CN113877565B - Preparation method of non-noble metal CDPF catalyst based on sodium metavanadate - Google Patents
Preparation method of non-noble metal CDPF catalyst based on sodium metavanadate Download PDFInfo
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- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
- B01J27/224—Silicon carbide
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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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
- B01J37/0215—Coating
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
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- F01N3/033—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
- F01N3/035—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES
- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
- F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
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Abstract
The invention provides a preparation method of a non-noble metal CDPF catalyst based on sodium metavanadate, which takes sodium metavanadate as a catalytic active component, wherein the catalytic active component is carried and dispersed on a cordierite carrier through a carrying component to prepare an integral catalyst, and the carrying component is one of alumina, silicon carbide and ceria. The catalyst coating activates O 2 by taking sodium metavanadate as a catalytic active component to generate active oxygen so as to react with PM; the catalytic active component is carried and dispersed on the cordierite carrier to prepare a monolithic catalyst by the carrying component, and the carrying component not only increases the contact area of the catalytic active component and PM, but also prevents the agglomeration effect of the catalytic active center.
Description
Technical Field
The invention relates to a catalyst and the preparation field thereof. In particular to a preparation method of a non-noble metal CDPF catalyst based on sodium metavanadate.
Background
Combustion of fossil fuels is a significant cause of air pollution, with PM2.5 being the most harmful to the human body. PM2.5 can accumulate a large amount of harmful substances such as organic pollutants, toxic heavy metals, acid oxides and the like, and penetrate into human organs and blood systems to cause respiratory diseases and harm human health.
Fuel emissions from mobile emissions sources such as motor vehicles, aircraft, marine vessels, off-road mobile machinery, etc. are one of the important sources of PM 2.5. In order to cope with the harm of mobile emissions sources to the atmosphere and human health, the emission regulation limits are actively established by various countries around the world to limit the emissions of mobile sources.
In recent years, particulate emission control technology has been developed as emission regulation limits of various countries are tightened. The in-machine purifying technology and the tail gas post-treatment technology are key technologies for effectively controlling and reducing the emission of the diesel engine. In particular, DPF technology is widely used for trapping diesel particulate. However, DPF technology is used to trap particulate matter, but does not have the function of oxidizing particulate matter itself. That is, the DPF carrier does not have a function of removing particulate matter, and as the number of particulate matters trapped in the DPF increases, the exhaust back pressure increases, and the performance of the engine deteriorates, and the power performance and economy deteriorate. Therefore, particulate removal is critical to the DPF. By incorporating an active component into the DPF catalyst, the activation performance of the soot particles is weakened, and the light-off temperature of the soot (which is typically greater than 500 ℃ in the absence of an active component) is reduced so that it can be oxidized at lower temperatures, a technique known as CDPF technique.
Currently, noble metal catalysts Pt, pd, and Rh are the most widely used catalysts with the best catalytic performance among CDPF catalysts, particularly Pt. The Pt catalyst oxidizes NO 2 in the tail gas, and then the soot reacts with NO 2 to produce CO 2 and N 2. In the process, NO 2 acts as a gas catalyst to realize the oxidization and catalysis of the carbon particles and the catalyst under the condition of indirect contact, and the efficiency of catalyzing and oxidizing the carbon particles is effectively improved. Although the noble metal catalyst Pt is a catalyst with good catalytic effect, the noble metal catalyst Pt is expensive, and in addition, the noble metal SO 2 has good oxidation activity, sulfate is easy to generate, and the catalyst poisoning phenomenon occurs.
The non-noble metal catalyst includes perovskite type catalysts, spinel type catalysts, transition metal type catalysts, and molten salt type catalysts. Wherein, the molten salt type catalyst containing alkali metal is melted into liquid phase near the reaction temperature of PM, the contact area between the catalyst and PM is greatly increased, and the catalytic performance is greatly improved.
On the one hand, the molten salt type catalyst exhibits a sufficient catalytic activity by changing to a liquid phase, and on the other hand, the possibility of migration and evaporation increases, so that the durability of the existing molten salt type catalyst is inferior to that of the noble metal catalyst.
Disclosure of Invention
The object of the present invention is to reduce the light-off temperature of PM while ensuring high durability of the catalyst by providing a CDPF catalyst that does not contain noble metals.
In order to achieve the above purpose, the invention provides a preparation method of a non-noble metal CDPF catalyst based on sodium metavanadate, which comprises the following steps:
Step S1, catalyst preparation: firstly, preparing sodium metavanadate catalyst solution by sodium chloride and vanadium pentoxide, preparing mixed solution by the sodium metavanadate catalyst solution and a supported component, and sequentially drying, roasting and crushing the mixed solution to prepare catalyst particles with the particle size of 2-1000 mu m;
Step S2, adding the catalyst particles crushed in the step S1 into deionized water, stirring, uniformly mixing, then adding sol and thickener, mixing and stirring to prepare slurry, and finally, adjusting the pH value of the slurry to 3-5 by adding sulfuric acid;
Step S3, coating and firing the slurry: and (3) coating the catalyst slurry on a cordierite carrier according to the coating amount of 5-15 g/L by a coating device, drying the coated catalyst for 3-7 hours at the temperature of 100-200 ℃, and finally, placing the coated catalyst into a muffle furnace to bake for 1-5 hours at the temperature of 500-600 ℃ to prepare the CDPF catalyst whole taking sodium metavanadate as an active component.
Further, the supporting component is selected from one of alumina, silicon carbide and ceria.
Further, the mass ratio of the components in the slurry is as follows: 3-4% of sodium chloride, 1.5-2.5% of vanadium pentoxide, 40-90% of sol and 40-90% of thickener.
Further, in the step S1, the drying temperature is 100-120 ℃, the drying time is 3-6 hours, the roasting temperature is 400-600 ℃, and the roasting time is 1-6 hours.
Further, the cordierite carrier is of a wall flow type structure, and the mesh number of the carrier is 200-600 meshes.
The preparation method is simple, and the prepared catalyst has larger specific surface area, better combustion performance and high durability. The catalyst coating activates O 2 by taking sodium metavanadate as a catalytic active component to generate active oxygen so as to react with PM; the catalytic active component is carried and dispersed on the cordierite carrier to prepare a monolithic catalyst by the carrying component, and the carrying component not only increases the contact area of the catalytic active component and PM, but also prevents the agglomeration effect of the catalytic active center.
Drawings
FIG. 1 is a chart depicting a catalyst preparation flow scheme of the present invention;
FIG. 2 is a graph depicting catalyst stability versus activity for different active components of the present invention;
FIG. 3 is a chart depicting the active ingredients and supported ingredients selected for the examples and comparative examples of the present invention;
FIG. 4 is a graph depicting the activity of sodium metavanadate catalysts of different loading compositions according to the invention.
Enthalpy of formation refers to: at a certain temperature and pressure, generating a thermal effect of 1mol of pure substance, also called heat generation, from the most stable simple substance; t max refers to the maximum oxidation particle rate temperature. The smaller the enthalpy of formation, the higher the stability of the catalytically active component; the smaller T max, the better the activation performance of the catalytically active component.
Detailed Description
The technical scheme of the invention is further described below with reference to the accompanying drawings and examples.
Example 1
As shown in fig. 1, a method for preparing a non-noble metal CDPF catalyst based on sodium metavanadate comprises the following steps:
Step S1, catalyst preparation: firstly, preparing sodium metavanadate catalyst solution by sodium chloride and vanadium pentoxide, preparing mixed solution by the sodium metavanadate catalyst solution and a supported component, and sequentially drying, roasting and crushing the mixed solution to prepare catalyst particles with the particle size of 2-1000 mu m;
Step S2, adding the catalyst particles crushed in the step S1 into deionized water, stirring, uniformly mixing, then adding sol and thickener, mixing and stirring to prepare slurry, and finally, adjusting the pH value of the slurry to 3-5 by adding sulfuric acid;
Step S3, coating and firing the slurry: and (3) coating the catalyst slurry on a cordierite carrier according to the coating amount of 5-15 g/L by a coating device, drying the coated catalyst for 3-7 hours at the temperature of 100-200 ℃, and finally, placing the coated catalyst into a muffle furnace to bake for 1-5 hours at the temperature of 500-600 ℃ to prepare the CDPF catalyst whole taking sodium metavanadate as an active component.
As shown in FIG. 3, a specific comparative example is
Comparative example 1: the comparative example was carried out in the same manner as in example 1 except that the catalyst active ingredient was different from example 1, cesium undecanovanadate (Cs 2V4O11) catalyst solution was prepared from cesium sulfate and vanadium sulfate, and the whole CDPF catalyst was prepared.
The silicon carbide for supporting component separation of the comparative example comprises the following components in mass ratio: 3-4% of cesium sulfate, 1.5-2.5% of vanadium sulfate, 40-90% of sol and 40-90% of thickener.
The coating loading on the whole of the CDPF catalyst cordierite described in this comparative example was the same as in example 1.
Comparative example 2:
the comparative example was carried out in the same manner as in example 1, except that the catalyst active components were different from those of example 1 and comparative examples 1 and 2, and a rubidium metavanadate catalyst solution was prepared from rubidium chloride and vanadium pentoxide, and a CDPF catalyst monolith was prepared by the same preparation process as in example 1.
The supporting component in this comparative example is silicon carbide, and the mass ratio of the components in the slurry is: 3-4% of rubidium chloride, 1.5-2.5% of vanadium pentoxide, 40-90% of sol and 40-90% of thickener. .
The coating loading on the whole of the CDPF catalyst cordierite described in this comparative example was the same as in example 1.
Comparative example 3:
The catalytically active component, catalyst preparation process, loading and mass ratio of the components of this comparative example were the same as in example 1.
Further, the supporting component is alumina for separation.
Comparative example 4
The catalytically active component, catalyst preparation process, loading and mass ratio of the components of this comparative example were the same as in example 1.
The support component is ceria.
In example 1, comparative examples 2 and 3 for reducing PM emissions of diesel engines provided by the present invention, the catalyst formation enthalpy of sodium metavanadate as an active component was-1253 kJ/mol, T max was 476 ℃, the formation enthalpy of cesium undecanovanadate (Cs 2V4O11) as an active component was-1018 kJ/mol, T max was 487 ℃, the formation enthalpy of cesium undecanovanadate (Cs 2V4O11) as an active component was-1265 kJ/mol, and T max was 500 ℃. That is, example 1 is the most preferred catalyst active component, which has the best stability, strong durability, and the highest catalytic activity.
FIG. 4 shows a comparison of the activities of sodium metavanadate catalysts of different loading compositions, the loading composition of example 1 of the present invention being silicon carbide, having a T max of 476 ℃; the supporting component of comparative example 4 is alumina, the T max of which is greater than 600 ℃; the supporting component of comparative example 5 was ceria, and its T max was 522 ℃. That is, the catalytic activity of sodium metavanadate whose supporting component is silicon carbide is higher than that of the other two supporting components.
Claims (4)
1. A preparation method of a non-noble metal CDPF catalyst based on sodium metavanadate is characterized by comprising the following steps:
the method comprises the following steps:
step S1, catalyst preparation: firstly, preparing sodium metavanadate catalyst solution by sodium chloride and vanadium pentoxide, preparing mixed solution by the sodium metavanadate catalyst solution and silicon carbide, and sequentially drying, roasting and crushing the mixed solution to prepare catalyst particles with the particle size of 2-1000 mu m;
Step S2, adding the catalyst particles crushed in the step S1 into deionized water, stirring, uniformly mixing, then adding sol and thickener, mixing and stirring to prepare slurry, and finally, adjusting the pH value of the slurry to 3-5 by adding sulfuric acid;
Step S3, coating and firing the slurry: and (3) coating the catalyst slurry on a cordierite carrier according to the coating amount of 5-15 g/L by a coating device, drying the coated catalyst for 3-7 hours at the temperature of 100-200 ℃, and finally, placing the coated catalyst into a muffle furnace to bake for 1-5 hours at the temperature of 500-600 ℃ to prepare the CDPF catalyst whole taking sodium metavanadate as an active component.
2. The method for preparing a non-noble metal CDPF catalyst based on sodium metavanadate as claimed in claim 1, characterized in that: the mass ratio of the components in the slurry is as follows: 3-4% of sodium chloride, 1.5-2.5% of vanadium pentoxide, 40-90% of sol and 40-90% of thickener.
3. The method for preparing a non-noble metal CDPF catalyst based on sodium metavanadate as claimed in claim 1, characterized in that:
In the step S1, the drying temperature is 100-120 ℃, the drying time is 3-6 hours, the roasting temperature is 400-600 ℃, and the roasting time is 1-6 hours.
4. The method for preparing a non-noble metal CDPF catalyst based on sodium metavanadate as claimed in claim 1, characterized in that:
The cordierite carrier is of a wall flow type structure, and the mesh number of the carrier is 200-600 meshes.
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Citations (8)
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Effective date of registration: 20240725 Address after: Room 104, Building 3, Sevilla, 588 Xihu East Road, Huizhi Enterprise Center, Xishan Development Zone, Wuxi City, Jiangsu Province, China 214117 Patentee after: Wuxi Carbon and Carbon Search Technology Co.,Ltd. Country or region after: China Address before: 461000 Building 8, Weidu hi tech Industrial Park, Hongteng Road, Xuchang Weidu industrial cluster, gaoqiaoying street, Weidu District, Xuchang City, Henan Province Patentee before: Mobile source special fiber (Henan) Co.,Ltd. Country or region before: China |
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