CN108940304A - A kind of Mn/Ce/Cu base low-temperature plasma body catalyst and preparation and application - Google Patents
A kind of Mn/Ce/Cu base low-temperature plasma body catalyst and preparation and application Download PDFInfo
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- CN108940304A CN108940304A CN201810839900.3A CN201810839900A CN108940304A CN 108940304 A CN108940304 A CN 108940304A CN 201810839900 A CN201810839900 A CN 201810839900A CN 108940304 A CN108940304 A CN 108940304A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/80—Employing electric, magnetic, electromagnetic or wave energy, or particle radiation
- B01D2259/818—Employing electrical discharges or the generation of a plasma
Abstract
The invention belongs to catalysis material technical field, a kind of Mn/Ce/Cu base low-temperature plasma body catalyst and preparation and application are disclosed.Manganese Metal salt, salt containing ce metal and copper-containing metal salt will be contained to be dissolved in DMF, addition organic ligand ultrasonic mixing is uniform, and gained mixed solution is reacted at a temperature of 80~120 DEG C, and solid product is soaked in DMF and is activated, and obtains activation crystal；Gained activation crystal is washed, dry, it is then roasted in 300~400 DEG C, obtains Mn/Ce/Cu base low-temperature plasma body catalyst.MOFs material at high temperature calcining is directly prepared the carbon-based catalysis material of nanoporous by the present invention, has many advantages, such as metal active constituent high degree of dispersion, stable structure, and it is possible to prevente effectively from metal active constituent reunion, catalytic activity and stability significantly improve.
Description
Technical field
The invention belongs to catalysis material technical fields, and in particular to a kind of Mn/Ce/Cu base low-temperature plasma body catalyst and
Preparation and application.
Background technique
Volatile organic matter (volatile organic compounds, VOCs) is many kinds of, including alkanes, alkene,
Halogenated hydrocarbons, esters, aldehydes, ketone and aromatic compound etc. are mainly derived from the industries such as medicine, petrochemical industry, printing.Big portion
Point VOCs be it is toxic, can react to form photochemical fog under light illumination, be ozone pollution and PM2.5 precursor it
One, a possibility that of will increase the diseases such as cancer, is stayed in the environment containing volatile organic matter for a long time.Therefore, carry out industrial volatility
Organic pollution, which is administered, has extremely important application value.
It is polluted effectively to administer VOCs in organic exhaust gas, the technology being widely used both at home and abroad has Production by Catalytic Combustion Process, absorption
Method, absorption process etc., there are also biofilm, photocatalytic oxidation, plasma methods etc. for the Treatment process of Recent study.Many
In VOCs Treatment process, low temperature plasma at normal temperatures and pressures can fast degradation VOCs and be concerned.However, simple
Lower temperature plasma technology energy consumption it is high, selectivity it is low, part VOCs can be produced into toxic by-product in degradation process.For
Overcome these deficiencies, low temperature plasma coupled with catalytic oxidation technologies, i.e., loads and urge in the region of discharge of plasma
Agent, under plasma and catalyst synergistic effect, the catalysis oxidation efficiency and selectivity to VOCs organic pollutant are obtained
To greatly improving.Catalyst is the core of low temperature plasma catalytic oxidation technologies, and reported catalyst has transition metal
Catalyst, noble metal catalyst etc..For example, [An H T Q, Huu T P, Van the T L, et such as H.T.Quoc An
al.Application of atmospheric non thermal plasma-catalysis hybrid system for
air pollution control:Toluene removal[J].Catalysis Today,2011,176(1):474-
477.] catalyst series containing elements such as Ag, Au, Cu, Co, Mn, La and Nb are prepared for, wherein 1% (mass fraction) Au/Al2O3
And Nb2O5Catalyst reaches 96% to the conversion ratio of toluene.The Huanghai Sea protects et al. [Long Liping, Zhao Jianguo, under the room temperature such as Yang Lixian
MnO2/Al2O3Catalyst ozone oxidation toluene reacts [J] and is catalyzed journal, 2011,32 (6): 904-916.] by TiO2/
γ-/Al2O3/ Foamed Nickel and plasma combination processing VOCs, improve the CO of product2Selectivity, but this catalyst is easy because of pair
The accumulation of product and inactivate.[Wu Junliang, Xia Qibin, Liu Zhimeng wait .Mn, Fe and Cu oxide in low-temperature plasma to Wu Junliang etc.
Expression activitiy [J] functional material in body catalysis oxidation toluene system, 2012,43 (10): 1332-1335.] metal is organic
Framework material MIL-101 and plasma combination processing toluene, the conversion ratio of toluene reach 100%, CO2Selectivity reaches
70%, byproduct of reaction can be substantially reduced.Since MOFs skeleton itself has (including the thermostabilization of relatively poor stability
Property, chemical stability etc.), so its industrial application is greatly limited.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of Mn/
The preparation method of Ce/Cu base low-temperature plasma body catalyst.
Another object of the present invention is to provide a kind of Mn/Ce/Cu base low temperature being prepared by the above method etc. from
Daughter catalyst.
A further object of the present invention is to provide above-mentioned Mn/Ce/Cu base low-temperature plasma body catalysts in low-temperature plasma
Application in body catalyzing oxidizing degrading VOCs.
Another object of the present invention is to provide application among the above.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst, including following preparation step:
(1) manganese Metal salt, salt containing ce metal and copper-containing metal salt will be contained to be dissolved in DMF, organic ligand ultrasonic mixing is added
Uniformly, mixed solution is obtained；
(2) mixed solution obtained by step (1) is reacted at a temperature of 80~120 DEG C, solid product is soaked in DMF
It is activated, obtains activation crystal；
(3) activation crystal obtained by step (2) is washed, dry, it is then roasted in 300~400 DEG C, obtains Mn/Ce/Cu
Base low-temperature plasma body catalyst.
Further, salt containing manganese Metal described in step (1) in manganese nitrate, manganese sulfate, manganese carbonate, manganese acetate extremely
Few one kind；The salt containing ce metal is selected from least one of cerous nitrate, cerous sulfate, cerous carbonate, cerous acetate；The copper-containing metal
Salt is selected from least one of copper nitrate, copper sulphate.
Further, the dosage of salt containing manganese Metal, salt containing ce metal and copper-containing metal salt described in step (1) is according to manganese member
The molar ratio of element, Ce elements and copper is 1:2:(1~2).More preferably 1:2:1,1:2:1.5 or 1:2:2.
Further, organic ligand described in step (1) is selected from formic acid or acetic acid, more preferably formic acid.
Further, the dosage of organic ligand described in step (1) and the molar ratio of the manganese element in salt containing manganese Metal are
1:(5.8~9)；More preferably 1:5.8,1:7.2 or 1:9.
Further, the time of reaction described in step (2) is 10~15h.
Further, be soaked in described in step (2) time for being activated in DMF be 12~for 24 hours.
Further, roasting described in step (3) is to be roasted in air atmosphere, and calcining time is 2~3h.
A kind of Mn/Ce/Cu base low-temperature plasma body catalyst, is prepared by the above method.
Above-mentioned Mn/Ce/Cu base low-temperature plasma body catalyst answering in low temperature plasma catalyzing oxidizing degrading VOCs
With.
The principle of the present invention are as follows: directly by the high-temperature calcination under certain air atmosphere of MOFs material, organic ligand is carbonized,
Obtain the carbon-based catalysis material of nanoporous.The carbonization MOFs base catalysis material of this method preparation is with metal active constituent height point
It dissipating, the advantages that stable structure, and it is possible to prevente effectively from metal active constituent is reunited, catalytic activity and stability are significantly improved,
It is novel based on carbonization Mn/Ce/Cu base MOF catalysis material to can be used as one kind, is applied to low temperature plasma catalysis oxidation VOCs
In system, it can be achieved that under normal temperature and pressure conditions to the efficient removal of VOCs.
Preparation method of the invention and obtained product have the following advantages that and the utility model has the advantages that
(1) compared with traditional supported catalysts, catalyst of the invention has metal active constituent high degree of dispersion, hole
The characteristics of rate height, stable structure, makes it have high catalysis oxygen to VOCs such as toluene it is possible to prevente effectively from metal active constituent is reunited
Change activity；
(2) raw material that preparation method of the present invention uses is cheap and easily-available, and preparation method is simple, is conducive to industrialization and answers on a large scale
With；
(3) compared with existing catalysis technique, catalyst of the invention and plasma device combination can be at normal temperatures and pressures
Quick catalysis aoxidizes toluene, and the conversion ratio of toluene can reach 100%, CO2Selectivity up to 88%.
Detailed description of the invention
Fig. 1 is the XRD diagram of 1~3 gained Mn/Ce/Cu base low-temperature plasma body catalyst of the embodiment of the present invention.
Fig. 2 is 1~3 gained Mn/Ce/Cu base low-temperature plasma body catalyst of the embodiment of the present invention in different plasma energy
Toluene conversion figure under metric density.
Fig. 3 is 1~3 gained Mn/Ce/Cu base low-temperature plasma body catalyst of the embodiment of the present invention in different plasma energy
CO under metric density2Selective figure.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) Mn (NO for being 50% by the mass concentration of 520 μ L3)2Aqueous solution, 1.94gCe (NO3)3·6H2O and 0.54gCu
(NO3)2·3H2O is added in 80mLDMF, and 1000 μ L formic acid are added, and ultrasonic 10min is uniformly mixed, and obtains mixed solution；
(2) mixed solution 80 DEG C of baking oven reaction 10h are placed in remove supernatant after solution is cooling, fresh DMF is added,
Soaking at room temperature activates 12h, and activation crystalline material (Mn/Ce/Cu-MOF) is made；
(3) activation crystalline material is washed with DMF, filters, filtered material is put into 50 DEG C of vacuum drying ovens and is dried；
Crystalline material after drying is put into 300 DEG C of roasting 2h in Muffle furnace, Mn/Ce/Cu base low-temperature plasma body catalyst is made.
Embodiment 2
(1) Mn (NO for being 50% by the mass concentration of 520 μ L3)2Aqueous solution, 1.94gCe (NO3)3·6H2O and 0.81gCu
(NO3)2·3H2O is added in 80mLDMF, and 1200 μ L formic acid are added, and ultrasonic 10min is uniformly mixed, and obtains mixed solution；
(2) mixed solution is placed in 100 DEG C of baking oven reaction 12h and removes supernatant after solution is cooling, be added fresh
DMF, soaking at room temperature activate 18h, and activation crystalline material (Mn/Ce/Cu-MOF) is made；
(3) activation crystalline material is washed with DMF, filters, filtered material is put into 50 DEG C of vacuum drying ovens and is dried；
Crystalline material after drying is put into 350 DEG C of roasting 2.5h in Muffle furnace, the catalysis of Mn/Ce/Cu base low temperature plasma is made
Agent.
Embodiment 3
(1) Mn (NO for being 50% by the mass concentration of 520 μ L3)2Aqueous solution, 1.94gCe (NO3)3·6H2O and 1.08gCu
(NO3)2·3H2O is added in 80mLDMF, and 1500 μ L formic acid are added, and ultrasonic 10min is uniformly mixed, and obtains mixed solution；
(2) mixed solution is placed in 120 DEG C of baking oven reaction 15h and removes supernatant after solution is cooling, be added fresh
DMF, soaking at room temperature activate for 24 hours, and activation crystalline material (Mn/Ce/Cu-MOF) is made；
(3) activation crystalline material is washed with DMF, filters, filtered material is put into 50 DEG C of vacuum drying ovens and is dried；
Crystalline material after drying is put into 400 DEG C of roasting 3h in Muffle furnace, Mn/Ce/Cu base low-temperature plasma body catalyst is made.
The characterization and performance measurement of catalyst sample obtained by above embodiments:
(1) X-ray diffraction analysis
Using German Bruker company D8-ADVANCE type X-ray diffractometer, operating condition is copper target, 40KV, 40mA, step
It is 0.02 degree long, 17.7 seconds/step of scanning speed.Respectively to Mn/Ce/Cu base low-temperature plasma body catalyst prepared by example 1~3
It is characterized.
Fig. 1 is the XRD spectrum of Mn/Ce/Cu base low-temperature plasma body catalyst prepared by the embodiment of the present invention 1~3.By
For Fig. 1 as it can be seen that three kinds of catalyst all have identical XRD spectra, characteristic peak positions are identical, and peak width is wider, illustrate Examples 1 to 3
Final catalyst is synthesized.
(2) catalytic oxidation performance is tested
In Example 1~3 then gained Mn/Ce/Cu base low-temperature plasma body catalyst, pressure surface cross 40~60 mesh respectively
Sieve, is loaded among scan plasma device.Active testing condition is as follows: reaction temperature is 35 DEG C, and reaction pressure is normal pressure,
Total gas flow rate is 100mL/min, and toluene concentration 30ppm, carrier gas is dry air.Toluene concentration and CO2Concentration passes through gas phase
Chromatography detection.
Fig. 2 is toluene conversion of 1~3 gained catalyst of the embodiment of the present invention under different plasma energy density
Figure.Wherein the catalyst in embodiment 2 has best degradation of toluene ability, and degradation rate reaches when energy density is 294J/L
100%.
Fig. 3 is CO of 1~3 gained catalyst of the embodiment of the present invention under different plasma energy density2Selective figure.
It can be seen from the figure that with the increase of energy density, CO2Selectivity increases therewith, when energy density is 294J/L, embodiment
Catalyst in 2 has best CO2Selectivity, CO2Selectivity reaches 88%.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst, it is characterised in that including following preparation step:
(1) manganese Metal salt, salt containing ce metal and copper-containing metal salt will be contained to be dissolved in DMF, addition organic ligand ultrasonic mixing is uniform,
Obtain mixed solution；
(2) mixed solution obtained by step (1) is reacted at a temperature of 80~120 DEG C, solid product is soaked in DMF and carries out
Activation, obtains activation crystal；
(3) activation crystal obtained by step (2) is washed, dry, it is then roasted in 300~400 DEG C, it is low to obtain Mn/Ce/Cu base
Isothermal plasma catalyst.
2. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: salt containing manganese Metal described in step (1) is selected from least one of manganese nitrate, manganese sulfate, manganese carbonate, manganese acetate；It is described to contain
Ce metal salt is selected from least one of cerous nitrate, cerous sulfate, cerous carbonate, cerous acetate；The copper-containing metal salt be selected from copper nitrate,
At least one of copper sulphate.
3. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: the dosage of salt containing manganese Metal, salt containing ce metal and copper-containing metal salt described in step (1) is according to manganese element, Ce elements and copper
The molar ratio of element is 1:2:(1~2).
4. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: organic ligand described in step (1) is selected from formic acid or acetic acid.
5. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: the molar ratio of the manganese element in the dosage of organic ligand described in step (1) and salt containing manganese Metal is 1:(5.8~9).
6. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: the time of reaction described in step (2) is 10~15h.
7. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: be soaked in described in step (2) time for being activated in DMF be 12~for 24 hours.
8. a kind of preparation method of Mn/Ce/Cu base low-temperature plasma body catalyst according to claim 1, feature exist
In: roasting is to be roasted in air atmosphere described in step (3), and calcining time is 2~3h.
9. a kind of Mn/Ce/Cu base low-temperature plasma body catalyst, it is characterised in that: by described in any one of claim 1~8
Method be prepared.
10. Mn/Ce/Cu base low-temperature plasma body catalyst as claimed in claim 9 is in low temperature plasma catalyzing oxidizing degrading
Application in VOCs.
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Cited By (10)
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| CN110465301A (en) * | 2019-08-23 | 2019-11-19 | 四川省达科特能源科技股份有限公司 | A kind of activated-carbon catalyst and its preparation method and application |
| CN110586065A (en) * | 2019-09-20 | 2019-12-20 | 天津大学 | Synthesis method and application of novel metal oxide catalyst derived from metal organic framework |
| CN110947394A (en) * | 2019-11-15 | 2020-04-03 | 华南理工大学 | ZIF-67-Mn/Co-based low-temperature NO oxidation catalyst, and preparation method and application thereof |
| CN112452129A (en) * | 2020-12-14 | 2021-03-09 | 苏州大学 | Ternary NiO nanosheet @ bimetal CeCuOxMethod for low-temperature heat treatment of toluene by using microchip core-shell structure composite material |
| CN112452335A (en) * | 2020-12-14 | 2021-03-09 | 苏州大学 | Ternary NiO nano sheet @ bimetal CeCuOxMicro-sheet core-shell structure composite material and preparation and application thereof |
| CN112499685A (en) * | 2020-11-26 | 2021-03-16 | 南昌航空大学 | Preparation of MnO2Method for preparing @ porous carbon composite wave-absorbing material |
| CN112973673A (en) * | 2021-02-03 | 2021-06-18 | 中国科学院合肥物质科学研究院 | Manganese-cerium oxide material with adjustable oxygen vacancy as well as preparation method and application thereof |
| CN114388828A (en) * | 2021-12-29 | 2022-04-22 | 天津大学 | Alloy nanocrystal, carbon cloth loaded with alloy nanocrystal, preparation method and application |
| CN114405519A (en) * | 2021-12-30 | 2022-04-29 | 广东省科学院化工研究所 | Solid acid-bimetal nanoparticle composite material and preparation method and application thereof |
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| CN110586065A (en) * | 2019-09-20 | 2019-12-20 | 天津大学 | Synthesis method and application of novel metal oxide catalyst derived from metal organic framework |
| CN110947394A (en) * | 2019-11-15 | 2020-04-03 | 华南理工大学 | ZIF-67-Mn/Co-based low-temperature NO oxidation catalyst, and preparation method and application thereof |
| CN112499685B (en) * | 2020-11-26 | 2023-02-10 | 南昌航空大学 | Preparation of MnO 2 Method for preparing @ porous carbon composite wave-absorbing material |
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| CN112452335B (en) * | 2020-12-14 | 2022-04-15 | 苏州大学 | Ternary NiO nano sheet @ bimetal CeCuOxMicro-sheet core-shell structure composite material and preparation and application thereof |
| CN112973673A (en) * | 2021-02-03 | 2021-06-18 | 中国科学院合肥物质科学研究院 | Manganese-cerium oxide material with adjustable oxygen vacancy as well as preparation method and application thereof |
| CN114388828A (en) * | 2021-12-29 | 2022-04-22 | 天津大学 | Alloy nanocrystal, carbon cloth loaded with alloy nanocrystal, preparation method and application |
| CN114388828B (en) * | 2021-12-29 | 2023-08-22 | 天津大学 | Alloy nanocrystalline, carbon cloth loaded with alloy nanocrystalline, preparation method and application |
| CN114405519A (en) * | 2021-12-30 | 2022-04-29 | 广东省科学院化工研究所 | Solid acid-bimetal nanoparticle composite material and preparation method and application thereof |
| CN114405519B (en) * | 2021-12-30 | 2023-12-05 | 广东省科学院化工研究所 | Solid acid-bimetallic nanoparticle composite material and preparation method and application thereof |
| CN114772677A (en) * | 2022-05-23 | 2022-07-22 | 常州大学 | Plasma microbubble wastewater purification device and method |
| CN114772677B (en) * | 2022-05-23 | 2023-11-28 | 常州大学 | Plasma microbubble wastewater purification device and method |
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