CN102744074A - Oxygen storage material for catalytic purification of automobile exhaust and preparation method of oxygen storage matrial - Google Patents
Oxygen storage material for catalytic purification of automobile exhaust and preparation method of oxygen storage matrial Download PDFInfo
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- CN102744074A CN102744074A CN2012102379278A CN201210237927A CN102744074A CN 102744074 A CN102744074 A CN 102744074A CN 2012102379278 A CN2012102379278 A CN 2012102379278A CN 201210237927 A CN201210237927 A CN 201210237927A CN 102744074 A CN102744074 A CN 102744074A
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- oxygen storage
- hydrogen
- preparation
- storing material
- tail gas
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Abstract
The invention relates to an oxygen storage material for the catalytic purification of automobile exhaust and a preparation method of the oxygen storage material. The oxygen storage material has a structure formula of CexZr(0.93-x)FeyLa(0.07-y)O2, wherein x is equal to 0.2-0.8 and y is equal to 0-0.01. The preparation method comprises the steps of weighing cerium salt, zircon salt, lanthanum salt and ferric salt according to the stoichiometric proportion in the structure formula and adding the salts in deionized water to prepare mixed solution; adding polyethylene glycol with a molecular weight of 2000-6000 into the mixed solution and adding a precipitator under stirring condition for reaction; after the reaction, carrying out ageing and filtration; and carrying out washing, drying and roasting on filtered matters. The oxygen storage material provided by the invention has good oxygen storage property, after being aged at a high temperature of 1000 DEG C for 5h, the oxygen storage material still has higher oxygen storage property, so that the oxygen storage material has high-temperature ageing resistance which is better than that of cerium-zircon composite oxide oxygen storage materials; and the oxygen storage material is simple in preparation method, easy to operate and suitable for industrial production.
Description
Technical field
The invention belongs to and pollute control and technical field, relate to a kind of hydrogen-storing material that is used for catalytic cleaning of car tail gas and preparation method thereof.
Background technology
Vehicle exhaust has become one of primary pollution source of urban atmospheric pollution, has caused the extensive concern and the great attention of countries in the world.The catalytic cleaning of car tail gas technology be administer now the auto-pollution thing the most effectively, one of reliable technique.The cerium zirconium sosoloid hydrogen-storing material is a kind of catalyst aid of important purifying vehicle exhaust, is used for the coating of cleaning catalyst for tail gases of automobiles, to improve the storage oxygen performance of cleaning catalyst for tail gases of automobiles.In order to improve the storage oxygen performance of cerium zirconium sosoloid, main way is introducing the 3rd even the plain multicomponent composite oxide that forms of quaternary in cerium zirconium sosoloid at present, to improve the storage oxygen performance of solid solution.On the one hand less metal ion replaces bigger metal ion and produces more lattice defect, effectively improves Lattice Oxygen in the migration velocity of body in mutually; The variation of substituted metal ionic valence condition helps the more oxygen vacancies of the middle mutually generation of body on the other hand, thereby improves the storage oxygen performance of solid solution.Big quantity research shows, in cerium zirconium sosoloid, introduces the ion of trivalent or divalence, like Pr
3+, Nd
3+, Y
3+, La
3+, Sm
3+, Ba
2+, Sr
2+Can effectively improve the high-temperature aging resisting performance of hydrogen-storing material Deng rare earth or alkaline earth element.With respect to simple cerium zirconium sosoloid, the compound hydrogen-storing material of multicomponent cerium zirconium all is significantly improved at oxygen storage capacity, the aspects such as texture property that store oxygen speed and material.
Chinese patent publication number CN1314205A discloses a kind of composite oxide material and preparation method with high oxygen storage power, by CeO
2And TiO
2Form.This hydrogen-storing material has higher storage oxygen performance, and the oxygen storage capacity of Ce/Ti comparison composite oxides has considerable influence, and when Ce/Ti=5/5 is that storage oxygen performance is best, its oxygen storage capacity can reach 1070 μ mol/g.But the high temperature ageing condition is not mentioned storage oxygen Effect on Performance.
Chinese patent publication number CN101637721A discloses a kind of porous yttrium-cerium-zirconium solid solution and preparation method thereof, and general formula is Ce
xZe
0.9-xY
0.1This yttrium-cerium-zirconium solid solution fresh sample i.e. oxygen storage capacity of 500 ℃ of roasting 2h is 324～405 μ mol/g, and the oxygen storage capacity behind 900 ℃ of aging 4h is 193～271 μ mol/g.Aging back solid solution oxygen storage capacity descends obviously.
Chinese patent publication number CN101549256A discloses a kind of hydrogen-storing material that can keep storage oxygen performance 900 ℃ of high temperature, and general formula is (Ce
0.6Ze
0.4)
xFe
1-xO
2This hydrogen-storing material storage oxygen is functional, and particularly after 900 ℃ of high-temperature roastings, the oxygen storage capacity of this material does not reduce.But the storage oxygen performance of this hydrogen-storing material behind 1000 ℃ of high temperature ageings do not mentioned.
In the above-mentioned patent documentation, the introduction that has have the composite oxide material and the preparation method of high oxygen storage power, but the high-temperature aging resisting performance is not mentioned; The investigation that has the high-temperature aging resisting performance of hydrogen-storing material, but aging back oxygen storage capacity obviously descends; The introduction that has the high-temperature aging resisting performance of hydrogen-storing material, but the storage oxygen performance of hydrogen-storing material behind 1000 ℃ of high temperature ageings do not mentioned.At present also there is not one piece to disclose a kind of preparation method that the oxygen performance is good, behind 1000 ℃ of high temperature ageings, still keep the hydrogen-storing material of higher storage oxygen performance that stores up.
Summary of the invention
The purpose of this invention is to provide a kind of hydrogen-storing material that is used for catalytic cleaning of car tail gas, can be used in the coating of cleaning catalyst for tail gases of automobiles, to solve the cleaning catalyst for tail gases of automobiles problem that storage oxygen performance descends under high temperature and long-term user mode.
The present invention realizes through following measure:
A kind of hydrogen-storing material that is used for catalytic cleaning of car tail gas of the present invention is characterized in that its general structure is: Ce
xZr
0.93-xFe
yLa
0.07-yO
2, x=0.2～0.8 wherein; Y=0～0.01;
In the said structure formula, be preferably x=0.3～0.7; The storage oxygen performance of the solid solution in y=0.001～0.005, preferable range and heat resistance are best.
The preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas of the present invention:
(1) presses structural formula Ce
xZr
0.93-xFe
yLa
0.07-yO
2In stoichiometric proportion take by weighing cerium salt, zirconates, lanthanum salt and molysite, join then and be made into mixed solution in the deionized water;
(2) adding molecular weight in the mixed solution is 2000～6000 polyethylene glycol, and the adding precipitating reagent reacts under stirring condition again;
(3) after reaction finishes,, will leach thing again, promptly obtain hydrogen-storing material of the present invention through washing, drying and roasting through ageing, filtration.
Said cerium salt, zirconates, lanthanum salt and molysite are selected this area cerous nitrate, zirconyl nitrate or zirconium nitrate, lanthanum nitrate, ferric nitrate commonly used for use, and the cerium salinity is 0.1～1mol/L in the mixed solution.Concentration is crossed low nonsensical, and excessive concentration can make the deposition caking, and is influential to the structure of product.
Said molecular weight be 2000～6000 polyethylene glycol in the present invention as protective agent, be used for controlling the speed of sediment crystal growth in the solution.The dosage of polyethylene glycol accounts for the 1-5% of mixed solution gross mass.In this scope, the control effect that plays is best.
Described precipitating reagent is ammoniacal liquor-ammonium carbonate buffer solution, and wherein, the mass fraction of ammonia is 5～10%, and the mass fraction of ammonium carbonate is 10～15%, and it is best that concentration is controlled at the product effect that the precipitating reagent deposition in this scope obtains.The addition of precipitating reagent is so that the pH value of mixed liquor reaches 8.0～8.5 is advisable, to guarantee that deposition fully.
In the step (2), the described reaction time is 1～2h, in this scope, can guarantee fully reaction.
In the step (3), described digestion time is 1～2h, and described ageing is the operation commonly used in the chemical field, is meant to deposit a period of time solution is static, and digestion time is controlled in this scope, the deposition structural arrangement comparison rule that obtains.
In the step (3), described baking temperature is 100～150 ℃, and the time is 2～5h, makes sediment fully dry.
In the step (3), 500～600 ℃ of described sintering temperatures, the time is 3～5h, makes sediment be completed into solid solution.
The hydrogen-storing material (1000 ℃ of Muffle furnaces are handled 5h) behind high temperature ageing that is used for catalytic cleaning of car tail gas of the present invention still keeps higher storage oxygen performance, and preparation technology has that method is simple, easy operating, be suitable for advantage such as suitability for industrialized production.
The specific embodiment
For clearer explanation the present invention, enumerate following examples, but it has no restriction to scope of the present invention.
Comparative Examples
Get the 217.1g cerous nitrate; 99.4g zirconyl nitrate; Add deionized water preparation mixed salt solution 1L, add 30g Macrogol 2000 stirring and dissolving then, again under stirring condition with the mass fraction of ammonia be 5%, the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 10% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.0; React 1h and ageing 2h at normal temperatures; Filter, wash, at 100 ℃ of following dry 3h, desciccate obtains solid solution hydrogen-storing material Ce at 500 ℃ of roasting 4h at last
0.5Zr
0.43O
2
Embodiment 1
Get the 217.1g cerous nitrate, 99.4g zirconyl nitrate, 30.3g lanthanum nitrate; Add deionized water preparation mixed salt solution 1L; Adding 30g Macrogol 2000 stirring and dissolving then, is 5% with the mass fraction of ammonia under stirring condition again, and the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 10% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.0; React 1h and ageing 2h at normal temperatures; Filter, wash, at 100 ℃ of following dry 3h, desciccate obtains solid solution hydrogen-storing material Ce at 500 ℃ of roasting 4h at last
0.5Zr
0.43La
0.07O
2
Product labelling is A.
Embodiment 2
Get the 130.3g cerous nitrate, 145.7g zirconyl nitrate, 29.9g lanthanum nitrate and 0.40g ferric nitrate; Add deionized water preparation mixed salt solution 1L; Adding 30g Macrogol 2000 stirring and dissolving then, is 5% with the mass fraction of ammonia under stirring condition again, and the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 10% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.0; React 1h and ageing 2h at normal temperatures; Filter, wash, at 100 ℃ of following dry 3h, desciccate obtains solid solution hydrogen-storing material Ce of the present invention at 500 ℃ of roasting 4h at last
0.3Zr
0.63Fe
0.001La
0.069O
2
Product labelling is B.
Embodiment 3
Get the 173.7g cerous nitrate, 179.8g zirconium nitrate, 29.0g lanthanum nitrate and 1.2g ferric nitrate; Add deionized water preparation mixed salt solution 1L; Adding 30g Macrogol 4000 stirring and dissolving then, is 10% with the mass fraction of ammonia under stirring condition again, and the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 10% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.5; React 2h and ageing 1h at normal temperatures; Filter, wash, at 120 ℃ of following dry 2h, desciccate obtains solid solution hydrogen-storing material Ce of the present invention at 600 ℃ of roasting 3h at last
0.4Zr
0.53Fe
0.003La
0.067O
2
Product labelling is C.
Embodiment 4
Get the 217.1g cerous nitrate, 99.4g zirconyl nitrate, 28.1g lanthanum nitrate and 2.0g ferric nitrate; Add deionized water preparation mixed salt solution 1L; Adding 30g Macrogol 2000 stirring and dissolving then, is 5% with the mass fraction of ammonia under stirring condition again, and the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 15% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.0; React 1h and ageing 2h at normal temperatures; Filter, wash, at 150 ℃ of following dry 4h, desciccate obtains solid solution hydrogen-storing material Ce of the present invention at 500 ℃ of roasting 5h at last
0.5Zr
0.43Fe
0.005La
0.065O
2
Product labelling is D.
Embodiment 5
Get the 260.6g cerous nitrate, 111.9g zirconium nitrate, 27.3g lanthanum nitrate and 2.8g ferric nitrate; Add deionized water preparation mixed salt solution 1L; Adding 30g Macrogol 6000 stirring and dissolving then, is 10% with the mass fraction of ammonia under stirring condition again, and the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 15% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.5; React 2h and ageing 1h at normal temperatures; Filter, wash, at 110 ℃ of following dry 5h, desciccate obtains solid solution hydrogen-storing material Ce of the present invention at 600 ℃ of roasting 4h at last
0.6Zr
0.33Fe
0.007La
0.063O
2
Product labelling is E.
Embodiment 6
Get the 304.0g cerous nitrate, 53.18g zirconyl nitrate, 26.0g lanthanum nitrate and 4.0g ferric nitrate; Add deionized water preparation mixed salt solution 1L; Adding 30g Macrogol 4000 stirring and dissolving then, is 10% with the mass fraction of ammonia under stirring condition again, and the mass fraction of ammonium carbonate is that ammoniacal liquor-ammonium carbonate buffer solution of 15% adds mixed salt solution and makes the pH value of mixed liquor remain on 8.5; React 1h and ageing 2h at normal temperatures; Filter, wash, at 130 ℃ of following dry 3h, desciccate obtains solid solution hydrogen-storing material Ce of the present invention at 500 ℃ of roasting 3h at last
0.7Zr
0.23Fe
0.01La
0.06O
2
Product labelling is F.
The performance test of storage oxygen:
The said storage oxygen of the present invention performance is the buffer capacity of solid solution to oxygen, with its in oxidation environment, store oxygen and in reducing environment the ability of release oxygen estimate.Solid solution is at first containing 10%H
2Hydrogen nitrogen mixed gas in temperature programmed reduction, be cooled to 400 ℃ then and carry out the pulse of oxygen titration, use the thermal conductivity detector (TCD) analytical gas.Calculate storage oxygen performance by the amount of the oxygen that consumes.The characteristic value of storage oxygen performance is represented with the μ mol number of the oxygen that every gram solid solution is consumed.In order to measure the storage oxygen performance behind the hydrogen-storing material high temperature ageing, the sample that makes is handled 5h in 1000 ℃ of Muffle furnaces, to obtain the hydrogen-storing material after aging.
The situation of change of oxygen storage capacity before and after table 1. hydrogen-storing material is aging
Test result by table 1 can find out that the storage oxygen performance of hydrogen-storing material of the present invention all is superior to Comparative Examples.Along with the increase of iron content, storage oxygen performance fall reduces behind 1000 ℃ of high temperature ageings of solid solution hydrogen-storing material.This explains that we have fine storage oxygen performance and high-temperature aging resisting performance by the powder of preparation, are suitable for as the three-effect catalysis agent aid.
The above is merely preferred embodiments of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a hydrogen-storing material that is used for catalytic cleaning of car tail gas is characterized in that, its general structure is:
Ce
xZr
0.93-xFe
yLa
0.07-yO
2, x=0.2～0.8 wherein, y=0～0.01.
2. the hydrogen-storing material that is used for catalytic cleaning of car tail gas as claimed in claim 1 is characterized in that, x=0.3～0.7, y=0.001～0.005.
3. claim 1 or the 2 described preparation methods that are used for the hydrogen-storing material of catalytic cleaning of car tail gas is characterized in that step is following:
(1) takes by weighing cerium salt, zirconates, lanthanum salt and molysite by the stoichiometric proportion in claim 1 structural formula, join then and be made into mixed solution in the deionized water;
(2) adding molecular weight in the mixed solution is 2000～6000 polyethylene glycol, and the adding precipitating reagent reacts under stirring condition again;
(3) after reaction finishes,, will leach thing again, promptly get through washing, drying and roasting through ageing, filtration.
4. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3 is characterized in that, in the step (1), the cerium salinity is 0.1～1mol/L in the mixed solution.
5. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3 is characterized in that, in the step (2), said molecular weight is that the dosage of 2000～6000 polyethylene glycol is the 1-5% of mixed solution gross mass.
6. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3; It is characterized in that in the step (2), described precipitating reagent is ammoniacal liquor-ammonium carbonate buffer solution; The mass fraction of ammonia is 5～10% in the buffer solution, and the mass fraction of ammonium carbonate is 10～15%; The addition of precipitating reagent is so that the pH value of mixed solution reaches 8.0～8.5 is as the criterion.
7. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3 is characterized in that, in the step (2), the reaction time is 1～2h.
8. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3 is characterized in that, in the step (3), digestion time is 1～2h.
9. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3 is characterized in that, in the step (3), baking temperature is 100～150 ℃, and the time is 2～5h.
10. the preparation method who is used for the hydrogen-storing material of catalytic cleaning of car tail gas as claimed in claim 3 is characterized in that, in the step (3), and 500～600 ℃ of sintering temperatures, the time is 3～5h.
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| CN107235706A (en) * | 2017-06-26 | 2017-10-10 | 俞秀英 | A kind of functional ceramic powder material and preparation method thereof |
| CN107244885A (en) * | 2017-06-27 | 2017-10-13 | 过春明 | A kind of photocatalysis ceramics powder body material and preparation method thereof |
| CN111417452A (en) * | 2018-01-08 | 2020-07-14 | 太平洋工业发展公司 | Catalyst comprising a ceria-zirconia-oxygen storage material and method for producing the catalyst |
| WO2021198644A1 (en) * | 2020-03-30 | 2021-10-07 | Johnson Matthey Public Limited Company | Oxygen storage capacity material |
| CN115974549A (en) * | 2022-12-02 | 2023-04-18 | 常州大学 | Preparation method of cerium-zirconium solid solution and method for regulating cerium valence ratio and oxygen vacancy concentration of cerium-zirconium solid solution |
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Application publication date: 20121024 |