CN101940921A - Bilayer structured oxygen storage material and preparation method thereof - Google Patents
Bilayer structured oxygen storage material and preparation method thereof Download PDFInfo
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- CN101940921A CN101940921A CN2010101849845A CN201010184984A CN101940921A CN 101940921 A CN101940921 A CN 101940921A CN 2010101849845 A CN2010101849845 A CN 2010101849845A CN 201010184984 A CN201010184984 A CN 201010184984A CN 101940921 A CN101940921 A CN 101940921A
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Abstract
The invention discloses a bilayer structured oxygen storage material and a preparation method thereof. The material is prepared by compounding ceria-zirconia solid solution and gamma-Al2O3 with a great specific surface, wherein the general formula is RexCeyZr1-x-yO2-Al2O3. The preparation method comprises the following steps of: (1) putting lanthanum nitrate solution, cerous nitrate solution, yttrium nitrate solution and zirconium nitrate solution into a container, adding ammonia water into the mixture for precipitation so as to obtain precipitates; (2) adding industrial hydrogen peroxide in the mass of cerium oxide into the precipitates in the step (1) to obtain a ceria-zirconia precursor compound RexCeyZr1-x-y(OH)2; (3) mixing the RexCeyZr1-x-yO2 and the gamma-Al2O3 in a mass ratio of 1:1 and uniformly stirring to obtain a mixture; and (4) firing the mixture in the step (3), decomposing the ceria-zirconia precursor compound RexCeyZr1-x-y (OH)2 into RexCeyZr1-x-yO2, and performing fluid energy milling to obtain the powder oxygen storage material with a bilayer structure. The surfactant adopted by the invention can form interfacial films among ions to avoid the phenomenon of great agglomeration among the ions and to make macropores in the ceria-zirconia solid solution relatively increased, so that the ageing resistance of the oxygen storage material is improved.
Description
Technical field
The present invention relates to car tail gas purificant, is a kind of double-decker hydrogen-storing material and preparation method thereof.
Background technology
Because vehicle exhaust severe contamination atmosphere is so how those skilled in the art have proposed more technical scheme aspect the purifying automobile tail gas.At present, using more cleaning catalyst for tail gases of automobiles mainly is to be hydrogen-storing material with cerium zirconium sosoloid, and still, there is following defective in it, because CeO in the cerium zirconium sosoloid
2Easy-sintering when high temperature, particle is grown up, and specific area reduces, and then reduces Ce
4+/ Ce
3+Redox property reduces catalyst purifying automobile tail gas function.For this reason, γ-Al is adopted in this area
2O
3Solve this defective, found that yet use, though γ-Al
2O
3Have bigger specific area, can make cerium zirconium sosoloid and catalyst activity sexual element high degree of dispersion, improve purification efficiency on its surface, still, because γ-Al
2O
3With mixing of cerium zirconium sosoloid physics, be immersed in the honeycomb support surface jointly through hydrogen-storing material and platinum, zirconium, palladium isoreactivity composition again through ball milling, the hydrogen-storing material that reaches the component preparation in this way is more than 1000 ℃, still can make coating material generation sintering, cause the porous oxide duct to cave in, specific area is reduced, weaken thereby cause storing the oxygen ability, and make and be dispersed in its surperficial noble metal and be received in the duct that caves in, and then reduce catalytic capability.
Summary of the invention
The objective of the invention is, a kind of double-decker hydrogen-storing material and preparation method thereof is provided,, further improve the detergent power of catalyst to solve the deficiency that prior art exists.
The present invention is achieved through the following technical solutions for achieving the above object: a kind of double-decker hydrogen-storing material, it is by cerium zirconium sosoloid and Large ratio surface γ-Al
2O
3Be composited, its general formula is:
Re
xCe
yZr
1-x-yO
2-Al
2O
3, wherein x is 0-0.2, y is 0.2-0.8.
The preparation method of a kind of double-decker hydrogen-storing material of the present invention may further comprise the steps:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution, in its oxide mass than 5-10: 20-60: 5-7: the 30-70 ratio is mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 2-10mol/L, be precipitated to till solution PH＞8.5-10, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2
3. with Re
xCe
yZr
1-x-y (OH)
2Press RexCeyZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes at 1: 1, and stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 55 ℃ of-85 ℃ of deionized waters, filters, add surfactant again, the addition of surfactant is the nitrate of rare earth and the 10-50% of zirconia gross mass, after the making beating, 80-200 ℃ of oven dry down, then 500-800 ℃ of following calcination, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material.
The surfactant of step described in 4. is polyoxyethylene pentaerythritol, any of polyester ethylene oxide or butyl ether.
The oxide mass ratio of the 1. described lanthanum nitrate hexahydrate of step, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution is 5: 20: 5: 70.
The invention has the advantages that: hydrogen-storing material is made double-decker, make the cerium zirconium sosoloid height be dispersed in bigger serface γ-Al uniformly
2O
3The surface, the catalytic active site of the active ingredient that is dispersed in the surface is increased, increased substantially the stability of cerium zirconium sosoloid under the hot conditions, hydrogen-storing material of the present invention is under 1000 ℃-1100 ℃, the amplitude that specific area reduces significantly reduces, and has increased substantially purification function.
Because the surfactant that the present invention adopts, can between ion, form interfacial film, stop big agglomeration takes place between the ion, and emit more heat can in the calcination process, decompose the time, make it to have the effect of reaming, macropore in the cerium zirconium sosoloid is increased relatively, thereby improved the ageing resistace of hydrogen-storing material.
Because the preparation method of hydrogen-storing material of the present invention is by with rare earth modified γ-Al
2O
3Mix with the sedimentary solution of cerium zirconium, can make cerium zirconium sosoloid relatively be dispersed in γ-Al
2O
3The surface has obtained high-temperature stability preferably, and show 1000-1100 ℃ of aging 6 hours test result: the BET specific area can reach 49.2-58.47m
2/ g.
The specific embodiment
Embodiment
The present invention at first provides a kind of double-decker hydrogen-storing material for solving the deficiency of prior art, and it is by cerium zirconium sosoloid and Large ratio surface γ-Al
2O
3Be composited, its general formula is:
Re
xCe
yZr
1-x-yO
2-Al
2O
3, wherein x is 0-0.2, y is 0.2-0.8.
Re
xCe
yZr
1-x-yO
2With γ-Al
2O
3Mass ratio be 1: 1.
The preparation method of hydrogen-storing material of the present invention may further comprise the steps:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution, in its oxide mass than 55-10: 20-60: 5-7: the 30-70 ratio is mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 2-10mol/L, be precipitated to till solution PH＞8.5-10, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R exCeyZr
1-x-y (OH)
2
3. with RexCeyZr
1-x-y (OH)
2Press Re
xCe
yZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes at 1: 1, and stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 55 ℃ of-85 ℃ of deionized waters, filters, add surfactant again, the addition of surfactant is the nitrate of rare earth and the 10-50% of zirconia gross mass, after the making beating, 80-200 ℃ of oven dry down, then 500-800 ℃ of following calcination, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material.Double-deck hydrogen-storing material chemical general formula is Re
xCe
yZr
1-x-yO
2-Al
2O
3, the D50 of double-deck powder hydrogen-storing material is 1.5-4.0um.
The surfactant of step described in 4. is polyoxyethylene pentaerythritol, any of polyester ethylene oxide or butyl ether.
The oxide mass ratio of the 1. described lanthanum nitrate hexahydrate of step, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution can be 5: 20: 5: 70, and this is a kind of preferred relatively scheme.
The concentration of lanthanum nitrate hexahydrate, cerous nitrate solution and the zirconium nitrate solution of the step of said method in 1. is generally 100-350g/L.γ-the Al of step in 3.
2O
3Be rare earth modified γ-Al
2O
3
The yttrium nitrate of step in 1. can adopt praseodymium nitrate or neodymium nitrate to substitute.
The 2. middle industrial hydrogen peroxide that adds of step is 50% of a cerium oxide quality, and promptly cerium oxide is 100, and industrial hydrogen peroxide is 50.
Hydrogen-storing material of the present invention can be produced in order to the below method:
1, a kind of preparation method of double-decker hydrogen-storing material, its concrete steps are:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution, in its oxide mass than 5: 30: 5: 60 ratios are mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 4mol/L, be precipitated to till solution PH=8.5, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2
3. with Re
xCe
yZr
1-x-y (OH)
2Press Re
xCe
yZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes γ-Al at 1: 1
2O
3Be rare earth modified γ-Al
2O
3, stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 55 ℃ of deionized waters, filters, add polyoxyethylene pentaerythritol again, the addition of polyoxyethylene pentaerythritol is 10% of the nitrate of rare earth and a zirconia gross mass, after the making beating, 80 ℃ of oven dry down, then 500 ℃ of following calcinations, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material, its chemical general formula is: Re
xCe
yZr
1-x-yO
2-Al
2O
3, the double-deck hydrogen-storing material D50 of powder is 1.5-4.0um, and the powder hydrogen-storing material of this layer structure wore out 6 hours down at 1000 ℃, and the BET specific area is 52.13m
2/ g.
2, a kind of preparation method of double-decker hydrogen-storing material, its concrete steps are:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution, in its oxide mass than 10: 53: 7: 30 ratios are mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 2mol/L, be precipitated to till solution PH=9, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2
3. with Re
xCe
yZr
1-x-y (OH)
2Press Re
xCe
yZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes γ-Al at 1: 1
2O
3Be rare earth modified γ-Al
2O
3, stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 85 ℃ of deionized waters, filters, add the polyester ethylene oxide again, the addition of polyester ethylene oxide is 40% of the nitrate of rare earth and a zirconia gross mass, after the making beating, 100 ℃ of oven dry down, then 800 ℃ of following calcinations, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material, its chemical general formula is: Re
xCe
yZr
1-x-yO
2-Al
2O
3, double-deck powder hydrogen-storing material D50 is 1.5-4.0um, and this powder body material wore out 6 hours down at 1100 ℃, and the BET specific area is 55.36m
2/ g.
3, a kind of preparation method of double-decker hydrogen-storing material, its concrete steps are:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, praseodymium nitrate and zirconium nitrate solution, in its oxide mass than 5: 60: 5: 30 ratios are mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 10mol/L, be precipitated to till solution PH=10, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2
3. with Re
xCe
yZr
1-x-y (OH)
2Press Re
xCe
yZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes γ-Al at 1: 1
2O
3Be rare earth modified γ-Al
2O
3, stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 70 ℃ of deionized waters, filters, add butyl ether again, the addition of butyl ether is 50% of the nitrate of rare earth and a zirconia gross mass, after the making beating, 200 ℃ of oven dry down, then 700 ℃ of following calcinations, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material, its chemical general formula is: Re
xCe
yZr
1-x-yO
2-Al
2O
3, double-deck powder hydrogen-storing material D50 is 1.5-4.0um, and this powder body material wore out 6 hours down at 1100 ℃, and the BET specific area is 49.2m
2/ g.
4, a kind of preparation method of double-decker hydrogen-storing material, its concrete steps are:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution, in its oxide mass than 5: 20: 5: 70 ratios are mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 7mol/L, be precipitated to till solution PH=8.5, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2
3. with Re
xCe
yZr
1-x-y (OH)
2Press Re
xCe
yZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes γ-Al at 1: 1
2O
3Be rare earth modified γ-Al
2O
3, stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 60 ℃ of deionized waters, filters, adding two kinds of surfactants of polyester ethylene oxide and butyl ether again mixed by 1: 1, the addition of polyester ethylene oxide and butyl ether is 30% of the nitrate of rare earth and a zirconia gross mass, after the making beating, 180 ℃ of oven dry down, then 600 ℃ of following calcinations, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material, its chemical general formula is: Re
xCe
yZr
1-x-yO
2-Al
2O
3, double-deck powder hydrogen-storing material D50 is 1.5-4.0um, and this powder body material wore out 6 hours down at 1000 ℃, and the BET specific area is 58.47m
2/ g.
Re with the inventive method acquisition
xCe
yZr
1-x-yO
2-Al
2O
3, wherein x is 0-0.2, y is 0.2-0.8.
Claims (4)
1. double-decker hydrogen-storing material, it is characterized in that: it is by cerium zirconium sosoloid and Large ratio surface γ-Al
2O
3Be composited, its general formula is:
Re
xCe
yZr
1-x-yO
2-Al
2O
3, wherein x is 0-0.2, y is 0.2-0.8.
2. the preparation method of the described a kind of double-decker hydrogen-storing material of claim 1 is characterized in that: may further comprise the steps:
1. get lanthanum nitrate hexahydrate, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution, in its oxide mass than 5-10: 20-60: 5-7: the 30-70 ratio is mixed, insert stir in the container after, adding concentration is the ammoniacal liquor of 2-10mol/L, be precipitated to till solution PH＞8.5-10, obtain sediment;
2. 50% of adding cerium oxide quality industrial hydrogen peroxide in step sediment 1. makes Ce
3+Be oxidized to Ce
4+, obtain cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2
3. with Re
xCe
yZr
1-x-y (OH)
2Press RexCeyZr
1-x-yO
2With γ-Al
2O
3Mass ratio mixes at 1: 1, and stirring after the mixing obtains mixture;
4. after the mixture of step in 3. washs in 55 ℃ of-85 ℃ of deionized waters, filters, add surfactant again, the addition of surfactant is the nitrate of rare earth and the 10-50% of zirconia gross mass, after the making beating, 80-200 ℃ of oven dry down, then 500-800 ℃ of following calcination, cerium zirconium precursor compound R e
xCe
yZr
1-x-y (OH)
2Be decomposed into Re
xCe
yZr
1-x-yO
2, carry out air-flow at last and pulverize, obtain double-deck powder hydrogen-storing material.
3. the preparation method of a kind of double-decker hydrogen-storing material according to claim 2 is characterized in that: the surfactant of step described in 4. is polyoxyethylene pentaerythritol, any of polyester ethylene oxide or butyl ether.
4. the preparation method of a kind of double-decker hydrogen-storing material according to claim 2 is characterized in that: the oxide mass ratio of the 1. described lanthanum nitrate hexahydrate of step, cerous nitrate solution, yttrium nitrate and zirconium nitrate solution is 5: 20: 5: 70.
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| CN102247826A (en) * | 2011-05-27 | 2011-11-23 | 济南大学 | Cubic phase cerium and zirconium based composite oxide with high specific surface area and preparation method thereof |
| CN102580719A (en) * | 2012-03-13 | 2012-07-18 | 上海华明高纳稀土新材料有限公司 | Nanometer ceria-zirconium solid solution and preparation method thereof |
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2010
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| CN102247826A (en) * | 2011-05-27 | 2011-11-23 | 济南大学 | Cubic phase cerium and zirconium based composite oxide with high specific surface area and preparation method thereof |
| CN102580719A (en) * | 2012-03-13 | 2012-07-18 | 上海华明高纳稀土新材料有限公司 | Nanometer ceria-zirconium solid solution and preparation method thereof |
| CN102580719B (en) * | 2012-03-13 | 2014-01-29 | 上海华明高纳稀土新材料有限公司 | Nanometer ceria-zirconium solid solution and preparation method thereof |
| CN102962047A (en) * | 2012-11-12 | 2013-03-13 | 上海华明高纳稀土新材料有限公司 | Aluminum-cerium-zirconium based composite oxide catalytic material and preparation method thereof |
| JP2014122149A (en) * | 2012-11-22 | 2014-07-03 | Toyota Motor Corp | Composite oxide particle and catalyst for exhaust gas purification using the same |
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| CN103816886A (en) * | 2014-01-27 | 2014-05-28 | 江苏振邦尾气净化有限公司 | Method for preparing rare earth oxygen-storage material with large specific surface |
| CN103816886B (en) * | 2014-01-27 | 2017-01-04 | 江苏几维环境科技有限公司 | A kind of preparation method of Large ratio surface rare earth oxygen storage material |
| CN107107037A (en) * | 2015-01-19 | 2017-08-29 | 优美科股份公司及两合公司 | The double-deck three-way catalyst of ageing stability with raising |
| CN107107037B (en) * | 2015-01-19 | 2020-08-04 | 优美科股份公司及两合公司 | Dual-layer three-way catalyst with improved aging stability |
| CN105642269A (en) * | 2016-02-26 | 2016-06-08 | 赣州博晶科技有限公司 | Composite ceria-zirconia solid solution and preparation method thereof |
| CN105642269B (en) * | 2016-02-26 | 2018-07-27 | 江西国瓷博晶新材料科技有限公司 | A kind of compound cerium zirconium sosoloid and preparation method thereof |
| CN107213887A (en) * | 2017-07-10 | 2017-09-29 | 中自环保科技股份有限公司 | Functional material and preparation method thereof |
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Application publication date: 20110112 |