CN114251158B - Diesel exhaust particulate matter catalytic filter and method for manufacturing same - Google Patents
Diesel exhaust particulate matter catalytic filter and method for manufacturing same Download PDFInfo
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- CN114251158B CN114251158B CN202011016991.4A CN202011016991A CN114251158B CN 114251158 B CN114251158 B CN 114251158B CN 202011016991 A CN202011016991 A CN 202011016991A CN 114251158 B CN114251158 B CN 114251158B
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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
- F01N3/021—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
- 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, e.g. catalysed diesel particulate filters
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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
-
- 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
-
- 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
Abstract
The invention provides a diesel engine exhaust particulate matter catalytic filter without a noble metal catalyst and a manufacturing method thereof, the catalytic particulate matter filter comprises a DPF carrier and a catalyst coating coated in the DPF carrier, the catalyst coating takes a cerium-zirconium composite oxide as an inner coating and a lanthanum-manganese-copper composite oxide as an outer coating, and the manufacturing method comprises the steps of preparing the cerium-zirconium composite oxide, coating the inner coating, preparing a lanthanum-manganese-copper solution, coating the outer coating and heating and sintering. The particulate filter can increase the combustion speed of particulate matter.
Description
Technical Field
The present invention relates to a diesel exhaust particulate catalytic filter and a method for manufacturing the same.
Background
The catalyst adopted by the DPF of the diesel engine exhaust particulate matter catalytic filter on the market is a noble metal catalyst coated on a coating layer of a cocatalyst such as alumina/cerium oxide, and the coating amount of the noble metal is generally 10-20 g/ft 3 The larger the amount of the noble metal coatingThe better the catalytic effect. However, the noble metal is expensive and difficult for users to bear.
CN101767000A provides a direct oxidation catalyst for exhaust soot of a diesel vehicle and a preparation method thereof. The catalytic material is composed of oxide carrier MO 2 And a bimetal oxide active component AxByOz, and the structure is AxByOz/MO 2 . A, B is two metals of La, Ce, Fe, K and Cu, MO 2 Is TiO 2 、γ-Al 2 O 3 、CeO 2 、ZrO 2 And the like. The preparation method comprises the steps of forming a complexing solution by the ionic solution of A, B and complexing agents such as citric acid, urea, PVP, oxalic acid and the like, adding one of the oxides, simultaneously mechanically stirring to fully adsorb the oxides, then placing the solution into a muffle furnace at the temperature of 500 ℃ and 700 ℃, and rapidly reacting and decomposing the solution to synthesize the active component on the surface of the oxide in situ.
CN102000565A discloses a preparation method of a composite catalyst for eliminating carbon smoke of a diesel vehicle, which takes a Ce-Zr-based rare earth compound as a carrier and carries La-Mn-based perovskite as an active component; the carrier contains cerium dioxide and zirconium dioxide, and alumina or rare earth oxide is added as a crystal form stabilizer, and the preparation process comprises the following steps: (1) respectively dissolving nitrate or carbonate of cerium, zirconium and a stabilizer, adding a surfactant solution, adjusting the reaction pH to 7-11, then obtaining a precipitation solution, and roasting to prepare a Ce-Zr-based rare earth composite carrier; (2) respectively dissolving nitrates or citrates of lanthanum, manganese and an auxiliary agent to prepare a sol impregnation solution, impregnating the Ce-Zr-based rare earth compound carrier in sol, evaporating, drying and roasting to obtain the composite catalyst.
The catalyst particles prepared by the scheme can be combined into the DPF carrier only by using auxiliary agents such as a binder and the like in the process of coating the catalyst particles on the DPF, the addition of the auxiliary agents causes the coating liquid to have chemical reaction with the catalyst particles in the processes of preparation and sintering, and the catalytic performance of the coated catalyst particles is greatly reduced.
CN108906072A discloses a diesel vehicle soot particle catalytic combustion catalyst and a preparation method thereof, the catalyst comprises a carrier, a catalytic coating is coated on the carrier, the coating amount of the catalytic coating is 5-20 g/L, the catalytic coating comprises aluminum oxide and composite oxide, the weight ratio of the aluminum oxide to the composite oxide is 0.05:1, and the composite oxide comprises alkali metal oxide, transition metal oxide, cerium oxide, zirconium oxide and lanthanum oxide. The prepared catalyst has lower catalytic combustion ignition temperature and carbon deposit balance point temperature of carbon smoke particles, but is still insufficient.
Disclosure of Invention
The object of the present invention is to provide a catalytic particulate filter for diesel exhaust aftertreatment that does not require a noble metal catalyst and that can improve the particulate combustion rate, and a method for manufacturing the same.
The catalytic particulate filter comprises a DPF carrier and a catalyst coating coated in the DPF carrier, wherein the catalyst coating takes a cerium-zirconium composite oxide as an inner coating and a lanthanum-manganese-copper composite oxide as an outer coating, the molar ratio of cerium to zirconium elements in the cerium-zirconium composite oxide is 1: 0.1-0.4, the molar ratio of lanthanum to manganese to copper elements in the lanthanum-manganese-copper composite oxide is 1: 1.2-3: 0-0.5, the coating amount of the inner coating is 15-40 g/L in terms of the volume of the DPF, and the weight ratio of the outer coating to the inner coating is 0.5-1.2: 1.
Preferably, the cerium-zirconium element in the cerium-zirconium composite oxide has a molar ratio of 1: 0.2-0.3. In the lanthanum-manganese-copper composite oxide, the molar ratio of lanthanum, manganese and copper elements is preferably 1: 1.5-2.5: 0-0.5, more preferably 1: 1.8-2.4: 0.2-0.35.
The method for manufacturing the catalytic particulate filter of the present invention comprises the steps of:
A. preparing a cerium-zirconium composite oxide: dissolving cerium nitrate and zirconium nitrate in water according to the proportion, adding citric acid according to 1-1.5 times of the total molar amount of cerium and zirconium, stirring and heating at 80-100 ℃ to dryness, heating to 550-650 ℃ at the speed of 50-100 ℃/h, preserving heat for 1-3 hours, cooling, and performing ball milling for 8-24 hours to obtain a cerium-zirconium composite oxide;
B. preparing alumina sol: mixing pseudo-boehmite, concentrated nitric acid and water according to the mass ratio of 1: 0.75-1: 10, heating in water bath at 80 ℃ and stirring for 3-8 hours to obtain alumina sol;
C. coating of an inner coating: preparing 5-20% of cerium-zirconium composite oxide, 10-30% of alumina sol and the balance of water, coating the coating liquid in DPF, drying, heating to 550-650 ℃ at the speed of 50-100 ℃/h, preserving heat for 1-3 h, and cooling;
D. repeating step C until the coating amount of the inner coating is reached;
E. coating of the outer coating: dissolving lanthanum nitrate, manganese nitrate and copper nitrate into water according to the proportion, adding citric acid according to 1-1.5 times of the total molar weight of lanthanum, manganese and copper to prepare a solution with the total concentration of lanthanum, manganese and copper ions of 0.5-3 mol/L, dipping the DPF coated with the inner coating into the solution, taking out and drying the solution, heating the solution to 550-650 ℃ at the speed of 50-100 ℃/h, preserving heat for 1-3 hours, and cooling;
F. and E, repeating the step E until the coating weight of the outer coating is reached to obtain the catalytic particulate filter.
Preferably, in the step C, the cerium zirconium oxide powder is contained in an amount of 8 to 10%.
In the step E, the total concentration of lanthanum, manganese and copper ions is 1.5-2.5 mol/L.
The material of DPF carrier can use cordierite, silicon carbide or aluminium titanate, the mesh number is 100-300, preferably the common 200 mesh cordierite or silicon carbide honeycomb wall flow type carrier.
The invention has firm adhesion, adopts an air gun with the air pressure of 8kg to sweep, has no shedding phenomenon, completely does not use expensive noble metal catalyst, greatly reduces the cost, reduces the consumption of noble metal, has the performance which is comparable with that of the noble metal catalyst, directly coats the mixture of metal salt on the DPF, becomes the catalyst in the sintering process, and has wide popularization value.
Detailed Description
The following examples used a cylindrical wall-flow cordierite substrate having a DPF diameter of 143.8mm, a length of 152.4mm and a mesh number of 200, and a volume of 2.47L.
Example 1
Preparation of cerium-zirconium composite oxide: dissolving cerium nitrate, zirconium nitrate and citric acid in water according to the molar ratio of 1: 0.25: 1.25 to prepare a solution with the total concentration of metal ions of 1.5mol/L, heating and concentrating in a water bath at 80-100 ℃ to dryness under stirring, heating to 600 ℃ at the speed of 100 ℃/h, and preserving the temperature for 1 h to obtain a solid ball-milled cerium-zirconium composite oxide for 16 h.
Preparing alumina sol: mixing pseudo-boehmite, concentrated nitric acid and water according to the mass ratio of 1: 0.75: 10, and heating and stirring in a water bath at the temperature of 80 ℃ for 6 hours to obtain the alumina sol.
Coating of an inner coating: preparing internal coating liquid according to the proportion of 9 percent of cerium-zirconium composite oxide, 15 percent of alumina sol and 76 percent of water by weight percentage, sucking the coating liquid into honeycomb holes of a DPF carrier under the stirring state by negative pressure, removing the negative pressure to enable the coating liquid to naturally flow out to finish coating, heating the carrier to 600 ℃ at the speed of 100 ℃/hour after drying, preserving the temperature for 1 hour, cooling along with a furnace to finish the first layer coating, and testing to obtain the coating amount of the internal coating of 30 g/L.
Coating of the outer coating: dissolving lanthanum nitrate, manganese nitrate and citric acid in water according to the molar ratio of 1: 2: 3 to prepare a solution with the total concentration of metal ions of 2mol/L, dipping the DPF coated with the inner coating into the solution for 1-2 minutes to complete coating, heating to 600 ℃ at the speed of 100 ℃/hour after drying, preserving heat for 1 hour, and cooling with a furnace to obtain a finished product. The overcoat layer was tested to be applied at 28 g/L.
Example 2
Preparation of cerium-zirconium composite oxide: dissolving cerium nitrate, zirconium nitrate and citric acid in water according to the molar ratio of 1: 0.30: 1.30 to prepare a solution with the total concentration of metal ions of 1.5mol/L, heating in a water bath at the temperature of 80-100 ℃ while stirring, evaporating and concentrating to dryness, heating to 600 ℃ at the speed of 100 ℃/h, and preserving the temperature for 1 h to obtain a solid, and ball-milling the solid for 16 h to obtain the cerium-zirconium composite oxide.
Preparation of alumina sol: mixing pseudo-boehmite, concentrated nitric acid and water according to the mass ratio of 1: 0.75: 10, and heating and stirring in a water bath at the temperature of 80 ℃ for 6 hours to obtain the alumina sol.
Coating of an inner coating: preparing internal coating liquid according to the proportion of 9 percent of cerium-zirconium composite oxide, 15 percent of alumina sol and 76 percent of water by weight percentage, sucking the coating liquid into honeycomb holes of the DPF carrier under the stirring state by negative pressure, removing the negative pressure to enable the coating liquid to naturally flow out to finish coating, heating to 600 ℃ at the speed of 100 ℃/hour after drying, preserving the temperature for 1 hour, cooling along with a furnace, and finishing the internal coating. The coating amount of the inner coating layer was tested to be 30 g/L.
Coating of the outer coating: dissolving lanthanum nitrate, manganese nitrate, copper nitrate and citric acid in water according to the molar ratio of 1: 2: 0.3: 3.3 to prepare a solution with the total concentration of metal ions being 2mol/L, dipping the DPF coated with the inner coating layer in the solution for 1-2 minutes to complete coating, heating to 600 ℃ at the speed of 100 ℃/hour after drying, preserving the temperature for 1 hour, and cooling with a furnace to obtain a finished product. The coating amount of the overcoat layer was tested to be 28 g/L.
Performance testing
The test method comprises the following steps: the DPF of example 1 and example 2 was packaged with a coating of 10g/ft of the same commercial dimensions 3 For comparison, a silicon carbide DPF of platinum catalyst was connected to the exhaust system of a diesel engine.
Testing of PM treatment efficiency: on a dynamometer bench provided with a 55KW diesel engine with a calibrated power, different exhaust temperatures are obtained by adjusting the output power at a fixed rotating speed of 1500 r/min. The PM emissions per hour of the engine at each exhaust temperature were measured using a DPF not coated with any catalyst. The DPF is operated at an engine exhaust temperature of 250 ℃ for 1.5-2 g/L by accumulating PM as an initial weight, and then the weight of the DPF is measured, and the amount of the DPF per liter per hour at each exhaust temperature is calculated as the amount of the DPF per liter per hour = (initial weight + amount of PM discharged from the engine per hour at the temperature-weight of the DPF after operation)/volume of the DPF.
The efficiency of the DPF in PM treatment at each exhaust temperature of the engine is as follows:
| exhaust temperature C | 300 | 325 | 350 | 375 | 400 | 425 | 450 |
| Example 1 treatment efficiency g/Lhr | 0.1 | 0.4 | 0.7 | 1.2 | 1.5 | 2.5 | 3.5 |
| Example 2 treatment efficiency g/Lhr | 0.1 | 0.4 | 0.6 | 1.2 | 1.5 | 2.5 | 3.5 |
| Commercial DPF treatment efficiency g/Lhr | 0 | 0.1 | 0.15 | 0.2 | 0.6 | 1.0 | 1.3 |
The front end of the DPF is connected with a commercially available coating of 20g/ft 3 In the case of DOC with a platinum catalyst, the PM treatment efficiency at each exhaust temperature of the engine is as follows:
| exhaust temperature of | 300 | 325 | 350 | 375 | 400 | 425 | 450 |
| Example 1 treatment efficiency g/Lhr | 0.2 | 0.8 | 1.2 | 2.0 | 2.2 | 3.2 | 5 |
| Example 2 treatment efficiency g/Lhr | 0.2 | 0.9 | 1.2 | 1.9 | 2.3 | 3.5 | 5 |
| Commercial DPF treatment efficiency g/Lhr | 0.3 | 0.9 | 1.1 | 1.8 | 2.0 | 3 | 4 |
Therefore, the performance of the DPF prepared by the method is similar to that of the DPF coated with the noble metal catalyst, and the DPF can be used for the exhaust aftertreatment of a diesel engine instead of the DPF coated with the noble metal catalyst.
Claims (7)
1. A catalytic particulate filter for diesel engine exhaust aftertreatment comprises a DPF carrier and a catalyst coating coated in the DPF carrier, and is characterized in that the catalyst coating takes a cerium-zirconium composite oxide as an inner coating and a lanthanum-manganese-copper composite oxide as an outer coating, wherein the molar ratio of cerium to zirconium elements in the cerium-zirconium composite oxide is 1: 0.1-0.4, the molar ratio of lanthanum to manganese-copper elements in the lanthanum-manganese-copper composite oxide is 1: 1.2-3: 0-0.5, the coating amount of the inner coating is 15-40 g/L based on the volume of the DPF, and the weight ratio of the outer coating to the inner coating is 0.5-1.2: 1.
2. The catalytic particulate filter of claim 1, wherein a molar ratio of cerium to zirconium in the cerium-zirconium composite oxide is 1: 0.2 to 0.3.
3. The catalytic particulate filter of claim 1 or 2, wherein a molar ratio of the lanthanum, manganese, and copper elements in the lanthanum, manganese, and copper composite oxide is 1: 1.5-2.5: 0-0.5.
4. The catalytic particulate filter of claim 3, wherein a molar ratio of the lanthanum, manganese, and copper elements in the lanthanum, manganese, and copper composite oxide is 1: 1.8-2.4: 0.2-0.35.
5. The method of manufacturing a catalyzed particulate filter according to any one of claims 1 to 4, comprising the steps of:
A. preparing a cerium-zirconium composite oxide: dissolving cerium nitrate and zirconium nitrate into water according to the molar ratio of cerium and zirconium elements, adding citric acid which is 1 to 1.5 times of the total molar weight of cerium and zirconium, stirring and heating at the temperature of between 80 and 100 ℃ to dry, heating to the temperature of between 550 and 650 ℃ at the speed of between 50 and 100 ℃/hour, preserving heat for 1 to 3 hours, cooling, and performing ball milling for 8 to 24 hours to obtain a cerium-zirconium composite oxide;
B. preparing alumina sol: mixing pseudo-boehmite, concentrated nitric acid and water according to the mass ratio of 1: 0.75-1: 10, heating in water bath at 80 ℃ and stirring for 3-8 hours to obtain alumina sol;
C. coating of an inner coating: preparing 5-20% of cerium-zirconium composite oxide, 10-30% of alumina sol and the balance of water, coating the coating liquid in DPF, drying, heating to 550-650 ℃ at the speed of 50-100 ℃/h, preserving heat for 1-3 h, and cooling;
D. repeating step C until the coating amount of the inner coating is reached;
E. coating of the outer coating: dissolving lanthanum nitrate, manganese nitrate and copper nitrate into water according to the molar ratio of lanthanum, manganese and copper elements, adding citric acid according to 1-1.5 times of the total molar amount of lanthanum, manganese and copper to prepare a solution with the total concentration of lanthanum, manganese and copper ions of 0.5-3 mol/L, dipping the DPF coated with the inner coating into the solution, taking out and drying the solution, heating the solution to 550-650 ℃ at the speed of 50-100 ℃/h, preserving heat for 1-3 h, and cooling;
F. and E, repeating the step E until the coating weight of the outer coating is reached to obtain the catalytic particulate filter.
6. The method of manufacturing a catalytic particulate filter according to claim 5, wherein in the step C, the coating liquid is composed of 8 to 10% of the cerium-zirconium composite oxide, 10 to 20% of the alumina sol, and the balance being water.
7. The method of manufacturing a catalytic particulate filter according to claim 5 or 6, wherein the total concentration of lanthanum manganese copper ions in the step E is 1.5 to 2.5 mol/L.
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| CN114849697B (en) * | 2022-05-23 | 2023-10-27 | 东风汽车集团股份有限公司 | Catalyst based on three-way catalyst ceramic carrier and preparation method thereof |
| CN115487824B (en) * | 2022-08-18 | 2023-10-13 | 无锡双翼汽车环保科技有限公司 | Tail gas purifying device of mining explosion-proof diesel engine |
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