CN102716733A - Preparation method of high performance cerium zirconium aluminum oxygen-storage material - Google Patents
Preparation method of high performance cerium zirconium aluminum oxygen-storage material Download PDFInfo
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- CN102716733A CN102716733A CN2012101488846A CN201210148884A CN102716733A CN 102716733 A CN102716733 A CN 102716733A CN 2012101488846 A CN2012101488846 A CN 2012101488846A CN 201210148884 A CN201210148884 A CN 201210148884A CN 102716733 A CN102716733 A CN 102716733A
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Abstract
The invention relates to a preparation method of a high performance cerium zirconium aluminum oxygen-storage material, which comprises the following steps: 1) mixing boehmite, deionized water and a nitric acid solution with mass ratio of 1:10-20:0.1-0.5 and then stirring; 2) taking zirconium and cerium as well as soluble salts of rare earth elements such as lanthanum, yttrium, praseodymium and neodymium, adding deionized water to prepare a cerium zirconium mixed aqueous solution; 3) mixing aluminum sol and the cerium zirconium mixed aqueous solution with the mass ratio of (Ce-Zr) to Al2O3 being 1:0.1-3 and then stirring; 4) mutually and uniformly mixing an organic polymer modifier and 2-6 mol of an alkaline precipitant with the mass ratio of 5-10:90-95; 5) mixing the cerium zirconium aluminum composite sol and the modified alkaline precipitant and then coprecipitating; 6) carrying out vacuum pumping filtration and washing for the cerium zirconium aluminum hydroxide gel; 7) placing the cerium zirconium aluminum hydroxide gel in a muffle furnace for calcining; and 8) crushing the burned material to obtain the cerium zirconium aluminum product. The preparation method of the high performance cerium zirconium aluminum oxygen-storage material has simple steps, and the cerium zirconium aluminum oxygen-storage material has good high thermostability.
Description
Technical field
The present invention relates to a kind of preparation method of high-performance cerium zirconium aluminium hydrogen-storing material.
Background technology
Cerium zirconium aluminum composite oxides is a kind of novel rare earth hydrogen-storing material, has the common advantage of hydrogen-storing material and activated alumina concurrently.Thereby it purifies and shows more excellent heat endurance and oxygen storage capacity at three-effect catalysis purification (TWC), catalytic combustion, diesel engine DOC, POC.
The method for preparing at present cerium zirconium aluminum composite oxides mainly contains infusion process, coprecipitation, sol-gel process, microemulsion method, mechanical mixing etc.Wherein, coprecipitation is simple because of technology, condition is easy to control, the product homogeneity is good, production cost is lower, be convenient to advantage such as suitability for industrialized production has obtained using widely, but existing coprecipitation complicated steps, and production cost is high.
Summary of the invention
For solving the problems of the technologies described above, the present invention provides a kind of preparation method of high-performance cerium zirconium aluminium hydrogen-storing material, and step is simple, and prepared cerium zirconium aluminium hydrogen-storing material has excellent heat endurance and oxygen storage capacity.
The preparation method of high-performance cerium zirconium aluminium hydrogen-storing material of the present invention may further comprise the steps:
1) boehmite is processed aluminium colloidal sol with nitric acid reaction, diaspore: deionized water: the mass ratio of salpeter solution is 1: 10-20: 0.1-0.5 mixing stirring obtains finely dispersed aluminium colloidal sol, Al in the diaspore
2O
3Mass fraction be 70%, the mass fraction of nitric acid is 60% in the salpeter solution;
2) take zirconium and cerium and rare earth element-doped lanthanum, yttrium, praseodymium, neodymium soluble salt, add deionized water to make a total ion concentration of 0.5-1.5mol / l aqueous solution of cerium-zirconium mixed, the mixed solution of Ce and Zr molar ratio of 0.5 - 3; rare earth doping element is lanthanum, yttrium, praseodymium, neodymium, one or more, by weight of the cerium-zirconium 2-10%;
3) the aluminium colloidal sol and the step 2 that step 1) are obtained) the cerium zirconium mixed liquor that obtains presses (Ce-Zr): Al
2O
3Mass ratio is 1: 0.1-3 mixing stirring obtain finely dispersed cerium zirconium aluminium complex sol, and to control its oxide total concentration is 50-100g/l;
4) alkaline precipitating agent of organic polymer modifier and the 2-6mol mass ratio according to 5-10: 90-95 is mixed each other, obtain the modified alkaline precipitating reagent;
5) with the cerium zirconium aluminium complex sol of step 3) acquisition and the modified alkaline precipitating reagent mixing co-precipitation of step 4) acquisition, control terminal point PH＞8 obtain cerium zirconium aluminium hydroxide gel;
6) cerium zirconium aluminium hydroxide gel is carried out vacuum filtration and washing, control washing electrical conductivity＜20ms/cm;
7) the cerium zirconium aluminium hydroxide gel that step 6) is obtained places in the Muffle furnace to be calcined, and 700-800 ℃ of control temperature calcined 2-6 hour;
8) thing that burns till that step 7) is obtained is pulverized the cerium zirconium aluminium product that obtains different-grain diameter through mechanical disintegration or air-flow.
The preparation method of high-performance cerium zirconium aluminium hydrogen-storing material of the present invention; In step 2) in: the soluble-salt of said cerium is cerous nitrate, ammonium ceric nitrate, cerous acetate, cerium chloride; The soluble-salt of said zirconium is zirconium nitrate, acetic acid zirconium, zirconium oxychloride, and the soluble-salt of said rear-earth-doped element lanthanum, yttrium, praseodymium, neodymium is nitrate, acetate, chloride.
The preparation method of high-performance cerium zirconium aluminium hydrogen-storing material of the present invention is in step 4): said organic polymer modifier organic polymer acids or alcohols.
The preparation method of high-performance cerium zirconium aluminium hydrogen-storing material of the present invention, in step 4): said alkaline precipitating agent is one or more in ammoniacal liquor, ammonium carbonate, the carbonic hydroammonium.
Beneficial effect compared with prior art of the present invention is: preparation method's step of high-performance cerium zirconium aluminium hydrogen-storing material of the present invention is simple; Zirconates and cerium salt with boehmite, solubility are raw material; Carrying out the peptization reaction and process colloidal sol, is precipitating reagent with alkali, and organic polymer acids, alcohols are modifier; Colloidal sol through organically-modified alkali lye post precipitation, is filtered, washs, calcines, pulverizes and make sediment.Prepared cerium zirconium aluminium hydrogen-storing material under 700 ℃-800 ℃ condition calcination 2-6 hour is tested its fresh specific area 120-140m
2/ g, 10 hours aging specific area＞60m of calcination under 1000 ℃ the condition
2/ g, 10 hours aging specific area＞40m of calcination under 1100 ℃ the condition
2/ g, prepared cerium zirconium aluminium hydrogen-storing material has good high thermal stability.
The specific embodiment
Below in conjunction with embodiment, specific embodiments of the invention describes in further detail.Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Embodiment 1
Get 64.3g boehmite (Al
2O
3: 70%), add deionized water 800ml, salpeter solution (the nitric acid mass fraction is 60%) 12ml mixes stirring and obtains aluminium colloidal sol; Get cerous nitrate 66.7ml (TREO:225g/L), zirconium nitrate 148.5ml (ZrO respectively
2: 202g/L), after lanthanum nitrate 20.8ml (TREO:240g/L), yttrium nitrate 20.8ml (TREO:240g/L) mix, join in the aluminium colloidal sol, and add pure water and be diluted to 1500ml, obtaining mass ratio is CeO
2: ZrO
2: La
2O
3: Y
2O
3: Al
2O
3=15: 30: 5: 5: 45 cerium zirconium aluminium colloidal sol; Modification aluminium colloidal sol is at room temperature joined in the ammoniacal liquor of the 4.6mol/L that is dissolved with 7.6% polymeric organic acid and precipitate; Controlling final PH is 8.3; Deposition finishes the final vacuum suction filtration and the electrical conductivity of washing to the washing lotion is 18ms/cm, obtains cerium zirconium aluminium hydroxide gel.Cerium zirconium alumina gel was obtained cerium zirconium aluminum oxide in 4 hours 700 ℃ of calcinings, and testing its specific area is 132.6m
2/ g, 1000 ℃ of 10 hours aging specific areas are 66.8m
2/ g, 1100 ℃ of 10 hours aging specific areas are 45.5m
2/ g.
Embodiment 2
Get 64.3g boehmite (Al
2O
3: 70%), add deionized water 800ml, salpeter solution (the nitric acid mass fraction is 60%) 15ml mixes stirring and obtains aluminium colloidal sol; Get cerous nitrate 133.3ml (TREO:225g/L), zirconium nitrate 74.2ml (ZrO respectively
2: 202g/L), after lanthanum nitrate 20.8ml (TREO:240g/L), yttrium nitrate 20.8ml (TREO:240g/L) mix, join in the aluminium colloidal sol, and add pure water and be diluted to 1500ml, obtaining mass ratio is CeO
2: ZrO
2: La
2O
3: Y
2O
3: Al
2O
3=30: 15: 5: 5: 45 cerium zirconium aluminium colloidal sol; Modification aluminium colloidal sol is at room temperature joined in the ammoniacal liquor of the 3.2mol/L that is dissolved with 6.5% polymeric organic acid and precipitate; Controlling final PH is 8.5; Deposition finishes the final vacuum suction filtration and the electrical conductivity of washing to the washing lotion is 16ms/cm, obtains cerium zirconium aluminium hydroxide gel.Cerium zirconium alumina gel calcined under 700 ℃ condition obtained cerium zirconium aluminum oxide in 4 hours, testing its specific area is 126.3m
2/ g, 10 hours aging specific areas of calcining are 62.6m under 1000 ℃ the condition
2/ g, 10 hours aging specific areas of calcining are 42.7m under 1100 ℃ the condition
2/ g.
Embodiment 3
Get 42.8g boehmite (Al
2O
3: 70%), add deionized water 600ml, salpeter solution (the nitric acid mass fraction is 60%) 10ml mixes stirring and obtains aluminium colloidal sol; After getting cerous nitrate 133.3ml (TREO:225g/L), zirconium nitrate 148.5ml (ZrO2:202g/L), lanthanum nitrate 20.8ml (TREO:240g/L), yttrium nitrate 20.8ml (TREO:240g/L) mixing respectively; Join in the aluminium colloidal sol; And add pure water and be diluted to 1500ml, obtaining mass ratio is CeO
2: ZrO
2: La
2O
3: Y
2O
3: Al
2O
3=30: 30: 5: 5: 30 cerium zirconium aluminium colloidal sol; Modification aluminium colloidal sol is at room temperature joined in the ammoniacal liquor of the 4mol/L that is dissolved with 8% polymeric organic acid and precipitate, controlling final PH is 9.2, and deposition finishes the final vacuum suction filtration and the electrical conductivity of washing to the washing lotion is 12ms/cm, obtains cerium zirconium aluminium hydroxide gel.Cerium zirconium alumina gel was obtained cerium zirconium aluminum oxide in 4 hours 700 ℃ of calcinings, and testing its specific area is 125m2/g, and 10 hours aging specific areas of calcining are 63m under 1000 ℃ the condition
2/ g, 10 hours aging specific areas of calcining are 41m under 1100 ℃ the condition
2/ g.
Preparation method's step of high-performance cerium zirconium aluminium hydrogen-storing material of the present invention is simple; Zirconates and cerium salt with boehmite, solubility are raw material; Carrying out the peptization reaction and process colloidal sol, is precipitating reagent with alkali, and organic polymer acids, alcohols are modifier; Colloidal sol through organically-modified alkali lye post precipitation, is filtered, washs, calcines, pulverizes and make sediment.Prepared cerium zirconium aluminium hydrogen-storing material under 700 ℃-800 ℃ condition calcination 2-6 hour, testing its fresh specific area is 120-140m
2/ g, 10 hours aging specific area＞60m of calcination under 1000 ℃ the condition
2/ g, 10 hours aging specific area＞40m of calcination under 1100 ℃ the condition
2/ g, prepared cerium zirconium aluminium hydrogen-storing material has good high thermal stability.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from know-why of the present invention; Can also make some improvement and modification, these improve and modification also should be regarded as protection scope of the present invention.
Claims (4)
1. the preparation method of a high-performance cerium zirconium aluminium hydrogen-storing material is characterized in that, may further comprise the steps:
1) boehmite is processed aluminium colloidal sol, diaspore with nitric acid reaction; Deionized water: the mass ratio of salpeter solution is 1: 10-20: 0.1-0.5 mixing stirring obtains finely dispersed aluminium colloidal sol, Al in the diaspore
2O
3Mass fraction be 70%, the mass fraction of nitric acid is 60% in the salpeter solution;
2) take zirconium and cerium and rare earth element-doped lanthanum, yttrium, praseodymium, neodymium soluble salt, add deionized water to make a total ion concentration of 0.5-1.5mol / l aqueous solution of cerium-zirconium mixed, the mixed solution of Ce and Zr molar ratio of 0.5 - 3; rare earth doping element is lanthanum, yttrium, praseodymium, neodymium, one or more, by weight of the cerium-zirconium 2-10%;
3) the aluminium colloidal sol and the step 2 that step 1) are obtained) the cerium zirconium mixed liquor that obtains presses (Ce-Zr): Al
2O
3Mass ratio is 1: 0.1-3 mixing stirring obtain finely dispersed cerium zirconium aluminium complex sol, and to control its oxide total concentration is 50-100g/l;
4) alkaline precipitating agent of organic polymer modifier and the 2-6mol mass ratio according to 5-10: 90-95 is mixed each other, obtain the modified alkaline precipitating reagent;
5) with the cerium zirconium aluminium complex sol of step 3) acquisition and the modified alkaline precipitating reagent mixing co-precipitation of step 4) acquisition, control terminal point PH＞8 obtain cerium zirconium aluminium hydroxide gel;
6) cerium zirconium aluminium hydroxide gel is carried out vacuum filtration and washing, control washing electrical conductivity＜20ms/cm;
7) the cerium zirconium aluminium hydroxide gel that step 6) is obtained places in the Muffle furnace to be calcined, and 700-800 ℃ of control temperature calcined 2-6 hour;
8) thing that burns till that step 7) is obtained is pulverized the cerium zirconium aluminium product that obtains different-grain diameter through mechanical disintegration or air-flow.
2. the preparation method of high-performance cerium zirconium aluminium hydrogen-storing material according to claim 1; It is characterized in that; In step 2) in: the soluble-salt of said cerium is cerous nitrate, ammonium ceric nitrate, cerous acetate, cerium chloride; The soluble-salt of said zirconium is zirconium nitrate, acetic acid zirconium, zirconium oxychloride, and the soluble-salt of said rear-earth-doped element lanthanum, yttrium, praseodymium, neodymium is nitrate, acetate, chloride.
3. the preparation method of high-performance cerium zirconium aluminium hydrogen-storing material according to claim 1 is characterized in that, in step 4): said organic polymer modifier organic polymer acids or alcohols.
4. the preparation method of high-performance cerium zirconium aluminium hydrogen-storing material according to claim 1 is characterized in that in step 4): said alkaline precipitating agent is one or more in ammoniacal liquor, ammonium carbonate, the carbonic hydroammonium.
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| CN107349923A (en) * | 2017-07-10 | 2017-11-17 | 中自环保科技股份有限公司 | Blending ingredients material and preparation method thereof |
| CN107694556A (en) * | 2017-10-17 | 2018-02-16 | 高俊 | A kind of preparation method of high storage oxygen high heat stability type hydrogen-storing material |
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| WO2022090404A1 (en) * | 2020-10-29 | 2022-05-05 | Basf Corporation | Three-way diesel catalyst for cold start technology |
| WO2022137910A1 (en) * | 2020-12-24 | 2022-06-30 | 三井金属鉱業株式会社 | Composite oxide and method for producing same |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104128173A (en) * | 2014-08-12 | 2014-11-05 | 淄博加华新材料资源有限公司 | Low-cost high-performance supported catalyst and preparation method thereof |
| CN104190438A (en) * | 2014-08-12 | 2014-12-10 | 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 |
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| CN107694556A (en) * | 2017-10-17 | 2018-02-16 | 高俊 | A kind of preparation method of high storage oxygen high heat stability type hydrogen-storing material |
| CN108970602A (en) * | 2018-08-01 | 2018-12-11 | 湖南稀土金属材料研究院 | Hydrogen-storing material and its preparation method and application |
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| WO2022090404A1 (en) * | 2020-10-29 | 2022-05-05 | Basf Corporation | Three-way diesel catalyst for cold start technology |
| WO2022137910A1 (en) * | 2020-12-24 | 2022-06-30 | 三井金属鉱業株式会社 | Composite oxide and method for producing same |
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