CN102500396A - Perovskite type oxide catalyst and preparation method thereof - Google Patents
Perovskite type oxide catalyst and preparation method thereof Download PDFInfo
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- CN102500396A CN102500396A CN2011103654390A CN201110365439A CN102500396A CN 102500396 A CN102500396 A CN 102500396A CN 2011103654390 A CN2011103654390 A CN 2011103654390A CN 201110365439 A CN201110365439 A CN 201110365439A CN 102500396 A CN102500396 A CN 102500396A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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Abstract
The invention discloses a perovskite type oxide catalyst and a preparation method thereof. The perovskite type oxide catalyst comprises a catalyst which is prepared according to a general formula of AxA'1-xByB'1-y-zPdzO3, wherein A represents a rare earth metal element; A' represents an alkaline metal element; B and B' represent different transition metal elements; x is greater than or equal to 0.6 and is less than or equal to 0.9; y is greater than or equal to 0 and is less than or equal to 0.5; and z is greater than 0 and is less than or equal to 0.1. The preparation method comprises the following steps of: dissolving a certain amount of nitrate of each said metal according to a stoichiometric ratio; adding citric acid as a complexing agent to prepare a citric acid complex; then adding palladium nitrate; and performing a high-temperature explosion method for synthesis after the citric acid is used for complexing. Through the catalyst prepared by the invention, carbon oxide and nitrogen oxide in motorcycle tail gas can be effectively reduced; the preparation method is more stable, the preparation process has easily controlled conditions, the repeatability is excellent, higher economy is realized, the nitrate is adopted for dissolving, each component is prepared by using a dissolving preparation method, and the steps are simplified; the preparation effect is better, and the catalyst performance is superior; and the oxide is introduced into the motorcycle catalyst, and the cost of the catalyst can be effectively reduced under the condition of guaranteeing the performance of the catalyst.
Description
Technical field
The invention belongs to catalyst preparation technical field, especially belong to the perofskite type oxide catalyst preparation technical field, particularly a kind of perofskite type oxide catalyst and preparation thereof that is used for motorcycle tail gas cleaning.
Background technology
The motorcycle emission contaminant problems is serious day by day, and for reducing the discharge capacity of pollutant in the motorcycle exhaust, country constantly promotes the discharge standard of motorcycle, and this just impels the researcher constantly to promote the vent gas treatment technology.At present, mainly be through using catalyst to handle the pollutant carbon monoxide in the motorcycle exhaust, nitrogen oxide, hydrocarbon.Along with the development of motorcycle industry, reduce catalyst cost (the catalyst prime cost is a noble metal dosage), improve the important requirement that catalyst performance becomes depot.Simultaneously, the difficult point of motorcycle exhaust processing is carbon monoxide, the conversion of nitrogen oxide.
Preparation of Catalyst is the very strong science of practicality; The catalyst performance of its preparation of difference of details such as different environment, different process, various conditions is very different, and this also is that the catalyst theory and practice also needs constantly to make great efforts the problem that solves probing into always.
Perofskite type oxide is as the at present existing certain research of catalyst, but how to select the combination of each composition, how to select that preparation is more stable, more economical, catalyst performance is more excellent, can effectively strengthen CO+NO → 0.5N
2+ CO
2Reaction, the conversion ratio of enhancing carbon monoxide and nitrogen oxide reduces the catalyst cost, and the motorcycle tail gas cleaning catalyst that combination property is more excellent also has a lot of problems to need constantly to make great efforts solution.
Summary of the invention
The present invention discloses a kind of perofskite type oxide Catalysts and its preparation method according to the deficiency of prior art, and the problem that the present invention will solve provides a kind of more stable, economy, the better perofskite type oxide method for preparing catalyst of processability; Second problem that the present invention solves is to provide a kind of performance more excellent, more economical, CO+NO → 0.5N particularly through said method
2+ CO
2The catalyst that catalytic reaction efficient is higher.
The present invention realizes through following technical scheme:
The perofskite type oxide method for preparing catalyst may further comprise the steps:
(1), forms metering by the perofskite type oxide catalyst and take by weighing corresponding rare-earth metal nitrate, alkaline earth nitrate, transition metal nitrate and palladium nitrate respectively;
(2), with rare-earth metal nitrate, alkaline earth nitrate and transition metal nitrate that (1) step takes by weighing, be dissolved in the deionized water, above-mentioned each metal ion summation is that 6.46-6.79 is than 1 with the mol ratio of deionized water;
(3), by the mol ratio of metal ion summation in (2) step and citric acid be 1 to 1.52 in step (2) gained solution the required weight citric acid of adding, stirring and dissolving;
(4), palladium nitrate that (1) step is taken by weighing is dissolved in the salting liquid that (3) step obtains, stirred 30 minutes;
(5), step (4) gained solution was worn out 2～7 hours under 70～80 ℃ of water bath condition;
(6), with step (5) gained colloidal sol in 500 ℃ the calcining 1 hour, 900 ℃ the calcining 3 hours, obtain black powder;
(7), step (6) gained black powder or black powder and other mixture that need add component are added bonding agent, be prepared into slurries, be coated on the carrier, drying and roasting makes catalyst.
Perofskite type oxide catalyst general formula is:
A
xA’
1-xB
yB’
1-y-zPd
zO
3；
Wherein, A represents thulium; A ' represents alkali earth metal; B and the different transition metal of B ' representative; 0.6≤x≤0.9,0≤y≤0.5,0＜z≤0.1.
Further perofskite type oxide catalyst general formula is:
La
xSr
1-xNi
yCo
1-y-zPd
zO
3；
Wherein: 0.6≤x≤0.9,0≤y≤0.5,0＜z≤0.1.
Preferred perofskite type oxide catalyst is formed: La
0.7Sr
0.3Nu
0.5Co
0.45Pd
0.05O
3
Another preferred version perofskite type oxide catalyst is formed: La
0.7Sr
0.3Co
0.96Pd
0.04O
3
Further also available Ca-Ti ore type oxide catalyst and Pt/Al
2O
3Or Rh/Al
2O
3The preparation of even load catalyst mix is suitable for the catalyst that motorcycle is suitable for.
The high temperature explosion method was synthesized after the present invention adopted citric acid complex; The preparation method is dissolved a certain amount of lanthanum nitrate, strontium nitrate, nickel nitrate, cobalt nitrate by stoichiometric proportion; Add citric acid and process citric acid complex, add palladium nitrate then, heat after several hours as complexing agent; In 500 ℃ of Muffle furnaces, decompose; Be high temperature explosive decomposition method, in 900 ℃ of roasting 3h, make the perovskite oxide powder sample behind the powder pressing of decomposition back.Add bonding agent in this powder, be prepared into slurries, apply on the cordierite ceramic honeycomb carrier, be prepared into single palladium catalyst, it is good and bad to estimate the performance of learning perovskite oxide.
The present invention confirms preparation perofskite type oxide total catalyst weight at first as required when the said catalyst of preparation; Then according to the perofskite type oxide catalyst molecule formula of gross weight, like La with the needs preparation
0.7Sr
0.3Ni
0.5Co
0.45Pd
0.05O
3, calculate the molal quantity of each metal ion; Again with the molal quantity of above-mentioned metal ion according to the different metal salt that adopts, like lanthanum nitrate [La (NO
3)
3.6H
2O], calculate in requisition for slaine weight take by weighing subsequent use; The mol ratio of each metal ion summation and deionized water is meant the metal ion summation of rare earth metal, alkaline-earth metal and transition metal and the mol ratio of deionized water in preparation process (2); The mol ratio of each metal ion summation and citric acid is meant the metal ion summation of rare earth metal, alkaline-earth metal and transition metal and the mol ratio of citric acid in preparation process (3).
This perovskite oxide, can with Pt/Al
2O
3Or Rh/Al
2O
3The mixed preparation of even load catalyst is used, and adds bonding agent, is prepared into slurries, is coated on the metal beehive carrier, and the roasting rear catalyst can be installed in the motorcycle muffler tail pipe, to carbon monoxide in the tail gas, and nitrogen oxide, hydrocarbon transforms.
Method for preparing catalyst of the present invention is more stable, and the preparation process condition is easy to control, and good reproducibility is more economical, adopts the nitrate dissolving, and each composition is all adopted the dissolving preparation method, has simplified step; The preparation better effects if, catalyst performance is more excellent, and through detecting, the catalyst of the present invention's preparation can effectively be strengthened CO+NO → 0.5N
2+ CO
2Reaction, the conversion ratio of raising carbon monoxide and nitrogen oxide; Perovskite oxide technology cost of the present invention is low, simple to operate, can use fast aborning; Simultaneously can effectively reduce the catalyst cost keeping under the constant condition of catalyst performance.The introducing of perovskite oxide of the present invention is high-performance, and catalyst research provides road cheaply.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is further specified, the specific embodiment is to the further specifying of the principle of the invention, and does not limit the present invention in any way, or similar techniques identical with the present invention all do not exceed the scope of the present invention's protection.
Embodiment 1
Perovskite oxide La
0.7Sr
0.3Co
0.96Pd
0.04O
3Preparation
With lanthanum nitrate [La (NO
3)
3.6H
2O] 65.92g, strontium nitrate [Sr (NO
3)
2] 13.74g, cobalt nitrate [Co (NO
3)
2.6H
2O] 61.77g is dissolved in the 62.5ml deionized water, is stirred to dissolving.Then, add citric acid [C
6H
8O
7.H
2O] 135.67g, be stirred to dissolving.Then, with palladium nitrate [Pd (NO
3)
2] 5.06g adds in the metal salt solution, stirs half an hour.Gained solution is aging about 2～7h under 70～80 ℃ of water bath condition.Colloidal sol is in 500 ℃ of calcining 1h after the water-bath, and 900 ℃ of calcining 3h obtain the black powder sample.Add bonding agent in the black powder, be prepared into slurries, be coated in the hole order and count 400cell/in
2, on the volume 2.5ml cordierite ceramic honeycomb carrier, drying and roasting, being bullion content is 40g/ft
3Single palladium catalyst.
Embodiment 2
Perovskite oxide La
0.8Sr
0.2Co
0.96Pd
0.04O
3Preparation
With lanthanum nitrate [La (NO
3)
3.6H
2O] 73.71g, strontium nitrate [Sr (NO
3)
2] 8.96g, cobalt nitrate [Co (NO
3)
2.6H
2O] 60.43g is dissolved in the 62.5ml deionized water, is stirred to dissolving.Then, add citric acid [C
6H
8O
7.H
2O] 132.73g, be stirred to dissolving.Then, with palladium nitrate [Pd (NO
3)
2] 4.95g adds in the metal salt solution, stirs half an hour.Other and embodiment 1 operate equally, obtain black powder sample and 40g/ft
3Single palladium catalyst.
Embodiment 3
Perovskite oxide La
0.9Sr
0.1Ni
0.2Co
0.75Pd
0.05O
3Preparation
With lanthanum nitrate [La (NO
3)
3.6H
2O] 81.04g, strontium nitrate [Sr (NO
3)
2] 4.38g, nickel nitrate [Ni (NO
3)
2.6H
2O] 12.15g, cobalt nitrate [Co (NO
3)
2.6H
2O] 46.14g is dissolved in the 62.5ml deionized water, is stirred to dissolving.Then, add citric acid [C
6H
8O
7.H
2O] 129.72g, be stirred to dissolving.Then, with palladium nitrate [Pd (NO
3)
2] 6.02g adds in the metal salt solution, stirs half an hour.Other and embodiment 1 operate equally, obtain black powder sample and 40g/ft
3Single palladium catalyst.
Embodiment 4
Perovskite oxide La
0.7Sr
0.3Ni
0.5Co
0.45Pd
0.05O
3Preparation
With lanthanum nitrate [La (NO
3)
3.6H
2O] 65.82g, strontium nitrate [Sr (NO
3)
2] 13.72g, nickel nitrate [Ni (NO
3)
2.6H
2O] 31.72g, cobalt nitrate [Co (NO
3)
2.6H
2O] 28.91g is dissolved in the 62.5ml deionized water, is stirred to dissolving.Then, add citric acid [C
6H
8O
7.H
2O] 135.46g.Then, with palladium nitrate [Pd (NO
3)
2] 6.29g adds in the metal salt solution, stirs half an hour.Other and embodiment 1 operate equally, obtain black powder sample and 40g/ft
3Single palladium catalyst.
More than each chemical reagent, nitrate etc. all have commercially available, also can be through conventional chemical reaction preparation.As passing through metathesis reaction, metal and nitric acid reaction etc.
Testing result
Single palladium catalyst among the above embodiment is carried out active evaluation test.Experimental condition is as follows:
Gas volume is formed: propane: 300ppm, and nitric oxide: 600ppm, carbon monoxide: 2.0%, carbon dioxide: 10%, steam: 10%, oxygen: 1.0～2.0%, nitrogen: balance gas; Air speed: 40000h
-1
Activity rating result such as following table
Can learn from last table:
Know from last table that (1) 4 kinds of catalyst of preparation have good NO and CO conversion temperature.Being suitable for present motorcycle tail gas cleaning needs.
(2) compare with embodiment 2 with embodiment 1; Single palladium catalyst of embodiment 3 and embodiment 4 is low to initiation temperature and the conversion temperature of NO and CO; The interpolation of Ni element in the calcium perovskite oxide is described, is helped promoting the black powder properties of sample, improve the catalytic performance of catalyst.
(3) single palladium catalyst of embodiment 4 is minimum to initiation temperature and the conversion temperature of NO and CO, and the catalytic performance of illustrative embodiment 4 catalyst is the highest, and the black powder properties of sample is best.
Comparative example 1:
With Pd/Al
2O
3, Pt/Al
2O
3, Rh/Al
2O
3Mix, add bonding agent, be prepared into slurries, be coated on the metal beehive carrier, 550 ℃ of roastings 2 hours, make catalyst (Pt: Pd: Rh=18.75: 33.75: 7.5,60g/ft
3).The carrier specification is: the hole order is counted 300cell/in
2, wall thickness 1.0mm, overall dimensions Φ 42mm (diameter) * 100 (shell is long) * 90 (inner core is long).
Above-mentioned catalyst is installed on the WY125-7A motor riding type car that certain company produces, and adopts the UDC test procedure of Chinese Industrial Standards (CIS) state III regulation, carries out bench test.The result is: the CO discharge capacity is 0.839g/km; The HC discharge capacity is 0.139g/km; The NO discharge capacity is 0.08g/km.
Embodiment 5:
With black powder sample among the embodiment 4, with Pt/Al
2O
3Mix, add bonding agent, be prepared into slurries, be coated on the metal beehive carrier, 550 ℃ of roastings 2 hours, make catalyst (Pt: Pd=3.75: 26.25,30g/ft
3).The carrier specification is identical in carrier specification and the comparative example 1.
Catalyst in the above-mentioned catalyst replaced comparative example 1 is installed on the WY125-7A motor riding type car of comparative example 1, adopts the UDC test procedure of Chinese Industrial Standards (CIS) state III regulation, carries out bench test.The result is: the CO discharge capacity is 0.826g/km; The HC discharge capacity is 0.14g/km; The NO discharge capacity is 0.083g/km.
Comparative result
Embodiment 5 is compared and can know with comparative example 1:
(1) the catalyst noble metal dosage is low among the embodiment 5, is less than 50% of noble metal dosage in the comparative example 1; The catalyst cost is far below comparative example 1 in the enforcement 6.
(2) among the embodiment 5 catalyst to CO, NO, catalyst is suitable in the conversion ratio of HC and the comparative example 1, the rig test result that shows as two kinds of catalyst is suitable.
(3) use perovskite oxide among the embodiment 5, do not used perovskite oxide in the comparative example 1.
The introducing of perovskite oxide can reduce noble metal dosage in the catalyst greatly keeping under the constant situation of catalyst performance, promptly effectively reduces the catalyst cost.
Claims (6)
1. perofskite type oxide catalyst is characterized in that:
Said perofskite type oxide catalyst general formula is: A
xA '
1-xB
yB '
1-y-zPd
zO
3
Wherein: A represents thulium; A ' represents alkali earth metal; B and the different transition metal of B ' representative; 0.6≤x≤0.9,0≤y≤0.5,0＜z≤0.1.
2. perofskite type oxide catalyst according to claim 1 is characterized in that: said perofskite type oxide catalyst general formula is: La
xSr
1-xNi
yCo
1-y-zPd
zO
3
Wherein: 0.6≤x≤0.9,0≤y≤0.5,0＜z≤0.1.
3. perofskite type oxide catalyst according to claim 2 is characterized in that: said perofskite type oxide catalyst composition is: La
0.7Sr
0.3Ni
0.5Co
0.45Pd
0.05O
3
4. perofskite type oxide catalyst according to claim 2 is characterized in that: said perofskite type oxide catalyst composition is: La
0.7Sr
0.3Co
0.96Pd
0.04O
3
5. perofskite type oxide catalyst according to claim 2 is characterized in that: said perofskite type oxide catalyst and Pt/Al
2O
3Or Rh/Al
2O
3The catalyst that supported catalyst is mixed with.
6. above-mentioned perofskite type oxide method for preparing catalyst is characterized in that may further comprise the steps:
(1), takes by weighing corresponding rare-earth metal nitrate, alkaline earth nitrate, transition metal nitrate and palladium nitrate respectively by the metering of perofskite type oxide catalyst proportion of composing;
(2), with rare-earth metal nitrate, alkaline earth nitrate and transition metal nitrate that (1) step takes by weighing, be dissolved in the deionized water, the mol ratio of above-mentioned each metal ion summation and deionized water is 6.46-6.79: 1;
(3), be 1: 1.52 required weight citric acid of adding in step (2) gained solution by the mol ratio of metal ion summation in (2) step and citric acid, stirring and dissolving;
(4), palladium nitrate that (1) step is taken by weighing is dissolved in the salting liquid that (3) step obtains, stirred 30 minutes;
(5), step (4) gained solution was worn out 2～7 hours under 70～80 ℃ of water bath condition;
(6), with step (5) gained colloidal sol in 500 ℃ the calcining 1 hour, 900 ℃ the calcining 3 hours, obtain black powder;
(7), step (6) gained black powder or black powder and other mixture that need add component are added bonding agent, be prepared into slurries, be coated on the carrier, drying and roasting makes catalyst.
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|---|---|---|---|
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|---|---|---|---|
| CN2011103654390A CN102500396A (en) | 2011-11-17 | 2011-11-17 | Perovskite type oxide catalyst and preparation method thereof |
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Family
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103349989A (en) * | 2013-07-20 | 2013-10-16 | 四川天健催化燃烧有限公司 | Catalytic agent and combustion board suitable for catalytic combustion and preparation method thereof |
| CN108654592A (en) * | 2018-04-29 | 2018-10-16 | 华中科技大学 | A kind of perovskite catalyst and preparation method thereof and home position testing method |
| CN111085200A (en) * | 2019-12-11 | 2020-05-01 | 山东科技大学 | Catalyst for purifying fuel oil tail gas particles and harmful gas and preparation method thereof |
| CN112337482A (en) * | 2020-11-16 | 2021-02-09 | 湖北航特科技有限责任公司 | Composite material, preparation method thereof and catalyst |
| CN112717943A (en) * | 2020-12-10 | 2021-04-30 | 昆明理工大学 | Nitric oxide oxidation catalyst and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671625A (en) * | 2002-07-09 | 2005-09-21 | 大发工业株式会社 | Process for producing perovskite-type composite oxide |
-
2011
- 2011-11-17 CN CN2011103654390A patent/CN102500396A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1671625A (en) * | 2002-07-09 | 2005-09-21 | 大发工业株式会社 | Process for producing perovskite-type composite oxide |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103349989A (en) * | 2013-07-20 | 2013-10-16 | 四川天健催化燃烧有限公司 | Catalytic agent and combustion board suitable for catalytic combustion and preparation method thereof |
| CN108654592A (en) * | 2018-04-29 | 2018-10-16 | 华中科技大学 | A kind of perovskite catalyst and preparation method thereof and home position testing method |
| CN111085200A (en) * | 2019-12-11 | 2020-05-01 | 山东科技大学 | Catalyst for purifying fuel oil tail gas particles and harmful gas and preparation method thereof |
| CN112337482A (en) * | 2020-11-16 | 2021-02-09 | 湖北航特科技有限责任公司 | Composite material, preparation method thereof and catalyst |
| CN112717943A (en) * | 2020-12-10 | 2021-04-30 | 昆明理工大学 | Nitric oxide oxidation catalyst and preparation method thereof |
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Application publication date: 20120620 |