CN108940304B - Mn/Ce/Cu-based low-temperature plasma catalyst and preparation and application thereof - Google Patents
Mn/Ce/Cu-based low-temperature plasma catalyst and preparation and application thereof Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- 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
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- 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
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Abstract
The invention belongs to the technical field of catalytic materials, and discloses a Mn/Ce/Cu-based low-temperature plasma catalyst, and preparation and application thereof. Dissolving manganese-containing metal salt, cerium-containing metal salt and copper-containing metal salt in DMF, adding an organic ligand, carrying out ultrasonic mixing uniformly, reacting the obtained mixed solution at the temperature of 80-120 ℃, and soaking a solid product in DMF for activation to obtain an activated crystal; and washing and drying the obtained activated crystal, and then roasting at 300-400 ℃ to obtain the Mn/Ce/Cu-based low-temperature plasma catalyst. The preparation method directly prepares the nano porous carbon-based catalytic material by calcining the MOFs material at high temperature, has the advantages of high dispersion of metal active components, stable structure and the like, can effectively avoid the agglomeration of the metal active components, and obviously improves the catalytic activity and the stability.
Description
Technical Field
The invention belongs to the technical field of catalytic materials, and particularly relates to a Mn/Ce/Cu-based low-temperature plasma catalyst, and preparation and application thereof.
Background
Volatile Organic Compounds (VOCs) are various, including alkanes, olefins, halogenated hydrocarbons, esters, aldehydes, ketones, aromatic compounds, and the like, and mainly come from the industries of medicine, petrochemical industry, printing, and the like. Most VOCs are toxic, can react under illumination to form photochemical smog, are one of precursors of ozone pollution and PM2.5, and can increase the possibility of diseases such as cancers and the like after being kept in an environment containing volatile organic compounds for a long time. Therefore, the development of industrial volatile organic compound pollution treatment has extremely important application value.
In order to effectively treat the pollution of VOCs in organic waste gas, catalytic combustion method, adsorption method, absorption method and the like are widely adopted at home and abroad, and treatment technologies researched in recent years comprise biomembrane method, photocatalytic oxidation method, plasma method and the like. In many VOCs treatment technologies, low-temperature plasma can be quickly reduced at normal temperature and normal pressureHas attracted much attention for the removal of VOCs. However, the pure low temperature plasma technique has high energy consumption and low selectivity, and some VOCs can be produced into toxic byproducts in the degradation process. In order to overcome the defects, the low-temperature plasma is coupled with the catalytic oxidation technology, namely, a catalyst is filled in a discharge area of the plasma, and the catalytic oxidation efficiency and selectivity of the low-temperature plasma on the VOCs organic pollutants are greatly improved under the synergistic action of the plasma and the catalyst. The catalyst is the core of the low-temperature plasma catalytic oxidation technology, and the reported catalysts comprise a transition metal catalyst, a noble metal catalyst and the like. For example, H.T.Quoc An et al [ An H T Q, Huu T P, Van T L, et al.application of exothermic non thermal plasma-catalytic system for air polarization control: Toluene removal [ J].Catalysis Today,2011,176(1):474-477.]Preparing a series of catalysts containing Ag, Au, Cu, Co, Mn, La, Nb and other elements, wherein 1 percent (mass fraction) of Au/Al2O3And Nb2O5The catalyst has a conversion rate of the toluene reaching 96%. MnO at ordinary temperature for Huanghaibao et al (Longlimnan, Zhao Jian Guo, Yang Li Mao, etc.)2/Al2O3Catalyst catalyzed ozone oxidation toluene reaction [ J]Catalytic journal, 2011,32(6): 904-.]Adding TiO into the mixture2/γ-/Al2O3Treatment of VOCs by combining foamed nickel with plasma to increase CO content of product2Selectivity, however, the catalyst is easily deactivated by the accumulation of by-products. Wu-Jun-an et al [ Wu-Jun-an, Xia-an, Liu-Zhi-an, etc.. comparison of activities of Mn, Fe and Cu oxides in low-temperature plasma catalytic oxidation toluene system [ J]Functional material 2012,43(10):1332-1335.]The metal organic framework material MIL-101 and the plasma are combined to treat the toluene, the conversion rate of the toluene reaches 100 percent, and CO is treated2The selectivity reaches 70%, and reaction byproducts can be obviously reduced. Because the MOFs frameworks themselves have relatively poor stability (including thermal stability, chemical stability, etc.), their industrial application is greatly limited.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a Mn/Ce/Cu-based low-temperature plasma catalyst.
The invention also aims to provide the Mn/Ce/Cu-based low-temperature plasma catalyst prepared by the method.
The invention further aims to provide the application of the Mn/Ce/Cu-based low-temperature plasma catalyst in the low-temperature plasma catalytic oxidation degradation of VOCs.
It is a further object of the present invention to provide the use as described above.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following preparation steps:
(1) dissolving manganese-containing metal salt, cerium-containing metal salt and copper-containing metal salt in DMF, adding an organic ligand, and performing ultrasonic mixing to obtain a mixed solution;
(2) reacting the mixed solution obtained in the step (1) at the temperature of 80-120 ℃, and soaking a solid product in DMF (dimethyl formamide) for activation to obtain an activated crystal;
(3) and (3) washing and drying the activated crystal obtained in the step (2), and then roasting at 300-400 ℃ to obtain the Mn/Ce/Cu-based low-temperature plasma catalyst.
Further, the manganese-containing metal salt in the step (1) is selected from at least one of manganese nitrate, manganese sulfate, manganese carbonate and manganese acetate; the cerium-containing metal salt is at least one selected from cerium nitrate, cerium sulfate, cerium carbonate and cerium acetate; the copper-containing metal salt is selected from at least one of copper nitrate and copper sulfate.
Further, the manganese-containing metal salt, the cerium-containing metal salt and the copper-containing metal salt in the step (1) are used in a molar ratio of manganese element to cerium element to copper element of 1:2 (1-2). More preferably 1:2:1, 1:2:1.5 or 1:2: 2.
Further, the organic ligand in step (1) is selected from formic acid or acetic acid, more preferably formic acid.
Further, the molar ratio of the dosage of the organic ligand in the step (1) to the manganese element in the manganese-containing metal salt is 1 (5.8-9); more preferably 1:5.8, 1:7.2 or 1: 9.
Further, the reaction time in the step (2) is 10-15 h.
Further, the time for soaking in DMF for activation in the step (2) is 12-24 h.
Further, in the step (3), the roasting is carried out in an air atmosphere, and the roasting time is 2-3 hours.
The Mn/Ce/Cu-based low-temperature plasma catalyst is prepared by the method.
The Mn/Ce/Cu-based low-temperature plasma catalyst is applied to the catalytic oxidation degradation of VOCs by low-temperature plasmas.
The principle of the invention is as follows: directly calcining the MOFs material at high temperature in a certain air atmosphere, and carbonizing the organic ligand to obtain the nano porous carbon-based catalytic material. The carbonized MOFs-based catalytic material prepared by the method has the advantages of high dispersion of metal active components, stable structure and the like, can effectively avoid agglomeration of the metal active components, obviously improves the catalytic activity and stability, can be used as a carbonized Mn/Ce/Cu-based MOF catalytic material, is applied to a low-temperature plasma catalytic oxidation VOCs system, and can realize efficient removal of VOCs under the conditions of normal temperature and normal pressure.
The preparation method and the obtained product have the following advantages and beneficial effects:
(1) compared with the traditional supported catalyst, the catalyst has the characteristics of high dispersion of metal active components, high porosity and stable structure, can effectively avoid the agglomeration of the metal active components, and has high catalytic oxidation activity on VOCs (volatile organic compounds) such as toluene;
(2) the raw materials used by the preparation method are cheap and easy to obtain, and the preparation method is simple and is beneficial to industrial large-scale application;
(3) compared with the prior catalysis technology, the catalyst provided by the invention can be used together with a plasma device to rapidly catalyze and oxidize methylbenzene at normal temperature and normal pressure, the conversion rate of the methylbenzene can reach 100%, and CO can reach2The selectivity is up to 88%.
Drawings
FIG. 1 is an XRD pattern of Mn/Ce/Cu-based low-temperature plasma catalyst obtained in examples 1-3 of the present invention.
FIG. 2 is a graph of the conversion rate of toluene in the Mn/Ce/Cu-based low-temperature plasma catalyst obtained in examples 1-3 of the present invention under different plasma energy densities.
FIG. 3 shows CO of Mn/Ce/Cu-based low-temperature plasma catalysts obtained in examples 1 to 3 of the present invention under different plasma energy densities2And (4) a selectivity graph.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) 520. mu.L of Mn (NO) with a mass concentration of 50%3)2Aqueous solution, 1.94gCe (NO)3)3·6H2O and 0.54gCu (NO)3)2·3H2Adding O into 80ml of DMMF, adding 1000 mu L of formic acid, and uniformly mixing by ultrasonic treatment for 10min to obtain a mixed solution;
(2) placing the mixed solution in an oven at 80 ℃ for reaction for 10h, removing supernatant after the solution is cooled, adding fresh DMF, soaking and activating at room temperature for 12h to prepare an activated crystal material (Mn/Ce/Cu-MOF);
(3) washing the activated crystal material with DMF, filtering, and drying the filtered material in a vacuum oven at 50 ℃; and (3) putting the dried crystal material into a muffle furnace, and roasting for 2h at 300 ℃ to prepare the Mn/Ce/Cu-based low-temperature plasma catalyst.
Example 2
(1) 520. mu.L of Mn (NO) with a mass concentration of 50%3)2Aqueous solution, 1.94gCe (NO)3)3·6H2O and 0.81gCu (NO)3)2·3H2Adding O into 80ml of DMMF, adding 1200 mu L of formic acid, and uniformly mixing by ultrasonic treatment for 10min to obtain a mixed solution;
(2) placing the mixed solution in an oven at 100 ℃ for reaction for 12h, removing supernatant after the solution is cooled, adding fresh DMF, soaking and activating at room temperature for 18h to prepare an activated crystal material (Mn/Ce/Cu-MOF);
(3) washing the activated crystal material with DMF, filtering, and drying the filtered material in a vacuum oven at 50 ℃; and (3) putting the dried crystal material into a muffle furnace, and roasting at 350 ℃ for 2.5h to prepare the Mn/Ce/Cu-based low-temperature plasma catalyst.
Example 3
(1) 520. mu.L of Mn (NO) with a mass concentration of 50%3)2Aqueous solution, 1.94gCe (NO)3)3·6H2O and 1.08gCu (NO)3)2·3H2Adding O into 80ml of DMMF, adding 1500 mu L of formic acid, and uniformly mixing by ultrasonic treatment for 10min to obtain a mixed solution;
(2) placing the mixed solution in a 120 ℃ oven for reaction for 15h, removing supernatant after the solution is cooled, adding fresh DMF, soaking and activating at room temperature for 24h to prepare an activated crystal material (Mn/Ce/Cu-MOF);
(3) washing the activated crystal material with DMF, filtering, and drying the filtered material in a vacuum oven at 50 ℃; and (3) putting the dried crystal material into a muffle furnace, and roasting for 3h at 400 ℃ to prepare the Mn/Ce/Cu-based low-temperature plasma catalyst.
Characterization and performance measurements of the catalyst samples obtained in the above examples:
(1) x-ray diffraction analysis
An X-ray diffractometer model D8-ADVANCE of Bruker company, Germany is adopted, the operation conditions are copper target, 40KV, 40mA, step length is 0.02 degree, and scanning speed is 17.7 seconds per step. The Mn/Ce/Cu-based low-temperature plasma catalysts prepared in examples 1-3 were characterized, respectively.
FIG. 1 is an XRD spectrum of a Mn/Ce/Cu-based low-temperature plasma catalyst prepared in examples 1-3 of the present invention. As can be seen from FIG. 1, the three catalysts all have the same XRD spectrogram, the same characteristic peak position and wider peak width, which shows that the target catalyst is synthesized in examples 1-3.
(2) Catalytic Oxidation Performance test
Respectively taking the Mn/Ce/Cu-based low-temperature plasma catalysts obtained in the embodiments 1-3, pressing the surfaces, then sieving the surfaces by a 40-60-mesh sieve, and filling the surfaces into a scanning plasma device. The activity test conditions were as follows: the reaction temperature is 35 ℃, the reaction pressure is normal pressure, the total flow of gas is 100mL/min, the concentration of toluene is 30ppm, and the carrier gas is dry air. Toluene concentrateDegree and CO2The concentration was determined by gas chromatography.
FIG. 2 is a graph showing the conversion rate of toluene in catalysts obtained in examples 1 to 3 of the present invention under different plasma energy densities. Wherein the catalyst in example 2 has the best toluene degradation capability, and the degradation rate reaches 100% at the energy density of 294J/L.
FIG. 3 shows CO of catalysts obtained in examples 1 to 3 of the present invention under different plasma energy densities2And (4) a selectivity graph. As can be seen from the graph, CO increases with the energy density2The selectivity increased with the catalyst of example 2 having the best CO at 294J/L2Selectivity to CO thereof2The selectivity reaches 88 percent.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A preparation method of a Mn/Ce/Cu-based low-temperature plasma catalyst is characterized by comprising the following preparation steps:
(1) dissolving manganese-containing metal salt, cerium-containing metal salt and copper-containing metal salt in DMF, adding an organic ligand, and performing ultrasonic mixing to obtain a mixed solution;
(2) reacting the mixed solution obtained in the step (1) at the temperature of 80-120 ℃, and soaking a solid product in DMF (dimethyl formamide) for activation to obtain an activated crystal;
(3) washing and drying the activated crystal obtained in the step (2), and then roasting at 300-400 ℃ to obtain a Mn/Ce/Cu-based low-temperature plasma catalyst;
the organic ligand in the step (1) is selected from formic acid or acetic acid.
2. The method for preparing a Mn/Ce/Cu-based low-temperature plasma catalyst according to claim 1, wherein the Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following steps: in the step (1), the manganese-containing metal salt is selected from at least one of manganese nitrate, manganese sulfate, manganese carbonate and manganese acetate; the cerium-containing metal salt is at least one selected from cerium nitrate, cerium sulfate, cerium carbonate and cerium acetate; the copper-containing metal salt is selected from at least one of copper nitrate and copper sulfate.
3. The method for preparing a Mn/Ce/Cu-based low-temperature plasma catalyst according to claim 1, wherein the Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following steps: in the step (1), the manganese-containing metal salt, the cerium-containing metal salt and the copper-containing metal salt are used according to the molar ratio of manganese element to cerium element to copper element of 1:2 (1-2).
4. The method for preparing a Mn/Ce/Cu-based low-temperature plasma catalyst according to claim 1, wherein the Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following steps: the molar ratio of the dosage of the organic ligand in the step (1) to the manganese element in the manganese-containing metal salt is 1 (5.8-9).
5. The method for preparing a Mn/Ce/Cu-based low-temperature plasma catalyst according to claim 1, wherein the Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following steps: the reaction time in the step (2) is 10-15 h.
6. The method for preparing a Mn/Ce/Cu-based low-temperature plasma catalyst according to claim 1, wherein the Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following steps: and (3) soaking in DMF for activation for 12-24 h in the step (2).
7. The method for preparing a Mn/Ce/Cu-based low-temperature plasma catalyst according to claim 1, wherein the Mn/Ce/Cu-based low-temperature plasma catalyst comprises the following steps: and (3) roasting in an air atmosphere for 2-3 h.
8. A Mn/Ce/Cu-based low-temperature plasma catalyst is characterized in that: prepared by the method of any one of claims 1 to 7.
9. The use of the Mn/Ce/Cu-based low temperature plasma catalyst of claim 8 in the catalytic oxidative degradation of VOCs by low temperature plasma.
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