CN102258995A - Ternary-cerium-based oxygen storage material and preparation method thereof - Google Patents
Ternary-cerium-based oxygen storage material and preparation method thereof Download PDFInfo
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- CN102258995A CN102258995A CN2011101213228A CN201110121322A CN102258995A CN 102258995 A CN102258995 A CN 102258995A CN 2011101213228 A CN2011101213228 A CN 2011101213228A CN 201110121322 A CN201110121322 A CN 201110121322A CN 102258995 A CN102258995 A CN 102258995A
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Abstract
The invention discloses a ternary-cerium-based oxygen storage material and a preparation method thereof. The oxygen storage material consists of an oxygen storage material main body, aids, and a dispersing agent; the oxygen storage material main body is a rare earth material which consists of cerous nitrate, zirconium nitrate and lanthanum nitrate; the aids are barium nitrate, copper nitrate, manganous nitrate or magnesium nitrate; the dispersing agent is polyvinyl alcohol, polyethylene glycol or citric acid; and the material has the advantage of obviously reducing the ignition temperature of tail gas catalytic conversion of a three-way catalytic converter, prolonging the service life of the three-way catalytic converter, and greatly reducing the fluctuation of air-fuel ratio windows during working of the three-way catalytic converter. Compared with the three-way catalytic converter in which the oxygen storage material is not adopted, the three-way catalytic converter in which the oxygen storage material is adopted has the advantage that the using amount of noble metal can be reduced by over 17 percent.
Description
Technical field
The present invention relates to a kind of ternary cerium-based oxygen storage material and preparation method thereof.
Background technology
The control technology of current mobility car pollutant emission can be divided three classes, and is respectively control technology before the burning, control technology and tail gas clean-up technology in the burning.Wherein the tail gas clean-up technology mainly adopts the triple-effect catalytic unit technology, and triple-effect catalytic unit (Three Way Catalyst) mainly contains four parts and forms: carrier, aluminum oxide coating layer, active component and auxiliary agent.By catalytic oxidation between CO, HC and the NOx and reduction reaction, three-way catalyst can make CO, the HC of gasoline engine and NOx discharging reduce more than 90% simultaneously simultaneously.The catalytic activity of three-way catalyst is relevant with air-fuel ratio, has an operation window in theoretical air-fuel ratio about 14.6, and the catalytic activity of CO, HC and NOx can reach 90% in the air-fuel ratio window ranges.But because motor vehicle quickens, slow down and road conditions complicated and changeable in the actual condition, air-fuel ratio always fluctuates about 14-15, can't satisfy the requirement of catalyzed conversion CO, HC and NOx simultaneously, makes catalytic conversion efficiency decline.
Hydrogen-storing material has effectively played the effect of regulating air-fuel ratio as one of core technology of triple-effect catalytic unit, makes the air-fuel ratio window about 14.6.Yet present hydrogen-storing material, its oxygen storage capacity store up the oxygen performance especially dynamically and are still waiting to improve, and the high temperature sintering resistant ability is also not enough, thereby have influenced the service life of triple-effect catalytic unit.
Summary of the invention
Total be exactly technical problem to be solved by this invention will be at existing hydrogen-storing material oxygen storage capacity and dynamically stored up oxygen performance deficiency, the high temperature sintering resistant ability is not enough, and a kind of high-performance cerium base ternary hydrogen-storing material and preparation method thereof is provided.
The present invention is made up of hydrogen-storing material main body, auxiliary agent, dispersant, and its weight portion proportioning is:
Hydrogen-storing material main body 80-95 auxiliary agent 3-10 dispersant 2-10;
Described hydrogen-storing material main body is a rare earth material, and rare earth material is made up of cerous nitrate, zirconium nitrate and lanthanum nitrate, and its weight portion proportioning is:
Cerous nitrate 0.5-0.8 zirconium nitrate 0.3-0.45 0.05-0.15 lanthanum nitrate;
Described auxiliary agent is barium nitrate, copper nitrate, manganese nitrate or magnesium nitrate, or wherein any two kinds and arbitrarily two or morely mix with arbitrary proportion, or all mix with arbitrary proportion;
Described dispersant is polyvinyl alcohol, polyethylene glycol or citric acid; Or wherein any two kinds mix with arbitrary proportion, or all mix with arbitrary proportion;
It also has oxidant, and oxidant is a hydrogen peroxide, and its weight portion proportioning is:
Preparation technology mainly may further comprise the steps:
1) takes by weighing Ce (NO in proportion
3)
36H
2O, Zr (NO
3)
45H
2O, La (NO
3)
36H
2O is mixed with solution, adds hydrogen peroxide again, adds auxiliary agent, makes mixed liquor;
2) ammonia spirit of preparation 3mol/L and the sal volatile of 3mol/L are mixing in 1: 1 by volume, make precipitated liquid,
3) under 45 ℃ of waters bath with thermostatic control, 200Kw ultrasound condition, mixed liquor and precipitating reagent are pressed 15: 10 weight portion proportioning and flowed stirring, pH value of solution is controlled at 8 in the co-current process, and stream continue to stir 1h after finishing, the polyethylene glycol that adds solid solution quality 8% then, regulate pH to 8-10, take out behind the 80-100 ℃ of ageing 2-4h, leave standstill 8-12h under the room temperature;
4) sediment process suction filtration, after the deionized water washing, pH=7,120 ℃ of dry 10-12h;
5) be warming up to 500 ℃ of insulation 4h behind 300 ℃ of roasting 0.5h of dried sample, can wait until hydrogen-storing material.
Compared with prior art, beneficial effect of the present invention is mainly reflected in the following aspects:
1) compare with the triple-effect catalytic unit that does not adopt this hydrogen-storing material to prepare, hydrogen-storing material of the present invention has significantly reduced the initiation temperature of triple-effect catalytic unit in tail gas catalyzed conversion.
2) hydrogen-storing material of the present invention possesses high specific surface area, and through behind 500 ℃, 4h roasting, the specific area of hydrogen-storing material reaches 147.09m
2/ g, through 700 ℃, after the 4h roasting, specific area is 102.52m
2/ g; Through 1000 ℃, 10% steam, after 5h was aging, specific area still can reach 46.79m
2/ g has prolonged service life of triple-effect catalytic unit.
3) hydrogen-storing material of the present invention possesses high oxygen storage capacity, and after 500 ℃ of fresh attitudes, the 4h roasting, the oxygen storage capacity of hydrogen-storing material reaches 292.2 μ molg
-1Through 1000 ℃, 10% steam, after 5h was aging, the oxygen storage capacity of hydrogen-storing material still can reach 201.8 μ molg
-1, the oxygen storage capacity of stability and high efficiency, the fluctuation of air-fuel ratio window when significantly having weakened triple-effect catalytic unit work.
4) hydrogen-storing material preparation technology of the present invention possesses the ability of large-scale production and application.
5) adopt the hydrogen-storing material of explained hereafter of the present invention, possess the economic advantages of low cost-high benefit, do not adopt the triple-effect catalytic unit of this hydrogen-storing material on year-on-year basis, noble metal dosage can reduce more than 17%.
Description of drawings
Fig. 1 is surface sweeping Electronic Speculum (SEM) picture that contains the catalyst converter coating of this hydrogen-storing material.
Fig. 2 is ESEM (SEM) picture of the catalyst converter coating of certain company's production.
Fig. 3 is the sample initiation temperature curve that is coated with noble metal of hydrogen-storing material preparation of the present invention.
Fig. 4 is the sample initiation temperature curve that is coated with noble metal of the sample storage material preparation of certain company's production.
Specific implementation method
Below with the specific embodiment technical scheme of the present invention is described
Hydrogen-storing material is made up of hydrogen-storing material main body, auxiliary agent, dispersant, and its weight portion proportioning is:
Hydrogen-storing material main body 80-95 auxiliary agent 3-10 dispersant 2-10;
Described hydrogen-storing material main body is a rare earth material, and rare earth material is made up of cerous nitrate, zirconium nitrate and lanthanum nitrate, and its weight portion proportioning is:
Cerous nitrate 0.5-0.8 zirconium nitrate 0.3-0.45 0.05-0.15 lanthanum nitrate;
Described auxiliary agent is barium nitrate, copper nitrate, manganese nitrate or magnesium nitrate, or wherein any two kinds and arbitrarily two or morely mix with arbitrary proportion, or all mix with arbitrary proportion;
Described dispersant is polyvinyl alcohol, polyethylene glycol or citric acid; Or wherein any two kinds mix with arbitrary proportion, or all mix with arbitrary proportion;
It also has oxidant, and oxidant is a hydrogen peroxide, and its weight portion proportioning is:
Preparation technology mainly may further comprise the steps:
1) takes by weighing Ce (NO in proportion
3)
36H
2O, Zr (NO
3)
45H
2O, La (NO
3)
36H
2O is mixed with solution, adds hydrogen peroxide again, adds auxiliary agent, makes mixed liquor;
2) ammonia spirit of preparation 3mol/L and the sal volatile of 3mol/L are mixing in 1: 1 by volume, make precipitated liquid,
3) under 45 ℃ of waters bath with thermostatic control, 200Kw ultrasound condition, mixed liquor and precipitating reagent to be pressed 15: 10 weight portion proportioning and flowed stirring, pH value of solution is controlled at 8 in the co-current process,
And stream continue to stir 1h after finishing, and adds the polyethylene glycol of solid solution quality 8% then, regulates pH to 8-10, takes out behind the 80-100 ℃ of ageing 2-4h, leaves standstill 8-12h under the room temperature;
4) sediment process suction filtration, after the deionized water washing, pH=7,120 ℃ of dry 10-12h;
5) be warming up to 500 ℃ of insulation 4h behind 300 ℃ of roasting 0.5h of dried sample, can wait until hydrogen-storing material.
The production technology of the concrete ternary cerium-based oxygen storage material of recommending is carried out according to following steps:
1) takes by weighing rare earth compound Ce (NO in proportion
3)
36H
2O, Zr (NO
3) 45H
2O, La (NO
3)
36H
2O dissolves in the solution that is mixed with the about 0.5mol/L of concentration of metal ions in the deionized water of 1400mL, adds the hydrogenperoxide steam generator of liquor capacity 1%, adds the copper nitrate of solid solution quality 5%.
2) sal volatile of the ammonia spirit of preparation 3mol/L and 3mol/L is mixing in 1: 1 by volume.
3) by proper proportion mixed liquor and precipitating reagent are also flowed stirring under 45 ℃ of waters bath with thermostatic control, 200Kw ultrasound condition, pH value of solution is controlled at 8 in the co-current process.And stream continue to stir 1h after finishing.The polyethylene glycol that adds solid solution quality 8% is then regulated pH to 10.Take out behind 100 ℃ of ageing 4h, leave standstill 12h under the room temperature.
4) sediment process suction filtration, after the deionized water washing, pH=7,120 ℃ of dry 12h.
5) be warming up to 500 ℃ of insulation 4h behind 300 ℃ of roasting 0.5h of dried sample, can obtain hydrogen-storing material.
Concrete, in this step 1), the technical staff can regulate the ratio of rare earth compound as required, whether adds oxidant and auxiliary agent, and adds which kind of oxidant and auxiliary agent and ratio etc. separately thereof;
In this step 3), the technical staff can be as required the experiment condition in this coprecipitation process more, comprise temperature, supersonic frequency;
In this step 5), the technical staff can adjust the temperature and time of roasting according to the resulting actual curve of thermogravimetric analysis (TG).
Embodiment one:
Take by weighing rare earth compound Ce (NO in 0.63: 0.32: 0.05 ratio
3)
36H
2O, Zr (NO
3) 45H
2O, La (NO
3)
36H
2O dissolves in the solution that is mixed with the about 0.5mol/L of concentration of metal ions in the deionized water of 1400mL, adds the hydrogenperoxide steam generator of liquor capacity 1%, adds the barium nitrate of solid solution quality 5%.The ammonia spirit of preparation 3mol/L and the sal volatile of 3mol/L are mixing in 1: 1 by volume, as precipitating reagent.
By proper proportion mixed liquor and precipitating reagent are also flowed stirring under 45 ℃ of waters bath with thermostatic control, 200Kw ultrasound condition, pH value of solution is controlled at 8 in the co-current process.And stream continue to stir 1h after finishing.The polyethylene glycol that adds solid solution quality 8% is then regulated pH to 10.Take out behind 100 ℃ of ageing 4h, leave standstill 12h under the room temperature.Sediment process suction filtration, after the deionized water washing, pH=7,120 ℃ of dry 12h.
Be warming up to 500 ℃ of insulation 4h behind 300 ℃ of roasting 0.5h of dried sample, can obtain molecular formula is 5%Ba-Ce
0.63Zr
0.32La
0.05O
1.95Hydrogen-storing material, the fresh attitude specific area of this hydrogen-storing material is 147.09m
2/ g, oxygen storage capacity are 292.2 μ molg
-1Through 1000 ℃, 10% steam, after 5h was aging, specific area still can reach 46.79m
2/ g, oxygen storage capacity are 201.8 μ molg
-1
Adopt ESEM technology (SEM) that the structure of hydrogen-storing material is characterized, specifically see Fig. 1.Adopt ESEM technology (SEM) that the hydrogen-storing material structure that certain company produces is characterized, specifically see Fig. 2.
Preparation adopts the sample of above-mentioned hydrogen-storing material and noble metal-coating to carry out the sample experiment on homemade sample detector, and the initiation temperature curve is specifically seen Fig. 3.The initiation temperature curve of certain company is specifically seen Fig. 4.
Embodiment two:
Take by weighing rare earth compound Ce (NO in 0.55: 0.35: 0.1 ratio
3)
36H
2O, Zr (NO
3) 45H
2O, La (NO
3)
36H
2O dissolves in the solution that is mixed with the about 0.5mol/L of concentration of metal ions in the deionized water of 1400mL, adds the hydrogenperoxide steam generator of liquor capacity 0.5%, adds the copper nitrate of solid solution quality 5%.The ammonia spirit of preparation 3mol/L and the sal volatile of 3mol/L are mixing in 1: 1 by volume, as precipitating reagent.
By proper proportion mixed liquor and precipitating reagent are also flowed stirring under 80 ℃ of waters bath with thermostatic control, 200Kw ultrasound condition, pH value of solution is controlled at 8 in the co-current process.And stream continue to stir 1h after finishing.The polyethylene glycol that adds solid solution quality 5% is then regulated pH to 10.Leave standstill 12h under the room temperature.Sediment process suction filtration, after the deionized water washing, pH=7,120 ℃ of dry 12h.
Be warming up to 680 ℃ of insulation 4h behind 320 ℃ of roasting 1h of dried sample, can obtain molecular formula is 5%Cu-Ce
0.53Zr
0.35La
0.1O
1.95Hydrogen-storing material.
Claims (3)
1. ternary cerium-based oxygen storage material is characterized in that hydrogen-storing material is made up of hydrogen-storing material main body, auxiliary agent, dispersant, and its weight portion proportioning is:
Hydrogen-storing material main body 80-95 auxiliary agent 3-10 dispersant 2-10;
Described hydrogen-storing material main body is a rare earth material, and rare earth material is made up of cerous nitrate, zirconium nitrate and lanthanum nitrate, and its weight portion proportioning is:
Cerous nitrate 0.5-0.8 zirconium nitrate 0.3-0.45 0.05-0.15 lanthanum nitrate;
Described auxiliary agent is barium nitrate, copper nitrate, manganese nitrate or magnesium nitrate, or wherein any two kinds and arbitrarily two or morely mix with arbitrary proportion, or all mix with arbitrary proportion;
Described dispersant is polyvinyl alcohol, polyethylene glycol or citric acid; Or wherein any two kinds mix with arbitrary proportion, or all mix with arbitrary proportion;
2. as the right 11 described ternary cerium-based oxygen storage material that requires, it is characterized in that it also has oxidant, its weight portion proportioning is:
3. as the preparation technology of right 1 or 2 described hydrogen-storing materials, it is characterized in that preparation technology mainly may further comprise the steps:
1) takes by weighing Ce (NO in proportion
3)
36H
2O, Zr (NO
3)
45H
2O, La (NO
3)
36H
2O is mixed with solution, adds hydrogen peroxide again, adds auxiliary agent, makes mixed liquor;
2) ammonia spirit of preparation 3mol/L and the sal volatile of 3mol/L are mixing in 1: 1 by volume, make precipitated liquid,
3) under 45 ℃ of waters bath with thermostatic control, 200Kw ultrasound condition, mixed liquor and precipitating reagent are pressed 15: 10 weight portion proportioning and flowed stirring, pH value of solution is controlled at 8 in the co-current process, and stream continue to stir 1h after finishing, the polyethylene glycol that adds solid solution quality 8% then, regulate pH to 8-10, take out behind the 80-100 ℃ of ageing 2-4h, leave standstill 8-12h under the room temperature;
4) sediment process suction filtration, after the deionized water washing, pH=7,120 ℃ of dry 10-12h;
5) be warming up to 500 ℃ of insulation 4h behind 300 ℃ of roasting 0.5h of dried sample, can wait until hydrogen-storing material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102744074A (en) * | 2012-07-10 | 2012-10-24 | 江苏高淳陶瓷股份有限公司 | Oxygen storage material for catalytic purification of automobile exhaust and preparation method of oxygen storage matrial |
| 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 |
| CN106268748A (en) * | 2016-09-09 | 2017-01-04 | 南京德普瑞克催化器有限公司 | A kind of high temperature resistant hydrogen-storing material and preparation method thereof |
| CN106311241A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Nickel-based catalyst, preparation method of nickel-based catalyst, reduction state nickel-based catalyst and method for preparing synthesis gas through methane auto-thermal reforming |
| CN106311250A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Nickel-based catalyst, preparation method of nickel-based catalyst, reduction state nickel-based catalyst and method for preparing synthesis gas through methane auto-thermal reforming |
| CN117654582A (en) * | 2024-01-31 | 2024-03-08 | 江苏国盛新材料有限公司 | Cerium-zirconium composite oxide and preparation method thereof |
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| US6387338B1 (en) * | 2000-03-15 | 2002-05-14 | Delphi Technologies, Inc. | Preparation of multi-component Ce, Zr, Mox high oxygen-ion-conduct/oxygen-storage-capacity materials |
| CN1403376A (en) * | 2002-10-15 | 2003-03-19 | 清华大学 | Cerium-base quaternary nano level composite RE oxide and its prepn process |
| CN1449863A (en) * | 2003-04-28 | 2003-10-22 | 华东理工大学 | A kind of nano-cerium-zirconium-based composite oxide and its preparation method |
| CN1935359A (en) * | 2006-10-16 | 2007-03-28 | 华东理工大学 | Spherical cerium-zirconium base composite oxide and its preparing method |
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2011
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Patent Citations (4)
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| US6387338B1 (en) * | 2000-03-15 | 2002-05-14 | Delphi Technologies, Inc. | Preparation of multi-component Ce, Zr, Mox high oxygen-ion-conduct/oxygen-storage-capacity materials |
| CN1403376A (en) * | 2002-10-15 | 2003-03-19 | 清华大学 | Cerium-base quaternary nano level composite RE oxide and its prepn process |
| CN1449863A (en) * | 2003-04-28 | 2003-10-22 | 华东理工大学 | A kind of nano-cerium-zirconium-based composite oxide and its preparation method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102744074A (en) * | 2012-07-10 | 2012-10-24 | 江苏高淳陶瓷股份有限公司 | Oxygen storage material for catalytic purification of automobile exhaust and preparation method of oxygen storage matrial |
| 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 |
| CN106311241A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Nickel-based catalyst, preparation method of nickel-based catalyst, reduction state nickel-based catalyst and method for preparing synthesis gas through methane auto-thermal reforming |
| CN106311250A (en) * | 2015-06-19 | 2017-01-11 | 中国石油化工股份有限公司 | Nickel-based catalyst, preparation method of nickel-based catalyst, reduction state nickel-based catalyst and method for preparing synthesis gas through methane auto-thermal reforming |
| CN106268748A (en) * | 2016-09-09 | 2017-01-04 | 南京德普瑞克催化器有限公司 | A kind of high temperature resistant hydrogen-storing material and preparation method thereof |
| CN117654582A (en) * | 2024-01-31 | 2024-03-08 | 江苏国盛新材料有限公司 | Cerium-zirconium composite oxide and preparation method thereof |
| CN117654582B (en) * | 2024-01-31 | 2024-04-23 | 江苏国盛新材料有限公司 | Cerium-zirconium composite oxide and preparation method thereof |
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