CN114570382A - Palygorskite/Mn-Cu composite catalyst and preparation method and application thereof - Google Patents
Palygorskite/Mn-Cu composite catalyst and preparation method and application thereof Download PDFInfo
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- CN114570382A CN114570382A CN202210254966.2A CN202210254966A CN114570382A CN 114570382 A CN114570382 A CN 114570382A CN 202210254966 A CN202210254966 A CN 202210254966A CN 114570382 A CN114570382 A CN 114570382A
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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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
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- 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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Abstract
The invention discloses a preparation method of a palygorskite/Mn-Cu composite catalyst, which specifically comprises the following steps; the palygorskite/Mn-Cu composite catalyst is obtained by taking palygorskite as a carrier, loading Mn and Cu active components in a dipping solution by a dipping method and roasting. Compared with the existing catalytic combustion technology, the catalytic combustion method has the advantages of low raw material price, rich reserves, large specific surface area, higher catalyst activity and better performance of catalytic combustion of toluene, and has wide application value in the industrial field of VOCs degradation.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a palygorskite/Mn-Cu composite catalyst, and a preparation method and application thereof.
Background
Volatile Organic Compounds (VOCs) emitted by industrial and commercial processes pose significant hazards to human health and the environment. Therefore, it is important to develop effective techniques for degradation of VOCs. The catalytic combustion technology has the advantages of low energy consumption, high removal rate, less secondary pollution and the like, and is generally considered to be the most promising VOCs control method. However, the industrial applicability of this technology depends to a large extent on the catalyst. Catalysts for catalytic combustion of VOCs include two major classes of noble metals and transition metals.
Among them, noble metal catalysts have been proved to have high low-temperature catalytic activity, but their wide application is limited by their disadvantages of high cost, easy poisoning, etc. In recent years, considerable work has been done by researchers in developing non-noble metal catalysts with good low temperature VOCs catalytic activity. Transition metal oxides such as oxides of Mn, Cu, Co, Fe, Cr, V, Ce, Zr are considered promising candidates, with manganese-based catalysts being the most active catalysts, especially manganese-copper bimetallic-based catalysts, but currently the preparation process is complex, the raw material cost is high, and the catalytic activity cannot meet the process requirements.
At present, the problem to be solved by those skilled in the art is to provide a composite catalyst with low raw material cost and higher catalyst activity.
Disclosure of Invention
Compared with the prior catalytic combustion technology, the palygorskite/Mn-Cu composite catalyst has the advantages of low raw material price, rich reserves, large specific surface area, higher catalyst activity and better performance of catalytic combustion of toluene, and has wide application value in the industrial field of VOCs degradation.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a palygorskite/Mn-Cu composite catalyst specifically comprises the following steps: the palygorskite/Mn-Cu composite catalyst is obtained by taking palygorskite as a carrier, loading Mn and Cu active components in a dipping solution by a dipping method and roasting.
Preferably, the raw material of the impregnating solution is Mn (NO)3)2And Cu (NO)3)2·6H2O。
The invention adopts nitrate to produce exhaust emission which is minimum relative to other salts.
Preferably, the Mn (NO)3)2Is 50 wt% Mn (NO)3)2Wherein the 50 wt% Mn (NO)3)2、Cu(NO3)2·6H2The mass volume ratio of O to water is 3.44-3.48g:1.0g:5.3 ml.
Preferably, the mass-volume ratio of the palygorskite to the impregnating solution is 1 g:1 ml.
Preferably, the calcination temperature is 400-.
The palygorskite/Mn-Cu composite catalyst is prepared by the preparation method.
The palygorskite/Mn-Cu composite catalyst prepared by the preparation method is applied to catalyzing the degradation of volatile organic compounds.
The palygorskite/Mn-Cu composite catalyst prepared by the preparation method is applied to catalytic combustion degradation of toluene.
Preferably, the reaction temperature of the catalysis is 100-400 ℃.
Compared with the prior art, the invention has the following beneficial effects: compared with the existing catalytic combustion technology, the catalytic combustion method has the advantages of low raw material price, rich reserves, large specific surface area, higher catalyst activity and better performance of catalytic combustion of toluene, and has wide application value in the industrial field of VOCs degradation.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an SEM image of palygorskite/Mn-Cu composite catalyst prepared by examples 1-5 of the present invention;
FIG. 2 is an XRD diffraction pattern of palygorskite/Mn-Cu composite catalysts prepared by examples 1-5 of the present invention;
FIG. 3 is a graph showing the conversion of toluene in the catalytic combustion of the palygorskite/Mn-Cu composite catalyst prepared in examples 1-5 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of a palygorskite/Mn-Cu composite catalyst specifically comprises the following steps:
the catalyst was prepared by an isovolumetric impregnation method, 2.60g of 50 wt% Mn (NO)3)20.75g of Cu (NO)3)2·6H2Adding O and a proper amount of deionized water into a 10mL centrifuge tube, stirring for dissolving, and uniformly mixing to prepare 4mL of impregnation liquid for later use;
weighing 4g of Pal powder sample, paving the sample at the bottom of a crucible, dropwise adding the impregnation liquid on the Pal, carrying out ultrasonic treatment at normal temperature, fully impregnating for 30min, then transferring the Pal powder sample into an oven to be dried for 12h at 100 ℃ (the dried sample is marked as Mn-Cu/Pal), and then roasting the Pal powder sample in a muffle furnace at 300 ℃ for 4h to obtain catalyst samples with Mn and Cu mass contents (wt%) of 10% and 5%, respectively, and marked as Mn-Cu/Pal-300.
Examples 2 to 5
The calcination temperatures were set to 400 deg.C, 500 deg.C, 600 deg.C and 700 deg.C, respectively, and the remaining steps and parameters were identical to those of example 1, to obtain catalyst samples having Mn and Cu mass contents (wt%) of 10% and 5%, respectively, labeled Mn-Cu/Pal-400, Mn-Cu/Pal-500, Mn-Cu/Pal-600, Mn-Cu/Pal-700, respectively, with the relevant SEM and XRD patterns for the samples shown in FIGS. 1 and 2,
the shape difference of Mn-Cu/Pal before roasting and Mn-Cu/Pal-T samples after roasting at different temperatures is inspected through SEM, and the results are shown in an SEM image, so that roasting operation and different roasting temperatures have obvious influence on the shape of the samples, and unfired samples do not present clear palygorskite shapes and probably have the surface covered by an active component precursor; the catalyst prepared by roasting at 300 ℃ gradually shows a palygorskite fibrous morphology, but still has an obvious agglomeration phenomenon, the temperature is continuously raised to 400 ℃, an obvious and uniformly distributed slender fibrous morphology can be observed on an SEM image of the catalyst, particles with the size of 10-20 nm are uniformly distributed on the surface of the catalyst, and the particles are related to Cu and Mn oxide active species; therefore, according to the BET result, the Mn-Cu/Pal-400 catalyst has the largest specific surface area, is beneficial to the diffusion and distribution of active components, continuously raises the temperature to 500 ℃, the fibrous morphology begins to become fuzzy, and when the roasting temperature reaches above 600 ℃, the originally slender fibers are obviously sintered and agglomerated, and the pore channel structure of the palygorskite collapses.
As can be seen from the XRD pattern, the XRD pattern of the unfired Mn-Cu/Pal sample mainly presents palygorskite (JCPDsNo.21-0957), SiO2(JCPDsNo.46-1045) and CuO (JCPDsNo. 48-1548). In contrast, the diffraction peak of the sample after roasting is obviously changed, which shows that the structure of the catalyst is correspondingly changed, and the XRD spectrogram of the catalyst obtained by roasting at the temperature of 300-500 ℃ mainly shows CuO and Mn2O3Characteristic peaks of (JCPDsNo.33-0900), indicating that stable CuO and Mn are formed2O3A crystalline phase; the roasting temperature is continuously increased to over 600 ℃, and the main crystal phase of the catalyst consists of original CuO and Mn2O3Phase coexistence to CuMn2O4The (JCPDsNo.34-1400) crystal phase is dominant. In addition, it is noted that the original palygorskite characteristic peak strength gradually decreases with the increase of the firing temperature, which is caused by the gradual collapse of the palygorskite structure at high temperature.
Application example
The catalyst obtained in the embodiment 1-5 is subjected to the activity evaluation of catalytic combustion toluene, and the method specifically comprises the following steps:
grinding and screening a catalyst on a quartz reactor (with the inner diameter of 800mm) of a fixed bed to 26-40 meshes, wherein the loading amount of the catalyst is 0.5g, and uniformly mixing the catalyst and quartz sand according to the volume ratio of 1:1 and then putting the mixture into the reactor;
air is used as carrier gas in the experiment, toluene gas is generated by air bubbling (constant temperature ice water bath), and is mixed with the other path of air to form toluene waste gas with certain concentration, and then the toluene waste gas enters a fixed bed reactor filled with a catalyst for reaction, and the flow rate of the toluene waste gas entering the fixed bed reactor is 150mL and the concentration is 1500ppm by adjusting the flow rate of the two paths of gas.
Reaction conditions are as follows: normal pressure, reaction temperature of 100-400 ℃, and space velocity (GHSV) of 20000h-1(ii) a The reaction tail gas enters a gas chromatograph (provided with a Flame Ionization Detector (FID) and a Thermal Conductivity Detector (TCD)) for qualitative and quantitative analysis, and the related detection results are shown in a figure 3;
as can be seen from FIG. 3, the calcination temperature has a significant effect on the toluene conversion rate in catalytic combustion of the catalyst, the Mn-Cu/Pal-300 catalyst participates in the reaction, the toluene conversion rate can only reach 43.2% at the reaction temperature of 300 ℃, the Mn-Cu/Pal-300 catalyst participates in the reaction, the toluene conversion rate can reach 62% at the reaction temperature of 300 ℃, and complete toluene conversion can be realized when the reaction temperature is increased to 335 ℃; when the roasting temperature of the catalyst is increased to 500 ℃, compared with Mn-Cu/Pal-400, the catalytic combustion performance of toluene is slightly reduced, the roasting temperature is continuously increased to more than 600 ℃, the activity of the catalyst is obviously reduced, and the complete conversion temperature of Mn-Cu/Pal-700 is 60 ℃ higher than that of the Mn-Cu/Pal-400 catalyst;
as can be seen from the above, the method takes the cheap and easily available palygorskite as the carrier, loads Mn-Cu by an impregnation method, and then prepares a series of catalysts by roasting at different temperatures, and the influence of the roasting temperature on the performance of catalytic oxidation of toluene has the following conclusion:
(1) the roasting temperature obviously influences the surface structure, chemical state and toluene oxidation and degradation catalytic performance of the catalyst.
(2) The catalyst calcined at 400 ℃ (Mn-Cu/Pal-400) possesses a relatively large specific surface area (84.478 m)2Per gram), highly dispersed active species, optimal redox performance, highest lewis acid ratio (56.5%) and most oxygen vacancies, which is the optimal firing temperature.
(3) The Mn-Cu/Pal-400 catalyst has the best catalytic performance, and the complete toluene conversion temperature of the Mn-Cu/Pal-400 catalyst is only 335 ℃, which is obviously lower than that of catalysts calcined at other temperatures.
The various embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the various embodiments can be referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. A preparation method of a palygorskite/Mn-Cu composite catalyst is characterized by comprising the following steps: the palygorskite/Mn-Cu composite catalyst is obtained by taking palygorskite as a carrier, loading Mn and Cu active components in a dipping solution by a dipping method and roasting.
2. The method for preparing a palygorskite/Mn-Cu composite catalyst according to claim 1, wherein the raw material of the impregnation liquid is Mn (NO)3)2And Cu (NO)3)2·6H2O。
3. The method for preparing a palygorskite/Mn-Cu composite catalyst according to claim 2, wherein the Mn (NO) is3)2Is 50 wt% Mn (NO)3)2Wherein the 50 wt% Mn (NO)3)2、Cu(NO3)2·6H2The mass volume ratio of O to water is 3.44-3.48g:1.0g:5.3 ml.
4. The method for preparing the palygorskite/Mn-Cu composite catalyst according to claim 1, wherein the mass-volume ratio of the palygorskite to the impregnating solution is 1 g:1 ml.
5. The method for preparing a palygorskite/Mn-Cu composite catalyst according to claim 1, wherein the calcination temperature is 400-500 ℃.
6. A palygorskite/Mn-Cu composite catalyst obtained by the production method as claimed in any one of claims 1 to 5.
7. The application of the palygorskite/Mn-Cu composite catalyst obtained by the preparation method of any one of claims 1-5 in catalyzing the degradation of volatile organic compounds.
8. Use of a palygorskite/Mn-Cu composite catalyst obtained by the preparation method according to any one of claims 1-5 in the catalytic combustion degradation of toluene.
9. The use according to claim 8, wherein the reaction temperature of the catalysis is 100-400 ℃.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116393140A (en) * | 2023-03-27 | 2023-07-07 | 唐山学院 | Preparation method of VOCs catalytic combustion catalyst |
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AU2005202194A1 (en) * | 2005-05-23 | 2006-12-14 | Jun Li | Methods of producing catalysts for synthesizing alcohols from water gas using palygorskite |
CN107008254A (en) * | 2017-04-19 | 2017-08-04 | 南京工业大学 | A kind of non-noble metal composite oxide monoblock type catalyst for catalytic combustion and its preparation method and application |
CN107442130A (en) * | 2017-08-24 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of palygorskite load type national standard method and its preparation method and application |
CN110590679A (en) * | 2019-09-26 | 2019-12-20 | 上海城建职业学院 | Method for catalytic synthesis of 5-substituted barbituric acid derivative by rare earth chloride |
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
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AU2005202194A1 (en) * | 2005-05-23 | 2006-12-14 | Jun Li | Methods of producing catalysts for synthesizing alcohols from water gas using palygorskite |
CN107008254A (en) * | 2017-04-19 | 2017-08-04 | 南京工业大学 | A kind of non-noble metal composite oxide monoblock type catalyst for catalytic combustion and its preparation method and application |
CN107442130A (en) * | 2017-08-24 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of palygorskite load type national standard method and its preparation method and application |
CN110590679A (en) * | 2019-09-26 | 2019-12-20 | 上海城建职业学院 | Method for catalytic synthesis of 5-substituted barbituric acid derivative by rare earth chloride |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN116393140A (en) * | 2023-03-27 | 2023-07-07 | 唐山学院 | Preparation method of VOCs catalytic combustion catalyst |
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