CN105817230B - The preparation method of ternary tail-gas catalyst - Google Patents
The preparation method of ternary tail-gas catalyst Download PDFInfo
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- CN105817230B CN105817230B CN201610267753.8A CN201610267753A CN105817230B CN 105817230 B CN105817230 B CN 105817230B CN 201610267753 A CN201610267753 A CN 201610267753A CN 105817230 B CN105817230 B CN 105817230B
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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
- 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
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20753—Nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
Abstract
The present invention relates to auto-exhaust catalyst, the specifically preparation method of ternary tail-gas catalyst, it is included zirconium oxide, cerium oxide and nickel powder mixing and ball milling by mass fraction, and then addition alumina powder continuation ball milling, obtains composite powder；Above-mentioned composite powder is configured to slurry with deionized water, then pretreated cordierite carrier is immersed in slurry；Then take out, and blow away slurry unnecessary in duct, then dried, roasted, obtain catalyst.The present invention refines catalyst fines particle by ball milling, its crystallite dimension reaches nanoscale；Meanwhile noble metal is substituted using transiting metal nickel part, since nickel is there are multiple states of oxidation, there is active redox property so that the activity of catalyst is improved, while reduces the cost of catalyst.
Description
Technical field
The present invention relates to the preparation method of auto-exhaust catalyst, specifically ternary tail-gas catalyst.
Background technology
With the increase of car ownership, CO, HC, NO that automobile is discharged into airXIt is more and more.At present, many states
Family has taken motor vehicle exhaust emission stringent control emission measure.Therefore the processing of vehicle exhaust has become important
Problem.In the prior art, the control to motor vehicle exhaust emission is realized by installing catalytic cleaner additional, and catalytic cleaner
Key be catalyst.Catalyst generally use three-decker is made of active component, washcoat and carrier.From rare earth calcium
Titanium ore oxide（PTO）Since tail gas catalyzed, since its A, B position can substitute and Lacking oxygen is produced, while such is urged
Agent has noble metal catalyst larger price advantage so that such catalyst becomes the hot spot of research.It is but existing single
The PTO catalytic performances of component are bad, stability is poor, it is impossible to meet increasingly serious motor vehicle exhaust emission pollution.
The content of the invention
For above-mentioned technical problem, the present invention provides a kind of system of stable, the lower-cost ternary tail-gas catalyst of performance
Preparation Method.
The technical solution adopted by the present invention is：The preparation method of ternary tail-gas catalyst, it comprises the following steps：
（1）By mass fraction by zirconium oxide, cerium oxide and nickel powder mixing and ball milling, then add alumina powder and continue ball milling,
Obtain composite powder；
（2）Above-mentioned composite powder is configured to slurry with deionized water, then pretreated cordierite carrier is immersed and is starched
In material；
（3）Then take out, and blow away slurry unnecessary in duct, then dried, roasted.
Preferably, in the composite powder, zirconium oxide accounts for 4-8wt%, and cerium oxide accounts for 15-20wt%, nickel accounts for 2-
4wt%, surplus are aluminium oxide.
Preferably, the mixing and ball milling time is 30-50h, continuation Ball-milling Time is 20-40h.
Preferably, ball milling uses the rotating speed of 180-220r/min, ratio of grinding media to material is（9—10）:1.
Preferably, step（2）In the immersion time be 2min..
Preferably, step（3）Using 130 DEG C of dry 3h, 600 DEG C of roasting 1h.
Preferably, then the pretreatment of the cordierite uses deionized water using the salpeter solution immersion 1h of 1mol/L
Cleaning, last 120 DEG C dry 3h.
As can be known from the above technical solutions, the present invention refines catalyst fines particle by ball milling, its crystallite dimension reaches
Nanoscale；Meanwhile noble metal is substituted using transiting metal nickel part, since nickel is there are multiple states of oxidation, there is active oxygen
Change reducing property so that the activity of catalyst is improved, while reduces the cost of catalyst.
Embodiment
The present invention is described more detail below, illustrative examples of the invention and explanation are used for explaining the present invention herein,
It is but not as a limitation of the invention.
The preparation method of ternary tail-gas catalyst, it comprises the following steps：
First by mass fraction by zirconium oxide, cerium oxide and nickel powder 30-50h of mixing and ball milling, add aluminium oxide and continue ball
Consume time 20-40h, obtains composite powder, and wherein zirconium oxide accounts for 4-8wt%, and cerium oxide accounts for 15-20wt%, and nickel accounts for 2-4wt%,
Surplus is aluminium oxide；The rotating speed of 180-220r/min is used in mechanical milling process,（9—10）:1 ratio of grinding media to material, can so obtain
Nano level composite powder.It is raw since stress-induced isomer phase transformation can occur for aluminium oxide ball milling in mechanical milling process
Into α-Al2O3It is unfavorable to catalytic performance, so should participate in grinding again after ball milling zirconium oxide, cerium oxide and nickel powder；And nickel powder exists
Ball milling there is very strong cold welding to act at early period, therefore should be mixed together ball milling with zirconium oxide, cerium oxide early period, otherwise be difficult thin
Change.The present invention first avoids aluminium oxide and only ball milling zirconium oxide, cerium oxide and nickel powder to a certain extent, then add aluminium oxide and continue
Ball milling, can be such that zirconium oxide is dissolved into completely in cerium oxide, reduce the lattice constant of cerium oxide, while can make nickel highly dispersed in oxygen
In the solid solution for changing cerium-cerium oxide；Therefore, this ball-milling technology can not only obtain cerium oxide-oxidation cerium solid solution, but also refine
Nickel powder, whole composite powder particle diameter can reach 60-90nm.
It is last to obtain nanometer grade composit powder, is configured to slurry with deionized water, then pretreated cordierite carrier is soaked
Enter in slurry, taken out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130 DEG C
Dry 3h, 600 DEG C of roasting 1h, can so obtain the catalyst of even compact on carrier.The pretreatment of cordierite uses 1mol/
The salpeter solution immersion 1h of L, is then cleaned, last 120 DEG C dry 3h with deionized water；Greatly promote the performance of catalyst.
Embodiment 1
Zirconium oxide, cerium oxide and nickel powder are mixed by mass fraction, using the rotating speed of 180r/min, 9:1 ratio of grinding media to material ball
30h is ground, aluminium oxide is added and continues Ball-milling Time 20h, obtain composite powder, wherein zirconium oxide accounts for 4wt%, and cerium oxide accounts for
15wt%, nickel account for 2wt%, and surplus is aluminium oxide；Then composite powder is configured to slurry with deionized water, then adopts cordierite
1h is soaked with the salpeter solution of 1mol/L, is then cleaned with deionized water, last 120 DEG C dry 3h postcoolings, are re-used as carrier
Immerse in slurry, taken out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130
DEG C dry 3h, 600 DEG C of roasting 1h, obtain three-way catalyst；The catalyst is tested, its conversion ratio to CO, HC and NO
Reach 96.7%, initiation temperature is between 190-210 DEG C.
Embodiment 2
Zirconium oxide, cerium oxide and nickel powder are mixed by mass fraction, using the rotating speed of 200r/min, 10:1 ratio of grinding media to material ball
40h is ground, aluminium oxide is added and continues Ball-milling Time 30h, obtain composite powder, wherein zirconium oxide accounts for 6wt%, and cerium oxide accounts for
18wt%, nickel account for 3wt%, and surplus is aluminium oxide；Then composite powder is configured to slurry with deionized water, then adopts cordierite
1h is soaked with the salpeter solution of 1mol/L, is then cleaned with deionized water, last 120 DEG C dry 3h postcoolings, are re-used as carrier
Immerse in slurry, taken out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130
DEG C dry 3h, 600 DEG C of roasting 1h, obtain three-way catalyst；The catalyst is tested, its conversion ratio to CO, HC and NO
Reach 97.2%, initiation temperature is between 170-190 DEG C.
Embodiment 3
Zirconium oxide, cerium oxide and nickel powder are mixed by mass fraction, using the rotating speed of 220r/min, 10:1 ratio of grinding media to material ball
50h is ground, aluminium oxide is added and continues Ball-milling Time 40h, obtain composite powder, wherein zirconium oxide accounts for 8wt%, and cerium oxide accounts for
20wt%, nickel account for 4wt%, and surplus is aluminium oxide；Then composite powder is configured to slurry with deionized water, then adopts cordierite
1h is soaked with the salpeter solution of 1mol/L, is then cleaned with deionized water, last 120 DEG C dry 3h postcoolings, are re-used as carrier
Immerse in slurry, taken out after about 1min, and blow away slurry unnecessary in duct, immerse 1min in slurry after drying again, then 130
DEG C dry 3h, 600 DEG C of roasting 1h, obtain three-way catalyst；The catalyst is tested, its conversion ratio to CO, HC and NO
Reach 97%, initiation temperature is between 170-190 DEG C.
The technical solution provided above the embodiment of the present invention is described in detail, specific case used herein
The principle and embodiment of the embodiment of the present invention are set forth, the explanation of above example is only applicable to help and understands this
The principle of inventive embodiments；Meanwhile for those of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
There will be changes in formula and application range, in conclusion this specification content should not be construed as limiting the invention.
Claims (6)
1. the preparation method of ternary tail-gas catalyst, it comprises the following steps：
（1）By mass fraction by zirconium oxide, cerium oxide and nickel powder mixing and ball milling, then add alumina powder and continue ball milling, obtain
Composite powder；
（2）Above-mentioned composite powder is configured to slurry with deionized water, then pretreated cordierite carrier is immersed in slurry；
（3）Then take out, and blow away slurry unnecessary in duct, then dried, roasted；In the composite powder, zirconium oxide
4-8wt% is accounted for, cerium oxide accounts for 15-20wt%, and nickel accounts for 2-4wt%, and surplus is aluminium oxide.
2. the preparation method of ternary tail-gas catalyst according to claim 1, it is characterised in that：The mixing and ball milling time for 30-
50h, continuation Ball-milling Time are 20-40h.
3. the preparation method of ternary tail-gas catalyst according to claim 1, it is characterised in that：Ball milling uses 180-220r/
The rotating speed of min, ratio of grinding media to material are（9—10）:1.
4. the preparation method of ternary tail-gas catalyst according to claim 1, it is characterised in that：Step（2）In immersion when
Between be 2min.
5. the preparation method of ternary tail-gas catalyst according to claim 1, it is characterised in that：Step（3）It is dry using 130 DEG C
Dry 3h, 600 DEG C of roasting 1h.
6. the preparation method of ternary tail-gas catalyst according to claim 1, it is characterised in that：The pretreatment of the cordierite
1h is soaked using the salpeter solution of 1mol/L, is then cleaned with deionized water, last 120 DEG C dry 3h.
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| CN201610267753.8A CN105817230B (en) | 2016-04-27 | 2016-04-27 | The preparation method of ternary tail-gas catalyst |
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| CN105817230B true CN105817230B (en) | 2018-04-24 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100427208C (en) * | 2006-01-19 | 2008-10-22 | 清华大学 | Method for preparing catalyst to purify automobile tail gas |
| GB2477630B (en) * | 2010-02-01 | 2014-11-12 | Johnson Matthey Plc | Filter comprising combined soot oxidation and nh3-scr catalyst |
| CN102762827B (en) * | 2010-04-14 | 2014-12-24 | 尤米科尔股份公司及两合公司 | Reduction-catalyst-coated diesel particle filter having improved characteristics |
| CN104190438B (en) * | 2014-08-12 | 2017-02-01 | 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: 20160803 Assignee: LIUZHOU YAXIANG TECHNOLOGY Co.,Ltd. Assignor: LIUZHOU SHENTONG AUTOMOBILE TECHNOLOGY Co.,Ltd. Contract record no.: 2018450000032 Denomination of invention: Preparation method of ternary tail gas catalyst Granted publication date: 20180424 License type: Common License Record date: 20180803 |
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Effective date of registration: 20230105 Address after: 545616 room 2-2, 2nd floor, No.60 zhengtongdao, Luorong Town, Liuzhou City, Guangxi Zhuang Autonomous Region Patentee after: Liuzhou Xinkai Chaohua Technology Co.,Ltd. Address before: 545000 Liudong New District, Liuzhou City, Guangxi Zhuang Autonomous Region, No. 2 Shuiwan Road, No. 2 Liudong Standard Factory Building, Second Floor 212 Patentee before: LIUZHOU SHENTONG AUTOMOBILE TECHNOLOGY Co.,Ltd. |
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