CN103908959A - Ce-Zr composite alumina oxide material and preparation method thereof - Google Patents
Ce-Zr composite alumina oxide material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Ce-Zr composite alumina oxide material and a preparation method thereof, relates to a rare earth material for automobile exhaust purification catalysts, and belongs to the technical field of rare earth materials. The Ce-Zr composite alumina material is prepared from the following ingredients in molar ratio (based on total composite oxide amount): 5-25mol% of cerium oxide, 5-25mol% of zirconium oxide and 70 mol% of alumina. A coprecipitation method is adopted for preparation, the Ce-Zr composite alumina material is calcinated at 880 DEGC, the specific surface area can be more than 210m<2>/g, and the pore volume can be more than 0.5cc/g; the Ce-Zr composite alumina material is calcinated at 1000 DEG C and aged, the specific surface area is still larger than 110m<2>/g, and the pore volume can be more than 0.3cc/g. The Ce-Zr composite alumina material has the relatively large specific surface area, the good heat stability and texture stability and the good catalytic activity and is widely applied to the automobile exhaust purification catalysts, combustion catalysts and other catalysts.
Description
Technical field
The invention belongs to rare earth material technical field, relate to a kind of rare earth material for cleaning catalyst for tail gases of automobiles, refering in particular to is Ce-Zr composite aluminium oxide material and preparation method thereof.
Background technology
As everyone knows, vehicle exhaust is the primary pollution source that causes atmosphere pollution, pollutant mainly contains hydrocarbon (HC), carbon monoxide (CO), nitrogen oxide (NOx), in addition, also have the harmful substances such as sulfur dioxide, not only severe contamination atmosphere, worsen environment, and directly threaten, people's is healthy.A large amount of human and material resources are all dropped in countries in the world, financial resources are administered automobile exhaust pollution, and most countries has all been formulated automobile exhaust emission standard increasingly strict, requires all motor vehicle discharged tail gas all must reach the required standards.
In the harsh environment of the high temperature such as catalytic cleaning of car tail gas, catalytic combustion, catalyst carrier alumina, due to the reason such as phase transformation and sintering, causes the very fast minimizing of specific area, thereby causes catalyst activity reduction.Therefore at high temperature there are larger specific surface and good heat endurance in the urgent need to development and exploitation.From the sixties in 20th century, many scholars have carried out large quantity research on alumina sintering and phase-change mechanism, find if effectively remove hydroxyl and the yin, yang ion cavities of alumina surface, just can improve the heat endurance of aluminium oxide, stop high temperature sintering and phase transformation and maintain its high-specific surface area.ZrO
2be conventional catalyst carrier, there is the effect that accelerating oxidation alumina transmits.In the research of modified aluminas, find to add ZrO
2can improve activity and the heat endurance of catalyst, in addition matrix γ-Al
2o
3with ZrO
2can interact.Ce can enter carrier A l
2o
3endoporus, can be evenly distributed on the surfaces externally and internally of sample, has good anti-sintering property.Ce can improve the heat endurance of aluminium oxide, and under reduction and Redox Condition, the stabilization of Ce is comparatively outstanding, and Ce forms CeAlO
3can stop crystal growth and phase transformation.
The present invention has larger specific area, good heat endurance, texture stability and catalytic activity preferably.Through 1000 DEG C of aging lower processing of calcining, still there is the specific area that is greater than 110m2/g, more than pore volume can reach 0.3cc/g.
Summary of the invention
For the deficiency existing in background technology, the invention provides a kind of specific area large, pore volume is large, and at high temperature specific area and pore volume keep rare earth material of higher stability and preparation method thereof.
On the material of the present invention's research, be mainly, at cerium zirconium aluminium composite material, different cerium zirconium ratios are carried out to modification, make catalysis material have significant effect on catalysis HC and these tail gas of CO.The initial specific surface of this material is good simultaneously, pore volume is also very large, and good transmitter substance in vent gas treatment process, makes HC be converted into water and carbon dioxide, and CO is converted into carbon dioxide.This material is at home without any manufacturer production simultaneously, and the new material of Shi Wo company independent research has certain competitive advantage in market.
For achieving the above object, the invention provides following technical scheme: Ce-Zr composite aluminium oxide material, mainly comprise cerium oxide, zirconia and aluminium oxide, composition component mole is configured to, in composite oxides total amount, cerium oxide 5mol%～25mol%, zirconia 5mol%～25mol%, aluminium oxide 70%, its crystal phase structure is cerium zirconium sosoloid, the low cerium type rare earth material that described material is prepared through roasting in 3 hours at 880 DEG C, its specific surface>=210m
2/ g, more than pore volume can reach 0.5cc/g, material at 1000 DEG C after roasting in 5 hours, its specific surface>=110m
2/ g, more than pore volume can reach 0.3cc/g.
Ce-Zr composite aluminium oxide material provided by the invention can be prepared by following process, and described process comprises following processing step:
(1), nitrate mixed solution processed and alkaline solution: the nitrate mixed solution by given material composition component preparation taking precursor cerous nitrate, zirconium nitrate and the aluminum nitrate of material institute oxidation-containing cerium, zirconia and aluminium oxide as solute, and alkaline solution using preparation as precipitating reagent;
(2), precipitation, ageing: add respectively oxidant and surfactant in nitrate mixed solution, nitrate mixed solution and alkaline solution with and the mode of flowing import reaction vessel and carry out precipitation reaction, and stir on two Bing Liu limit, solution limits, the pH value of precipitation reaction liquid remains on 8.0～9.3, then under the condition of 80～100 DEG C ageing >=6 hour;
(3), slurrying material: the reaction paste after ageing is carried out to Separation of Solid and Liquid by the mode of suction filtration or press filtration, and the solid phase of separating is first washed, then is mixed with slurry with surfactant and water;
(4), Ce-Zr composite aluminium oxide material processed: the above-mentioned slurry making carries out mist projection granulating by spray-dired mode, after powder after spraying is dry under the condition of 70～100 DEG C, under the condition of 880 DEG C, calcine 3 hours again, make Ce-Zr composite aluminium oxide material.
Above-mentioned nitrate mixed solution is by oxide weight concentration >=5%, and described precipitating reagent alkaline solution is selected from the one in three kinds of ammoniacal liquor, sal volatile, ammoniacal liquor and sal volatiles, precipitant solution pH value >=8.5.
Above-mentioned surfactant is for being selected from polyethylene glycol or polyvinyl alcohol.
The above-mentioned oxidant adding in nitrate mixed solution and surfactant, oxidant is hydrogen peroxide, and the molal weight of its consumption and cerium is 1.2:1, and the weight concentration of surfactant is the 30wt% of the weight concentration of precipitation reaction liquid.
The pH value of above-mentioned precipitation reaction liquid is 8.5～9.3.
The present invention's beneficial effect compared to existing technology: the preparation of Ce-Zr composite aluminium oxide material of the present invention, production equipment does not relate to pressure vessel, and production technology is simple, and investment of production equipment expense is low.
Brief description of the drawings
Fig. 1 is preparation technology's flow chart of the present invention;
Fig. 2 is fresh sample XRD spectra;
Fig. 3 is sample XRD spectra after aging 1000 DEG C.
Detailed description of the invention
Below in conjunction with drawings and Examples, to the specific embodiment of the present invention as preferred detailed description.Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
Shown in Fig. 1-Fig. 3, the said Ce-Zr composite aluminium oxide material of the present invention, mainly comprises cerium oxide, zirconia and aluminium oxide, and its structural formula can be expressed Ce
xzr
yaL
z, its molar ratio control range x is that 0.05～0.25, y is that 0.05～0.25, z is 0.70, the component of oxide mole is configured to cerium oxide 5mol%～25mol%, zirconia 5mol%～25mol%, aluminium oxide 70mol%.Material was through 880 DEG C of roastings 3 hours, and specific area is at 210m
2more than/g, more than pore volume can reach 0.5cc/g; At 1000 DEG C, after roasting in 5 hours, specific area is at 110m
2more than/g, pore volume is not less than 0.3cc/g.
Shown in Figure 1, Ce-Zr composite aluminium oxide material provided by the invention can be prepared by following process, and described process comprises following processing step:
, amount cerous nitrate, zirconium nitrate, the aluminum nitrate of the nitrate that converts out according to the amount of the oxide of given component, these nitrate are prepared into nitrate mixed solution, prepare the alkaline solution as precipitating reagent simultaneously;
(2), in nitrate mixed solution, once add oxidant (with the molal weight 1.2:1 of cerium oxide) and surfactant, then with precipitating reagent with and the mode of flowing import reaction vessel and carry out precipitation reaction, and stir on two Bing Liu limit, solution limits, the pH value of precipitation reaction liquid remains on 8.0～9.3, then ageing is no less than 3 hours under 80～100 DEG C of conditions;
(3) the reaction paste, after ageing is undertaken after Separation of Solid and Liquid, washing by suction filtration or press filtration mode, then is mixed with slurries with surfactant and water;
, the slurry that makes carries out mist projection granulating by spray-dired mode, the powder after spraying carries out after 70～100 DEG C of dry processing, the temperature lower calcinations of 880 DEG C 3 hours, makes Ce-Zr composite aluminium oxide material.
In above-mentioned preparation technology, said precipitant solution is alkaline solution, and precipitating reagent used is ammoniacal liquor, ammonium carbonate, ammoniacal liquor and ammonium carbonate mixed liquor conventionally, and the PH of precipitating reagent is not less than 8.5.Because they improve significantly the heat endurance of material in the process of preparing hydrogen-storing material.We have chosen taking ammonium carbonate and ammonia water mixture as precipitating reagent in preparation, and wherein ammoniacal liquor and ammonium carbonate mol ratio are controlled between 2-5:2-5.
At the PH for preparing our wayward nitrate in nitrate solution, should not directly control the ratio of their additions by controlling the addition of nitrate mixed solution and precipitating reagent, therefore by adopting and the mode of flowing joins reaction vessel limit edged and stirs and carry out coprecipitation reaction and control the pH value of coprecipitation reaction liquid and should not be less than 8.0, the preferential scope of selecting, 8.0～9.3, reaches by the flow velocity that regulates nitrate mixed solution and precipitating reagent.
In the above-mentioned method of preparing Ce-Zr composite aluminium oxide material, said surfactant is selected from least one of polyvinyl alcohol and polyethylene glycol, also can be that polyvinyl alcohol and polyethylene glycol are jointly as surfactant, preferentially select using polyvinyl alcohol and polyethylene glycol jointly as surfactant, wherein two kinds of surfactants divide two processing, first with surfactant, nitrate mixed solution is processed, as the protective agent of precipitating reagent; Then in sediment is processed, be mixed with by sediment and surfactant, water that slurries realize.Wherein sedimentary weight is at 6wt%～25wt% for the slurries of preparation, and the weight of surfactant accounts for 10wt%～40wt%.
In the method for the Ce-Zr composite aluminium oxide material of above-mentioned preparation, slurry carries out mist projection granulating by spray-dired mode in Separation of Solid and Liquid, obtains more uniform spheric granules and deals with comparison aspect, easily realizes industrialization.
The present invention is for the Ce-Zr composite aluminium oxide material preparing after 880 DEG C of calcining 3h, and its specific area can reach 210m
2more than/g, more than pore volume can reach 0.5cc/g.After 1000 DEG C of aging 5h of calcining, its specific area can reach 110m
2more than/g, more than pore volume can reach 0.3cc/g.Rare earth material than prior art is compared, and the one, specific surface and pore volume have all obtained increasing substantially.The 2nd, very good in the stability of texture property (particularly in specific area).
According to the preparation method of co-precipitation, 5 kinds of different cerium zirconiums are calculated than (Ce/Zr value is respectively 0.05/0.25,0.10/0.20,0.15/0.15,0.20/0.10,0.25/0.05).It is the cerium oxide of given material composition, zirconia, metal element content in aluminium oxide, calculate the precursor cerous nitrate of each oxide, zirconium nitrate and aluminum nitrate, be mixed with nitrate mixed solution, then add with 30% surfactant of the hydrogen peroxide of the molal weights such as cerous nitrate and metal oxide total content and process, surfactant is that concentration is 10% poly-vinyl alcohol solution, then adopt and flow joining in reaction vessel that mode and ammonium carbonate and ammoniacal liquor mixed solution limit edged stir, the addition of precipitating reagent keeps between 8.8-8.5 the pH value of reaction solution, slurry after reacting completely is put into water-bath ageing 6 hours, approximately 90 DEG C of Aging Temperatures, reacted slurry carries out Separation of Solid and Liquid by the mode of suction filtration, wash 2～3 with pure water, solid phase after having washed adds approximately 30% surfactant (polyglycol solution that concentration is 40%) and water furnishing slurry, the spray-dried mode of slurry is carried out mist projection granulating, powder after spraying dries 2 hours at 100 DEG C, roasting 3 hours at 880 DEG C again, make products C e-Zr composite aluminium oxide material.
The specific surface that table 1 is fresh and pore volume
Specific surface, the pore volume of measuring each Embodiment C e-Zr composite aluminium oxide material sample by NOVA series of high speed specific surface and voidage analyzer employing BET method, the results are shown in table 1.The specific surface, pore volume that can find out No. 1 and No. 3 all apparently higher than other cerium zirconium than material, and on fresh pore volume in preparation process cerium zirconium sosoloid have and be dispersed in preferably on activated alumina, so there is larger pore volume.
Specific surface after table 2 is aging and pore volume
Material is through 1000 DEG C of 5h, specific surface: No. >3, No. 1 >4 >4 of No. 5 > ≈, pore volume: No. >2, No. 5 >4 >3 of No. 1 ≈, the aging specific surface that can find out No. 5 and No. 1 on figure is larger, but be more or less the same compared with No. 1, pore volume remain No. 1 best.
By the preparation method of co-precipitation, to the Ce-Zr composite aluminium oxide material of 5 kinds of different cerium zirconium ratios, drawn by above data: the ratio of Ce:Zr=0.05:0.25 is best.Ce-Zr composite aluminium oxide material of the present invention has higher specific surface and pore volume, after 1000 DEG C of 5h, can keep good specific surface and pore volume, and structure thermal stability is good and heat-resistant stable is good.
The above is only the preferred embodiment of the present invention, it should be pointed out that for those skilled in the art, is not departing under the prerequisite of the technology of the present invention principle, makes some improvement and modification and also should be considered as protection scope of the present invention.
Claims (6)
1.Ce-Zr composite aluminium oxide material, it is characterized in that: mainly comprise cerium oxide, zirconia and aluminium oxide, composition component mole is configured to, in composite oxides total amount, cerium oxide 5mol%～25mol%, zirconia 5mol%～25mol%, aluminium oxide 70%, its crystal phase structure is cerium zirconium sosoloid, the low cerium type rare earth material that described material is prepared through roasting in 3 hours at 880 DEG C, its specific surface>=210m
2/ g, more than pore volume can reach 0.5cc/g, material at 1000 DEG C after roasting in 5 hours, its specific surface>=110m
2/ g, more than pore volume can reach 0.3cc/g.
2. the preparation method of Ce-Zr composite aluminium oxide material according to claim 1, is characterized in that: comprise following processing step:
(1), nitrate mixed solution processed and alkaline solution: the nitrate mixed solution by given material composition component preparation taking precursor cerous nitrate, zirconium nitrate and the aluminum nitrate of material institute oxidation-containing cerium, zirconia and aluminium oxide as solute, and alkaline solution using preparation as precipitating reagent;
(2), precipitation, ageing: add respectively oxidant and surfactant in nitrate mixed solution, nitrate mixed solution and alkaline solution with and the mode of flowing import reaction vessel and carry out precipitation reaction, and stir on two Bing Liu limit, solution limits, the pH value of precipitation reaction liquid remains on 8.0～9.3, then under the condition of 80～100 DEG C ageing >=6 hour;
(3), slurrying material: the reaction paste after ageing is carried out to Separation of Solid and Liquid by the mode of suction filtration or press filtration, and the solid phase of separating is first washed, then is mixed with slurry with surfactant and water;
(4), Ce-Zr composite aluminium oxide material processed: the above-mentioned slurry making carries out mist projection granulating by spray-dired mode, after powder after spraying is dry under the condition of 70～100 DEG C, under the condition of 880 DEG C, calcine 3 hours again, make Ce-Zr composite aluminium oxide material.
3. the preparation method of Ce-Zr composite aluminium oxide material as claimed in claim 2, it is characterized in that: described nitrate mixed solution is by oxide weight concentration >=5%, described precipitating reagent alkaline solution is selected from the one in three kinds of ammoniacal liquor, sal volatile, ammoniacal liquor and sal volatiles, precipitant solution pH value >=8.5.
4. the preparation method of Ce-Zr composite aluminium oxide material as claimed in claim 2, is characterized in that: described surfactant is for being selected from polyethylene glycol or polyvinyl alcohol.
5. the preparation method of Ce-Zr composite aluminium oxide material as claimed in claim 2, be characterised in that: the described oxidant adding in nitrate mixed solution and surfactant, oxidant is hydrogen peroxide, the molal weight of its consumption and cerium is 1.2:1, and the weight concentration of surfactant is the 30wt% of the weight concentration of precipitation reaction liquid.
6. the preparation method of Ce-Zr composite aluminium oxide material as claimed in claim 2, is characterized in that: the pH value of described precipitation reaction liquid is 8.5～9.3.
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| CN106732578A (en) * | 2016-11-14 | 2017-05-31 | 北京工业大学 | A kind of mesoporous cerium zirconium aluminum composite oxides carried noble metal nanocatalyst of efficient cryogenic, preparation method and applications |
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| CN110404592A (en) * | 2019-08-29 | 2019-11-05 | 昆明冶金研究院 | A kind of preparation method of low sodium catalyst carrier for purifying vehicle tail gas |
| CN112456979A (en) * | 2020-12-07 | 2021-03-09 | 深圳陶陶科技有限公司 | Preparation method of zirconia toughened alumina powder and ceramic |
| CN115916921A (en) * | 2021-06-14 | 2023-04-04 | 第一稀元素化学工业株式会社 | Composite oxide powder, friction material composition, and friction material |
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