 20h;Before regular substrate after hydro-thermal reaction is put into palladium
Drive liquid solution (by 0.02g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100mL/L 25% ammonium hydroxide and water
It is formulated) in, the sustained response 3h under 60 DEG C of bath temperatures finally takes out after being rinsed with water completely, dry to perseverance at 120 DEG C
Weight.
Embodiment 2
By the regular substrate of ceramic honey comb of 5 × 5 × 24mm size of 0.37g, the first room in the stannous chloride solution of 8g/L
Temperature dipping 15min, then the room temperature immersion 15min in the palladium chloride solution of 0.02/L, then take out and are rinsed with water completely;It will locate in advance
Regular substrate after reason is put into Mn oxide precursor solution (being formulated by 0.05mol/L potassium permanganate and water), and together
Be transferred in hydrothermal reaction kettle, 90 DEG C of sustained responses for 24 hours;By the regular substrate after hydro-thermal reaction be put into palladium precursor solution (by
0.04g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 25% ammonium hydroxide of 100mL/L and water are formulated)
In, the sustained response 2h under 80 DEG C of bath temperatures finally takes out after being rinsed with water completely, dry to constant weight at 120 DEG C.
Embodiment 3
By the regular substrate of ceramic honey comb of 5 × 5 × 24mm size of 0.37g, the first room in the stannous chloride solution of 12g/L
Temperature dipping 5min, then the room temperature immersion 5min in the palladium chloride solution of 0.05/L, then take out and are rinsed with water completely;It will pretreatment
Regular substrate afterwards is put into Mn oxide precursor solution (by the preparation of 0.15mol/L potassium permanganate, 0.3mol/L acetic acid and water
At), and be transferred in hydrothermal reaction kettle together, in 120 DEG C of sustained response 12h;Before regular substrate after hydro-thermal reaction is put into palladium
Drive liquid solution (by 0.03g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100mL/L 25% ammonium hydroxide and water
It is formulated) in, the sustained response 4h under 50 DEG C of bath temperatures finally takes out after being rinsed with water completely, dry to perseverance at 120 DEG C
Weight.
Embodiment 4
By the regular substrate of cellular activated carbon of 5 × 5 × 24mm size of 0.42g, first in the stannous chloride solution of 10g/L
Room temperature immersion 10min, then the room temperature immersion 10min in the palladium chloride solution of 0.03/L then take out and are rinsed with water completely;It will be pre-
Regular substrate that treated is put into Mn oxide precursor solution and (is matched by 0.1mol/L potassium permanganate, 0.1mol/L acetic acid and water
Make), and be transferred in hydrothermal reaction kettle together, in 100 DEG C of sustained response 18h;Regular substrate after hydro-thermal reaction is put into
Palladium precursor solution (by 0.03g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 100mL/L 25% ammonium hydroxide
It is formulated with water) in, the sustained response 2h under 70 DEG C of bath temperatures finally takes out after being rinsed with water completely, in 120 DEG C of dryings
To constant weight.
Embodiment 5
By the regular substrate of cellular activated carbon of 5 × 5 × 24mm size of 0.42g, first in the stannous chloride solution of 8g/L
Room temperature immersion 15min, then the room temperature immersion 10min in the palladium chloride solution of 0.03/L then take out and are rinsed with water completely;It will be pre-
Regular substrate that treated is put into Mn oxide precursor solution (being formulated by 0.05mol/L potassium permanganate and water), and one
Rise be transferred in hydrothermal reaction kettle, 90 DEG C of sustained responses for 24 hours;Regular substrate after hydro-thermal reaction is put into palladium precursor solution
(by the preparation of 0.04g/L palladium chloride, 5.0g/L sodium hypophosphite, 13.5g/L ammonium chloride, 25% ammonium hydroxide of 100mL/L and water
At) in, the sustained response 2h under 80 DEG C of bath temperatures finally takes out after being rinsed with water completely, dry to constant weight at 120 DEG C.
In conclusion carrying out surface-element analysis to catalyst made from embodiment 1 using EDS characterization technique, Fig. 1 is real
The EDS surface-element analysis chart of 1 gained catalyst sample of example is applied, as shown in Figure 1, in addition to tetra- kinds of ceramic bases of Si, Mg, Al and O
Outside element, it can also be observed that the presence of Mn and Pd element, thus proves to use in-situ self-grown provided in an embodiment of the present invention
The Mn oxide method mutually compound with auto-deposition precious metal palladium technology in situ, can bear two kinds of active components of Mn oxide and palladium
It is loaded in ceramic honey comb substrate surface.The SEM surface topography map of catalyst made from the position Fig. 2 embodiment 1, as shown in Figure 2, manganese oxidation
Object and precious metal palladium active component are uniformly distributed in ceramic honey comb substrate surface with near-spherical particle.By embodiment 2 and embodiment 3
Catalyst sample is made and carries out EDS elemental analysis and SEM Analysis of Surface Topography, obtained result and 1 gained catalyst of embodiment
The analysis result of sample is similar.
Catalyst is made in embodiment 4 and carries out the analysis of EDS surface-element, as a result such as Fig. 3, in addition to active carbon base metals C,
Outside Si, Al and O, it can also be observed that the presence of Mn and Pd element, thus prove to use this patent preparation method, it really can be
Two kinds of active components of Mn oxide and palladium are supported on cellular activated carbon substrate surface.Fig. 4 is the SEM that catalyst is made in embodiment 4
Surface topography map, Mn oxide and precious metal palladium active component are uniformly divided in cellular activated carbon substrate surface with near-spherical particle
Cloth.It chooses 5 gained catalyst sample of embodiment and carries out EDS elemental analysis and SEM Analysis of Surface Topography, obtained result and implementation
The analysis result of 4 gained catalyst sample of example is similar.
The EDS surface-element analysis result of the catalyst sample obtained by embodiment 1-5 can calculate each catalyst sample
The mass content of precious metal palladium in product, as shown in table 1.
By catalyst sample made from embodiment 1-5, purified using toluene catalytic combustion as probe reaction, in toluene sample introduction
Concentration is 1.0g/m3With volume space velocity 10000h-1Under the conditions of carry out catalyst activity evaluation, the results are shown in Table 1.Catalyst activity with
Reaction temperature T when toluene conversion is respectively 10%, 50% and 90%10、T50And T90As evaluation criterion, temperature value is got over
It is low to show that catalyst cleaning activity is more excellent.As shown in Table 1, very low (0.06-0.10wt.%) condition of palladium content in the catalyst
Under, it can be in 160-226 DEG C of low temperature ignition, and reach at 236-270 DEG C and be fully cleaned up, show superior toluene catalytic combustion
Purifying property.This should be attributed to the fact that using in the resulting compound monoblock type combustion catalyst of this patent preparation method, noble metal
Two kinds of active components of palladium and Mn oxide can uniformly be interspersed in the regular carrier surface of honeycomb, to more favorably play manganese oxygen
The oxygen uptake of compound and for oxygen characteristic, the low-temperature oxidation activity of precious metal palladium is effectively promoted by concerted catalysis.
The toluene burning purification activity of catalyst is made in 1 Examples 1 to 5 of table
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features;And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of Mn oxide noble metal composite catalyst, which comprises the following steps:
Step 1: catalyst carrier first being impregnated in stannous chloride solution, then is impregnated in palladium chloride solution;
Step 2: the catalyst carrier that step 1 is obtained is put into Mn oxide precursor solution and carries out hydro-thermal reaction;
Step 3: the catalyst carrier after hydro-thermal reaction is put into heating water bath, drying in palladium precursor solution;
The Mn oxide precursor solution includes potassium permanganate;
The palladium precursor solution includes palladium chloride solution.
2. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that described
Catalyst carrier is ceramic honey comb or cellular activated carbon.
3. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that described
The concentration of stannous chloride solution is 8-12g/L.
4. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that step
The concentration of palladium chloride solution described in 1 is 0.02-0.05g/L.
5. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that step
The temperature of hydro-thermal reaction described in 2 is 90-120 DEG C.
6. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that step
The temperature of heating water bath described in 3 is 50-80 DEG C.
7. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that described
The concentration of liquor potassic permanganate is 0.05-0.15mol/L in Mn oxide precursor solution, and the concentration of acetum is 0-
0.3mol/L。
8. the preparation method of Mn oxide noble metal composite catalyst according to claim 1, which is characterized in that described
The concentration of palladium chloride solution is 0.02-0.04g/L in palladium precursor solution, and the concentration of ortho phosphorous acid sodium solution is 5.0g/L, chlorine
The concentration for changing ammonium salt solution is 13.5g/L.
9. a kind of Mn oxide noble metal composite catalyst, which is characterized in that as described in claim 1~8 any one
The preparation method of Mn oxide noble metal composite catalyst is made.
10. Mn oxide noble metal composite catalyst according to claim 9 is as the net of volatile organic contaminant
The application of agent.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113477246A (en) * | 2021-06-30 | 2021-10-08 | 广东工业大学 | Manganese-containing integral electrically-assisted metal honeycomb catalyst and preparation method and application thereof |
CN113680390A (en) * | 2021-07-29 | 2021-11-23 | 佛山市顺德区金磊环保科技有限公司 | Foam material with formaldehyde purification function and preparation method and application thereof |
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CN101811046A (en) * | 2010-04-30 | 2010-08-25 | 华南理工大学 | Noble metal monolithic catalyst for purifying organic waste gas and preparation method thereof |
CN101829568A (en) * | 2010-05-07 | 2010-09-15 | 广东工业大学 | Preparation method of manganese oxide in-situ doping type palladium-based monolithic catalyst and application thereof |
CN102000570A (en) * | 2010-10-11 | 2011-04-06 | 广东工业大学 | Pd/Ce0.8Zr0.2O2/cordierite honeycomb ceramic monolithic catalyst, preparation method and application thereof |
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CN101811046A (en) * | 2010-04-30 | 2010-08-25 | 华南理工大学 | Noble metal monolithic catalyst for purifying organic waste gas and preparation method thereof |
CN101829568A (en) * | 2010-05-07 | 2010-09-15 | 广东工业大学 | Preparation method of manganese oxide in-situ doping type palladium-based monolithic catalyst and application thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN113477246A (en) * | 2021-06-30 | 2021-10-08 | 广东工业大学 | Manganese-containing integral electrically-assisted metal honeycomb catalyst and preparation method and application thereof |
CN113477246B (en) * | 2021-06-30 | 2023-08-01 | 广东工业大学 | Manganese-containing integral electric auxiliary metal honeycomb catalyst and preparation method and application thereof |
CN113680390A (en) * | 2021-07-29 | 2021-11-23 | 佛山市顺德区金磊环保科技有限公司 | Foam material with formaldehyde purification function and preparation method and application thereof |
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