CN105797737A - Preparation method of ternary catalyst - Google Patents
Preparation method of ternary catalyst Download PDFInfo
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- CN105797737A CN105797737A CN201610268279.0A CN201610268279A CN105797737A CN 105797737 A CN105797737 A CN 105797737A CN 201610268279 A CN201610268279 A CN 201610268279A CN 105797737 A CN105797737 A CN 105797737A
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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
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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
- B01J23/83—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 rare earths or actinides
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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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention relates to an automobile tail gas catalyst, in particular relates to a preparation process of a ternary catalyst. The preparation process comprises the following steps: mixing and carrying out ball milling on zirconium oxide, cerium oxide and nickel powder according to the mass parts; then adding aluminum oxide powder and continually carrying out ball milling to obtain compound powder; preparing the compound powder into paste with de-ionized water; immersing a carrier, and drying and roasting; then immersing the carrier into an ammine chloropalladium solution; taking out the product, and drying, roasting and cooling to obtain the catalyst. By carrying out ball milling to refine catalyst powder particles, the size of crystal grains reaches a nano grade; meanwhile, transition metal nickel is used for partially replacing noble metal; the nickel has a plurality of oxidization states and has an active oxidation-reduction property, so that the activity of the catalyst is improved; meanwhile, the cost of the catalyst is reduced; the carrier is further plated with palladium, and the ternary catalyst has a uniform and dense plated layer, good chemical stability, high rigidity, good lubricating property and strong abrasion resistance and anti-scratching capability.
Description
Technical field
The present invention relates to auto-exhaust catalyst, the preparation method of specifically a kind of three-way catalyst.
Background technology
Along with the increase of automobile pollution, CO, HC, NO that automobile discharges in airXMore and more.At present, motor vehicle exhaust emission has been taken strict control emission measure by many countries.Therefore the process of vehicle exhaust is increasingly becoming important problem.In the prior art, be realize by installing catalytic cleaner additional the control of motor vehicle exhaust emission, and catalytic cleaner it is crucial that catalyst.Catalyst generally adopts three-decker to be namely made up of active component, washcoat and carrier.From RE perovskite oxide (PTO) for since tail gas catalyzed, having produced Lacking oxygen owing to its A, B position can replace, noble metal catalyst is had bigger price advantage by such catalyst simultaneously so that such catalyst becomes the focus of research.But, the PTO catalytic performance of existing one-component is not good, poor stability, it is impossible to meets increasingly serious motor vehicle exhaust emission and pollutes.
Summary of the invention
For above-mentioned technical problem, the preparation method that the present invention provides a kind of stable performance, lower-cost three-way catalyst.
The technical solution used in the present invention is: the preparation method of a kind of catalytic agent, and it comprises the following steps:
(1) by mass fraction by zirconium oxide, cerium oxide and nikel powder mixing and ball milling, it is subsequently adding alumina powder and continues ball milling, obtain composite powder；
(2) above-mentioned composite powder deionized water is configured to slurry, more pretreated cordierite carrier is immersed in slurry, then take out, and blow away slurry unnecessary in duct, then carry out drying, roasting；
(3) then carrier is immersed in Palladous chloride. ammonia solution, then take out dry, roasting, it is thus achieved that catalyst.
As preferably, in described composite powder, zirconium oxide accounts for 4 8wt%, and cerium oxide accounts for 15 20wt%, and nickel accounts for 2 4wt%, and surplus is aluminium oxide.
As preferably, the mixing and ball milling time is 30 50h, and continuing Ball-milling Time is 20 40h.
As preferably, ball milling adopts the rotating speed of 180 220r/min, and ratio of grinding media to material is (9 10): 1.
As preferably, the immersion time in step (2) is 2min, adopts 130 DEG C of dry 3h, 600 DEG C of roasting 1h.
As preferably, in step (3), the concentration of Palladous chloride. ammonia solution is 1g/L, and the immersion time is 3h, adopts 120 DEG C of dry 4h, 500 DEG C of roasting 2h.
As can be known from the above technical solutions, the present invention makes catalyst fines grain refine by ball milling, and its crystallite dimension reaches nanoscale；Meanwhile, adopt transiting metal nickel part to replace noble metal, owing to nickel exists multiple state of oxidation, there is active redox property so that the activity of catalyst improves, reduce the cost of catalyst simultaneously；The present invention also carries out plating palladium on carrier, and not only coating is uniform, fine and close, and chemical stability is good, and hardness is high, and lubricity is good, resistance to wears and anti-scuffing function is strong.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
A kind of preparation method of three-way catalyst, it comprises the following steps:
First pressing mass fraction by zirconium oxide, cerium oxide and nikel powder mixing and ball milling 30 50h, add aluminium oxide and continue Ball-milling Time 20 40h, obtain composite powder, wherein zirconium oxide accounts for 4 8wt%, and cerium oxide accounts for 15 20wt%, and nickel accounts for 2 4wt%, and surplus is aluminium oxide；Mechanical milling process adopts the rotating speed of 180 220r/min, (9 10): the ratio of grinding media to material of 1, so can obtain nano level composite powder.In mechanical milling process, owing to stress-induced isomer phase transformation can occur aluminium oxide ball milling, the α-Al of generation2O3Catalytic performance is unfavorable, so should participate in again grinding after ball milling zirconium oxide, cerium oxide and nikel powder；And nikel powder has very strong cold welding effect in ball milling early stage, therefore answer early stage and zirconium oxide, cerium oxide to be mixed together ball milling, be otherwise difficult to refinement.The present invention first avoids aluminium oxide and only ball milling zirconium oxide, cerium oxide and nikel powder be to a certain extent, then add aluminium oxide and continue ball milling, zirconium oxide can be made to be solidly soluted into completely in cerium oxide, reduce the lattice paprmeter of cerium oxide, can make nickel highly dispersed in the solid solution of cerium oxide-cerium oxide simultaneously；Therefore, this ball-milling technology not only can obtain cerium oxide-cerium oxide solid solution, and has refined nikel powder, and whole composite powder particle diameter can reach 60 90nm.
Acquisition nanometer grade composit powder is last, it is configured to slurry with deionized water, again pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immersing 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h, so can obtain the impregnating slurry layer of even compact on carrier.
After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, make absorption palladium ion on carrier, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, it is thus achieved that be impregnated with the catalyst of palladium.
Embodiment 1
By mass fraction, zirconium oxide, cerium oxide and nikel powder are mixed, adopt the rotating speed of 180r/min, the ratio of grinding media to material ball milling 30h of 9:1, adding aluminium oxide and continue Ball-milling Time 20h, obtain composite powder, wherein zirconium oxide accounts for 4wt%, cerium oxide accounts for 15wt%, and nickel accounts for 2wt%, and surplus is aluminium oxide；Followed by deionized water, composite powder is configured to slurry, then pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h；After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, it is thus achieved that palladium load capacity is the catalyst of 1g/L；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 97.1% by it, and initiation temperature is between 180 200 DEG C.
Embodiment 2
By mass fraction, zirconium oxide, cerium oxide and nikel powder are mixed, adopt the rotating speed of 200r/min, the ratio of grinding media to material ball milling 40h of 10:1, adding aluminium oxide and continue Ball-milling Time 30h, obtain composite powder, wherein zirconium oxide accounts for 6wt%, cerium oxide accounts for 18wt%, and nickel accounts for 3wt%, and surplus is aluminium oxide；Followed by deionized water, composite powder is configured to slurry, then pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h；After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, it is thus achieved that palladium load capacity is the catalyst of 2g/L；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98.1% by it, and initiation temperature is between 160 180 DEG C.
Embodiment 3
By mass fraction, zirconium oxide, cerium oxide and nikel powder are mixed, adopt the rotating speed of 220r/min, the ratio of grinding media to material ball milling 50h of 10:1, adding aluminium oxide and continue Ball-milling Time 40h, obtain composite powder, wherein zirconium oxide accounts for 8wt%, cerium oxide accounts for 20wt%, and nickel accounts for 4wt%, and surplus is aluminium oxide；Followed by deionized water, composite powder is configured to slurry, then pretreated cordierite carrier is immersed in slurry, take out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C of dry 3h, 600 DEG C of roasting 1h；After slurry coats, carrier is immersed in the Palladous chloride. ammonia solution of 1g/L, magnetic agitation 4h, then take out, blow down redundant solution, dry, adopt 120 DEG C of dry 4h, 500 DEG C of roasting 2h, it is thus achieved that palladium load capacity is the catalyst of 2g/L；This catalyst is tested, and the conversion ratio of CO, HC and NO is reached 98.2% by it, and initiation temperature is between 150 170 DEG C.
The technical scheme above embodiment of the present invention provided is described in detail, principle and the embodiment of the embodiment of the present invention are set forth by specific case used herein, and the explanation of above example is only applicable to help to understand the principle of the embodiment of the present invention；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, all will change in detailed description of the invention and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (6)
1. a preparation method for three-way catalyst, it comprises the following steps:
(1) by mass fraction by zirconium oxide, cerium oxide and nikel powder mixing and ball milling, it is subsequently adding alumina powder and continues ball milling, obtain composite powder；
(2) above-mentioned composite powder deionized water is configured to slurry, more pretreated cordierite carrier is immersed in slurry, then take out, and blow away slurry unnecessary in duct, then carry out drying, roasting；
(3) then carrier is immersed in Palladous chloride. ammonia solution, then take out dry, roasting, it is thus achieved that catalyst.
2. the preparation method of three-way catalyst according to claim 1, it is characterised in that: in described composite powder, zirconium oxide accounts for 4 8wt%, and cerium oxide accounts for 15 20wt%, and nickel accounts for 2 4wt%, and surplus is aluminium oxide.
3. the preparation method of three-way catalyst according to claim 1, it is characterised in that: the mixing and ball milling time is 30 50h, and continuing Ball-milling Time is 20 40h.
4. the preparation method of three-way catalyst according to claim 1, it is characterised in that: ball milling adopts the rotating speed of 180 220r/min, and ratio of grinding media to material is (9 10): 1.
5. the preparation method of three-way catalyst according to claim 1, it is characterised in that: the immersion time in step (2) is 2min, adopts 130 DEG C of dry 3h, 600 DEG C of roasting 1h.
6. the preparation method of three-way catalyst according to claim 1, it is characterised in that: in step (3), the concentration of Palladous chloride. ammonia solution is 1g/L, and the immersion time is 3h, adopts 120 DEG C of dry 4h, 500 DEG C of roasting 2h.
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| CN201610268279.0A CN105797737B (en) | 2016-04-27 | 2016-04-27 | A kind of preparation method of three-way catalyst |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003023A (en) * | 2006-01-19 | 2007-07-25 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| WO2011092521A1 (en) * | 2010-02-01 | 2011-08-04 | Johnson Matthey Plc | Extruded scr filter |
| US20130004391A1 (en) * | 2010-04-14 | 2013-01-03 | Umicore Ag & Co. Kg | Reduction-catalyst-coated diesel particle filter having improved characteristics |
| CN104190438A (en) * | 2014-08-12 | 2014-12-10 | 淄博加华新材料资源有限公司 | High-performance cerium zirconium oxide and production method of high-performance cerium zirconium oxide |
| CN104772162A (en) * | 2015-04-11 | 2015-07-15 | 桂林理工大学 | Zr-Ce-Mn-Fe/ZSM-5 composite oxide catalyst for NOx reduction by using low-temperature NH3 and preparation method thereof |
-
2016
- 2016-04-27 CN CN201610268279.0A patent/CN105797737B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101003023A (en) * | 2006-01-19 | 2007-07-25 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| WO2011092521A1 (en) * | 2010-02-01 | 2011-08-04 | Johnson Matthey Plc | Extruded scr filter |
| US20130004391A1 (en) * | 2010-04-14 | 2013-01-03 | Umicore Ag & Co. Kg | Reduction-catalyst-coated diesel particle filter having improved characteristics |
| CN104190438A (en) * | 2014-08-12 | 2014-12-10 | 淄博加华新材料资源有限公司 | High-performance cerium zirconium oxide and production method of high-performance cerium zirconium oxide |
| CN104772162A (en) * | 2015-04-11 | 2015-07-15 | 桂林理工大学 | Zr-Ce-Mn-Fe/ZSM-5 composite oxide catalyst for NOx reduction by using low-temperature NH3 and preparation method thereof |
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Application publication date: 20160727 Assignee: Liuzhou Yaxiang Technology Co. Ltd. Assignor: LIUZHOU SHENTONG AUTOMOBILE TECHNOLOGY CO., LTD. Contract record no.: 2018450000033 Denomination of invention: Preparation method of three-way catalyst Granted publication date: 20180424 License type: Common License Record date: 20180803 |