CN111229220B - Preparation method of three-way catalyst - Google Patents
Preparation method of three-way catalyst Download PDFInfo
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- CN111229220B CN111229220B CN202010045865.5A CN202010045865A CN111229220B CN 111229220 B CN111229220 B CN 111229220B CN 202010045865 A CN202010045865 A CN 202010045865A CN 111229220 B CN111229220 B CN 111229220B
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- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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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
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
- B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0027—Powdering
- B01J37/0036—Grinding
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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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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
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Abstract
The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a three-way catalyst, which comprises the following steps: (1) primer coating: mixing the noble metal powder and the adhesive to prepare slurry, then immersing the treated metal carrier into the slurry, taking out, blowing off the redundant slurry in the pore channel, drying and roasting to obtain a semi-finished product; preparing a dispersion solution: mixing a dispersing agent, a reducing agent and water to obtain a dispersion solution; adding an alkaline solution into the noble metal solution, and adjusting the pH =0-3 of the noble metal solution; (2) Diluting the noble metal solution treated in the step (3) by using the dispersion solution in the step (1) to obtain a coating solution; (3) And (3) coating the coating liquid obtained in the step (2) on the semi-finished product obtained in the step (1), drying and roasting to obtain a catalyst finished product. The catalyst prepared by the method has high surface concentration of the noble metal, increased utilization rate of the noble metal, simple coating process and excellent performance.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method of a three-way catalyst.
Background
On 7 months and 1 day in 2019, the national emission standard of motorcycles, namely GB 14622-2016 (limit value for emission of pollutants for motorcycles) and a measurement method (working condition method, stage IV in China), is implemented. Compared with nation III, nation IV puts forward stricter limit requirements on emission limit, durability and the like. Wherein in terms of emission limits: the emission limits of CO, CH and NOx are respectively increased by 54.2%, 47.9% and 58.8%. In terms of durability, the national IV is 8000km more than the national III, and the durability is prolonged by 66.7 percent. In order to enable the pollutant emission of the motorcycle to meet the national regulation requirements, the motorcycle adopts an electronic fuel injection technology, so that the original emission of an engine can be effectively controlled; and subsequent catalyst technology is combined to meet the emission limit requirement of national IV standard.
Pollutants in motorcycle tail gas mainly contain carbon monoxide (CO), nitrogen oxides (NOx) and Hydrocarbons (HC), and because the motorcycle engine is a small engine and the combustion in the engine is insufficient, unburned fuel and oxygen in the tail gas are high in concentration, the working environment of the catalyst is harsh, and the requirement on the purification efficiency of the catalyst is high. The installation of a catalytic purifier is one of the most effective methods for preventing and treating the motorcycle tail gas pollution. The most commonly used catalytic cleaner at present is a three-way catalyst which can simultaneously clean CO and NO in the tail gas under the condition of controlling the air-fuel ratio x And toxic and harmful substances such as HC.
The three-way catalyst mainly comprises a carrier, an auxiliary agent and an active component. The active components commonly used in the three-way catalyst are precious metals Pt, pd and Rh. Pt and Pd generally perform the oxidation function of oxidizing CO and HC in the exhaust gas to CO 2 Rh as NO mainly x A reduced active component. Due to the shortage of precious metal resources and high price, the research on three-way catalysts mainly focuses on developing catalysts with low precious metal content and excellent performance, which makes how to maximize precious metal utilization a research focus and difficulty
The commonly used methods include increasing the surface concentration of the noble metal (the carrier is directly soaked in the noble metal solution), adjusting the regional distribution of the noble metal (the segmented layered coating technology), and the like. However, most metal carriers have ports, and the method of soaking noble metal solution can cause that the solution can not be completely absorbed, thereby causing the waste of noble metal; in addition, the water absorption performance of the metal carrier is poor, and the direct soaking can cause the adsorption time to be too long, thereby increasing the production period. If the catalyst is coated in a segmented and layered manner according to the gasoline car catalyst mode, the carrier of the motorcycle catalyst is too small, and the segmented coating process is too complex.
Disclosure of Invention
The invention aims to: aiming at the problems that the cost requirement of the catalyst is lower and lower but the performance requirement is stricter and stricter in the prior art, and the existing preparation method cannot meet the preparation of the motorcycle catalyst, the preparation method of the catalyst is provided.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a motorcycle catalyst comprises the following steps:
(1) Coating a bottom layer: mixing the noble metal powder and the adhesive to prepare slurry, then immersing the treated metal carrier into the slurry, taking out, blowing off the redundant slurry in the pore channel, drying and roasting to obtain a semi-finished product;
preparing a dispersion solution: mixing a dispersing agent, a reducing agent and water to obtain a dispersion solution;
preparing a noble metal solution: adding an alkaline solution into the noble metal solution, and adjusting the pH =0-3 of the noble metal solution to obtain a treated noble metal solution; preferably, the pH of the solution is adjusted to 1-2; more preferably, the pH of the solution is adjusted to 1.5 to 2.
(2) Diluting the treated noble metal solution by using the dispersion solution in the step (1) to obtain a coating solution;
(3) And (3) coating the coating liquid obtained in the step (2) on the semi-finished product obtained in the step (1), drying and roasting to obtain a catalyst finished product.
The preparation method of the motorcycle catalyst comprises the steps of preparing precious metal powder into slurry, coating the slurry to obtain a semi-finished product, wherein the semi-finished product coated with the slurry has good water absorption performance and is beneficial to adsorbing precious metals in a precious metal solution; and mixing the noble metal solution with pH =0-3 with a dispersant and a reducing agent, and performing secondary coating to obtain the catalyst. The pH value of the noble metal solution is controlled within the range of pH =0-3, so that the corrosion effect of the solution on the semi-finished coating is reduced, and the precipitation of heavy metals is avoided, thereby improving the performance of the catalyst.
In a preferable embodiment of the present invention, in step (1), the noble metal powder is obtained by loading a noble metal on an oxygen storage material or an alumina material by an equivalent volume impregnation method, and drying and roasting the noble metal powder; the oxygen storage material comprises CeO 2 ，CeO 2 -ZrO 2 ，CeO 2 -ZrO 2 -Y 2 O 3 ，CeO 2 -ZrO 2 -La 2 O 3 ，CeO 2 -ZrO 2 -La 2 O 3 -Y 2 O 3 One or more of (a); the alumina material includes Al 2 O 3 Rare earth modified Al 2 O 3 And alkaline earth modified Al 2 O 3 One or more of (a).
As a preferable embodiment of the present invention, in the step (1), the noble metal is one or both of Pt and Rh.
As a preferable scheme of the invention, in the step (1), when the bottom layer is coated, the size of the slurry is 3-10 mu m, and the loading amount on the coating is 100-200g/L.
As a preferable scheme of the invention, in the step (1), the dispersant comprises one or more of polyacrylamide, xanthan gum, hydroxyethyl cellulose and polyvinyl alcohol.
The addition of the dispersing agent can increase the viscosity of the noble metal solution and prevent the noble metal from arbitrarily flowing due to the action of gravity in the subsequent coating process.
In a preferable embodiment of the present invention, in step (1), the reducing agent is one or more selected from methanol, ethanol, ethylene glycol, isopropanol, glycerol, ascorbic acid, glucose, and alkali metal citrate.
The addition of the reducing agent reduces the active components into a simple substance state in the roasting process, which is beneficial to the increase of active centers and the catalytic reaction.
In a preferred embodiment of the present invention, in the step (2), the mass fraction of the dispersant in the dispersion solution is 0.5 to 2.5%.
In a preferred embodiment of the present invention, in the step (1), the mass ratio of the reducing agent to the dispersing agent is 1.
In a preferred embodiment of the present invention, in the step (1), the viscosity of the dispersion solution is 500 to 5000mpa.s.
As a preferable mode of the present invention, in the step (1), the noble metal solution is one or both of a Pt noble metal solution and a Rh noble metal solution.
In a preferred embodiment of the present invention, in the step (2), the mass fraction of the noble metal in the coating liquid is 0.05% to 2%.
As a preferable scheme of the invention, in the step (1), the alkaline solution is one or more of ammonia water, monoethanolamine, ethylenediamine and triethylamine.
As a preferable aspect of the present invention, in the step (3), the coating liquid is applied to the semi-finished product by using a vacuum suction apparatus having a negative pressure of 15kpa.
The precious metal can be quantitatively added at a fixed height by controlling the adding amount of the precious metal solution and the vacuum degree of the vacuum suction equipment, so that the saving rate of the precious metal in the coating process is greatly improved, and the cost is reduced.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the preparation method of the three-way catalyst comprises the steps of preparing precious metal powder into slurry, and coating to obtain a semi-finished product; and then mixing the noble metal solution with pH =0-3 with a dispersant and a reducing agent, and performing secondary coating to prepare the catalyst with high noble metal surface concentration, increased noble metal utilization rate, simple coating process and excellent performance. The preparation method is particularly suitable for preparing the motorcycle catalyst with small carrier.
2. According to the preparation method of the three-way catalyst, the pH value of the noble metal solution is adjusted to be =0-3, so that the acidity of the solution is reduced, the risk of coating shedding caused by corrosion of the acid solution on the base coat is avoided, and the stability of the catalyst is improved.
Drawings
FIG. 1 shows the results of CO emissions tests of the catalyst of the present invention on a motorcycle.
FIG. 2 shows the results of a NO emission test of the catalyst of the present invention on a motorcycle.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
1. The metal carrier is adopted, and the specification of the metal carrier is as follows: the number of the holes is 300 cells/in 2 Wall thickness 1.5 mm, size Φ 53 mm (diameter) 100 (shell length) 90 (core length). Roasting the carrier at 950 ℃ for 4h to prepare overgrown Al 2 O 3 A carrier for the crystalline material. The carrier was immersed in a silica adhesive, excess slurry was blown out with air, and dried with 150 ℃ air to form a transition layer on the surface of the carrier.
2. Coating a bottom layer: loading platinum nitrate solution on CeO by adopting an isometric immersion method 2 -ZrO 2 (wherein CeO) 2 Content 40%); loading rhodium nitrate on La-Al by the same method 2 O 3 (ii) a Drying and roasting to obtain noble metal Pt powder and Rh powder.
Mixing the Pt powder, rh powder and alumina sol, wherein the proportion of Pt to Rh is 4:7; the binder accounts for 5 percent, and the slurry with the solid content of 45 percent is obtained after ball milling for 10 min. Then, immersing the metal carrier treated in the step 1 into the slurry, taking out, blowing off the redundant slurry in the pore channel, drying and roasting to obtain a semi-finished product; the loading amount on the coating is 120g/L, and the particle size of the slurry is controlled to be 3-10 mu m.
3. Weighing 20 parts by weight of polyacrylamide, adding 980 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed polyacrylamide solution with the mass fraction of 2%; adding 1 part by weight of glycol solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 850mpa.s.
4. And (3) treating the noble metal solution: taking a platinum nitrate solution, adding ammonia water into the platinum nitrate solution, and adjusting the pH of the platinum nitrate solution to be =1.6.
5. And adding the dispersion solution into the treated platinum nitrate solution, and uniformly stirring. A coating solution with the mass fraction of the noble metal Pt of 0.14% was obtained.
6. Weighing 30g of coating liquid, placing the coating liquid on the semi-finished product obtained in the step 2, controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying the catalyst semi-finished product in a hot air oven at 70 ℃ for 4 hours, and roasting the catalyst semi-finished product at 500 ℃ for 1 hour to obtain a finished product. (the noble metal ratio is Pt: rh =7:4, the content is 15g/ft 3 ）
Example 2
Steps 1 and 2 are the same as those in example 1. Wherein the proportion of Pt and Rh is 8:1.
3. Weighing 10 parts by weight of xanthan gum, adding 990 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed xanthan gum solution with the mass fraction of 1%; adding 1 part by weight of glycerol solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 1500mpa.s.
4. And (3) treating the noble metal solution: weighing rhodium nitrate, adding monoethanolamine into the rhodium nitrate solution, and adjusting the pH =2.5 of the rhodium nitrate solution.
5. And adding the dispersion solution into the treated rhodium nitrate solution, and uniformly stirring. A coating solution having a mass fraction of the noble metal Rh of 0.09% was obtained.
6. Weighing 30g of coating liquid, placing the coating liquid on the semi-finished product obtained in the step 2, controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying the catalyst semi-finished product in a hot air oven at 70 ℃ for 4 hours, and roasting the catalyst semi-finished product at 500 ℃ for 1 hour to obtain a finished product. (the noble metal proportion is Pt: rh =7:4, the content is 15g/ft 3 ）
Example 3
Steps 1 and 2 are the same as those in example 1. The proportion of Pt and Rh is 0:1.
3. Weighing 10 parts by weight of hydroxyethyl cellulose, adding 980 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed hydroxyethyl cellulose solution with the mass fraction of 1%; adding 1 part by weight of isopropanol solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 4000mpa.s
4. And (3) treating the noble metal solution: taking a platinum nitrate solution, adding triethylamine to the platinum nitrate solution, and adjusting the pH =2 of the platinum nitrate solution.
5. Adding the dispersion solution into the treated noble metal solution, and uniformly stirring. A coating solution having a mass fraction of the noble metal Pt of 0.21% was obtained.
6. Weighing 30g of coating liquid, placing the coating liquid on the semi-finished product obtained in the step 2, controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying the catalyst semi-finished product in a hot air oven at 70 ℃ for 4 hours, and roasting the catalyst semi-finished product at 500 ℃ for 1 hour to obtain a finished product. (the noble metal proportion is Pt: rh =7:4, the content is 15g/ft 3 ）
Example 4
Steps 1 and 2 were the same as those in example 1. Wherein the proportion of Pt and Rh is 2:1.
3. Weighing 10 parts by weight of polyacrylamide and 10 parts by weight of xanthan gum, adding 980 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed hydroxyethyl cellulose solution with the mass fraction of 1%; adding 0.65 part by weight of ascorbic acid solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 1000mpa.s
4. And (3) treating the noble metal solution: mixing platinum nitrate and rhodium nitrate solution, wherein the proportion of Pt and Rh is 5:3, and adding diethylamine to adjust the pH =1.5 of the noble metal solution.
5. Adding the dispersion solution into the treated noble metal solution, and uniformly stirring. To obtain a coating liquid containing 0.10 mass% of the noble metal Pt and 0.06 mass% of Rh.
6. Weighing 30g of coating liquid, and placing in the step 2 to obtain a semi-finished productAnd (3) controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying in a hot air oven at 70 ℃ for 4h, and then roasting at 500 ℃ for 1h to obtain the finished product. (the noble metal ratio is Pt: rh =7:4, the content is 15g/ft 3 ）
Example 5
Steps 1 and 2 were the same as those in example 1. Wherein the proportion of Pt and Rh is 2:1.
3. Weighing 20 parts by weight of polyvinyl alcohol, adding 980 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed hydroxyethyl cellulose solution with the mass fraction of 1%; adding 0.5 part by weight of glucose solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 1000mpa.s
4. And (3) treating the noble metal solution: weighing platinum nitrate and rhodium nitrate solution, mixing, wherein the proportion of Pt and Rh is 5:3, and adding diethylamine to adjust the pH of the noble metal solution to be =3.
5. Adding the dispersion solution into the treated noble metal solution, and uniformly stirring. To obtain a coating liquid containing 0.10 mass% of the noble metal Pt and 0.06 mass% of Rh.
6. Weighing 30g of coating liquid, placing the coating liquid on the semi-finished product obtained in the step 2, controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying the catalyst semi-finished product in a hot air oven at 70 ℃ for 4 hours, and roasting the catalyst semi-finished product at 500 ℃ for 1 hour to obtain a finished product. (the noble metal proportion is Pt: rh =7:4, the content is 15g/ft 3 ）
Example 6
Steps 1 and 2 are the same as those in example 1. The mixing ratio of Pt and Rh is 2:1.
3. Weighing 20 parts by weight of polyacrylamide, adding 980 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed hydroxyethyl cellulose solution with the mass fraction of 1%; adding 2 parts by weight of magnesium citrate solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 1000mpa.s
4. And (3) treating the noble metal solution: weighing platinum nitrate and rhodium nitrate solution, mixing, wherein the proportion of Pt and Rh is 5:3, and adding diethylamine to adjust the pH =1 of the noble metal solution.
5. Adding the dispersion solution into the treated noble metal solution, and stirring uniformly. To obtain a coating liquid containing 0.10 mass% of the noble metal Pt and 0.06 mass% of Rh.
6. Weighing 30g of coating liquid, placing the coating liquid on the semi-finished product obtained in the step 2, controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying the catalyst semi-finished product in a hot air oven at 70 ℃ for 4 hours, and roasting the catalyst semi-finished product at 500 ℃ for 1 hour to obtain a finished product. (the noble metal proportion is Pt: rh =7:4, the content is 15g/ft 3 ）
Example 7
Steps 1 and 2 are the same as those in example 1. The proportion of Pt and Rh is 2:1.
3. Weighing 10 parts by weight of polyacrylamide and 10 parts by weight of hydroxyethyl cellulose, adding 980 parts by weight of deionized water, and stirring for 2 hours to obtain a uniformly mixed hydroxyethyl cellulose solution with the mass fraction of 1%; adding 2 parts by weight of glycerol solution into the solution, and continuously stirring for 0.5 hour to obtain a dispersion solution, wherein the viscosity of the dispersion solution is as follows: 2000mpa.s
4. And (3) treating the noble metal solution: weighing platinum nitrate and rhodium nitrate solution, mixing, wherein the proportion of Pt and Rh is 5:3, and adding diethylamine to adjust the pH =0.5 of the noble metal solution.
5. Adding the dispersion solution into the treated noble metal solution, and uniformly stirring. To obtain a coating liquid containing 0.10 mass% of the noble metal Pt and 0.06 mass% of Rh.
6. Weighing 30g of coating liquid, placing the coating liquid on the semi-finished product obtained in the step 2, controlling the negative pressure of vacuum suction equipment to be 15kpa, coating the coating liquid on the catalyst semi-finished product, drying the catalyst semi-finished product in a hot air oven at 70 ℃ for 4 hours, and roasting the catalyst semi-finished product at 500 ℃ for 1 hour to obtain a finished product. (the noble metal proportion is Pt: rh =7:4, the content is 15g/ft 3 ）
Comparative example 1
1. The metal carrier is adopted, and the specification of the metal carrier is as follows: the number of holes is 300 cells/in 2 Wall thickness 1.5 mm, size Φ 53 mm (diameter) 100 (shell length) 90 (core length). Roasting the carrier at 950 deg.C for 4h to obtain crystal full of Al2O3The vector of (1). The carrier was immersed in a silica adhesive, excess slurry was blown out with air, and dried with 150 ℃ air to form a transition layer on the surface of the carrier.
2. Coating a bottom layer: weighing a certain amount of noble metal Pt solution, and respectively loading the Pt solution on La-Al by adopting an isovolumetric impregnation method 2 O 3 ，CeO 2 -ZrO 2 (wherein CeO) 2 Content 40%); the precious metal Rh is loaded on the La-Al respectively by the same method 2 O 3 ，CeO 2 -ZrO 2 (wherein CeO) 2 Content 20%); drying and roasting to obtain noble metal Pt powder and Rh powder. And mixing the Pt powder and the Rh powder according to the proportion of Pt to Rh of 7:4, mixing the adhesive and deionized water according to a certain proportion, and ball-milling to prepare slurry; then immersing the treated metal carrier into the slurry, taking out, blowing off the redundant slurry in the pore channel, drying and roasting to obtain a finished product; the loading amount on the coating is 120g/L, and the particle size of the slurry is controlled to be 3-10 mu m. (the noble metal ratio is Pt: rh =7:4, the content is 15g/ft 3 ）
Test example 1
The catalysts obtained in examples 1 to 7 and the catalyst of comparative example 1 were mounted on a motorcycle manufactured by a certain company, and emission tests were carried out by using the WMTC test protocol specified in national standard No. iv of china. The test results are given in table 1 below:
TABLE 1 test results of the catalyst in motorcycles
As is apparent from the data in table 1, the catalysts prepared according to the catalyst preparation method of the present invention have high surface concentrations of the noble metals, and the catalysts of examples 1 to 7 exhibit excellent catalyst performance. Particularly, in the embodiment 3-4, the catalyst product obtained by controlling the pH value, selecting a proper reducing agent and a proper dispersing agent and screening the mixing ratio of Pt and Rh has higher conversion efficiency on CO, THC and NOx, and the CO, THC and NOx in the tail gas are effectively removed.
Comparative example 2
This comparative example differs from example 1 in that the reducing agent ethylene glycol was not added in step 3.
Comparative example 3
This comparative example is different from example 1 in that, in step 4, the hydrogen ion concentration of the noble metal solution was adjusted to 1.5mol/L.
Comparative example 4
The present comparative example differs from example 1 in that in step 4, the pH of the noble metal solution is adjusted to pH =4.
Table 2 results of comparative tests
As can be seen from the data in table 2, comparative example 2 without adding a reducing agent has a poorer effect than example 1, because the addition of the reducing agent makes the active ingredient more easily reduced to an elemental state during the calcination process, which is beneficial to the increase of the active center and the catalytic reaction.
From comparative example 3 and comparative example 4, the effect was poor after adjusting the pH outside the range of pH = 0-3. This is because when pH <0, the solution is too acidic, corrosive to the catalyst, and the catalyst performance is reduced; when the pH is greater than 3, the catalyst activity is lowered, the noble metal is liable to precipitate, and the catalyst performance is lowered.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (7)
1. A preparation method of a three-way catalyst is characterized by comprising the following steps:
(1) Coating a bottom layer: mixing the noble metal powder and the adhesive to prepare slurry, then soaking the treated metal carrier into the slurry, taking out, blowing off redundant slurry in a pore channel, drying and roasting to obtain a semi-finished product;
preparing a dispersion solution: mixing a dispersing agent, a reducing agent and water to obtain a dispersion solution;
preparing a noble metal solution: adding an alkaline solution into the noble metal solution, and adjusting the pH =0-3 to obtain a treated noble metal solution;
the noble metal powder is obtained by loading noble metal on an oxygen storage material or an aluminum oxide material by an isometric impregnation method, drying and roasting; the oxygen storage material comprises CeO 2 ，CeO 2 -ZrO 2 ，CeO 2 -ZrO 2 -Y 2 O 3 ，CeO 2 -ZrO 2 -La 2 O 3 ，CeO 2 -ZrO 2 -La 2 O 3 -Y 2 O 3 One or more of (a); the alumina material includes Al 2 O 3 Rare earth modified Al 2 O 3 And alkaline earth modified Al 2 O 3 One or more of (a);
the dispersing agent comprises one or more of polyacrylamide, xanthan gum, hydroxyethyl cellulose and polyvinyl alcohol;
the reducing agent is one or more of methanol, ethanol, ethylene glycol, isopropanol, glycerol, ascorbic acid, glucose and alkali metal citrate;
(2) Diluting the treated noble metal solution by using the dispersion solution in the step (1) to obtain a coating solution;
(3) And (3) coating the coating liquid obtained in the step (2) on the semi-finished product obtained in the step (1), drying and roasting to obtain a catalyst finished product.
2. The method of preparing a three-way catalyst according to claim 1, wherein in step (1), the noble metal is one or both of Pt and Rh.
3. The preparation method of the three-way catalyst according to claim 1, characterized in that in the step (1), the particle size of the slurry is 3-10 μm and the loading amount on the coating is 100-200g/L when the bottom layer is coated.
4. The method for preparing a three-way catalyst according to claim 1, wherein in the step (1), the mass fraction of the dispersant in the dispersion solution is 0.5 to 2.5%.
5. The method for preparing a three-way catalyst according to claim 1, wherein in the step (1), the mass ratio of the reducing agent to the dispersing agent is 1.
6. The method for preparing a three-way catalyst according to claim 1, wherein in the step (1), the viscosity of the dispersion solution is 500 to 5000mpa.s.
7. The method for preparing a three-way catalyst according to claim 1, wherein in the step (2), the mass fraction of the noble metal in the coating liquid is 0.05-2%.
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