CN1449863A - Nano Cerium-zirconium base compound oxide and preparation process thereof - Google Patents
Nano Cerium-zirconium base compound oxide and preparation process thereof Download PDFInfo
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Abstract
The present invention discloses a nano cerium zirconium based compound oxide and its preparation method. Said invented cerium zirconium based compound oxide includes (wt%) 10-90% of CeO2 and 10-90% of ZrO2, and its crystal grain size is greater than or equal to 4 nm or less than or equal to 80 nm. Its preparation method includes the following steps: dissolving nitrates of Ce, Zr and one or more than one metal elements B (B is Ca or Sr or Ba or Mn or Al or Si or any one of rare earth elements except for Ce) in water to prepare solution (I); using hydrogen peroxide and ammonia water and dissolving them in the water to obtain solution (II); adding solution (I) and solution (II) into ammonia water solution, reacting, ageing, suction filtering, drying and roasting at 500-1000 deg.C so as to obtain the invented product with higher chemical activity and thermal stability.
Description
Technical field
The present invention relates to a kind of catalysis material, be specifically related to a kind of catalysis material that is used for three-effect catalyst for purifying tail gas of car (TWC) and combustion catalyst.
Background technology
The pollution problem that motor vehicle exhaust emission produces has been subjected to paying attention to widely in current society.The catalytic purification of vehicle exhaust is a kind of effective way that reduces atmosphere pollution.Auto-exhaust catalyst can be with the harmful components CO in the tail gas, HC and NO
xChange into harmless CO
2, H
2O and N
2After remove, so claim three-way catalyst (TWC), the existing oxidation reaction of the reaction that it relates to simultaneously has reduction reaction again.Cleaning catalyst for tail gases of automobiles is different from most industrial catalyst, its operating condition (as temperature, capacity, gas composition etc.) is along with the difference of running car situation, all be in the variation, it is an operating process under unsteady state condition, the air-fuel ratio that is engine is in change near the scope of chemically correct fuel always, is divided into " poor combustion " and " rich combustion ".
In three-effect catalyst for purifying tail gas of car, CeO
2It is an important component.Because CeO
2Animal migration and cationic variable valency characteristic with Lattice Oxygen, by
(0 * 0.5) reaction possesses the ability that stores oxygen and discharge oxygen, thus the fluctuation of control reaction system oxygen content.When poor combustion, Ce
2O
3Can store oxygen, to guarantee NO
xBy CO and HC reduction, when richness is fired, CeO
2Can discharge oxygen, CO and the required oxygen of HC oxidation are provided, and CeO
2Itself also has catalytic activity, helps o'clock to eliminate CO, HC and NO at air/fuel simultaneously than λ=14.6
xThree kinds of pollutants.But pure CeO
2Easily sintering takes place at high temperature, particle is grown up, and causes specific area to reduce, thereby reduce until losing oxygen storage capacity (OSC), and can and γ-Al
2O
3Interact and form CeAlO
3Thereby, oxygen storage capacity is descended, influenced its promoting catalysis in three-way catalyst.Therefore, improve CeO
2Heat endurance be very important.Discovering in recent years, the interpolation of Zr and La can stop CeO effectively
2Sintering, particularly the cerium zirconium sosoloid of Sheng Chenging more helps to stop CeO
2Sintering, Zr
4+Adding can increase CeO
2In the mobility of oxygen, reduce Ce
4+The reduction activation energy, reduce the initial reduction temperature of body phase, thereby make cerium zirconium sosoloid have higher oxygen storage capacity; The simultaneous oxidation zirconium is the extraordinary oxide of a kind of heat endurance, and its interpolation can improve the heat endurance of cerium zirconium sosoloid.With pure CeO
2Compare, cerium zirconium sosoloid has good redox property and storage oxygen performance, and higher heat endurance and excellent low-temperature catalyzed performance have become the critical material of young mobile tail gas three-way catalyst.Therefore the preparation that has high-specific surface area, high oxygen storage power and high thermal stability cerium zirconium sosoloid is a technology with very high practical value.
Patent CN1263868A discloses a kind of nanometer cerium zirconium oxide and preparation method and purposes.This oxide comprises the CeO of 4～98% weight
2ZrO with 1～95% weight
2Its size of microcrystal 100nm, specific area is 5～120m
2/ g; The corresponding cerium zirconium precursor compound that the thermal decomposition under 200～1000 ℃ of temperature of its composite oxides contains hydrazine (or hydrazonium salt) makes.This method is made raw material with toxicant hydrazine (or hydrazonium salt), in process of production, can pollute environment, and the influence mankind's is healthy.
Patent CN1369460A discloses a kind of preparation method of Ce-Zr based composite oxide.With nitrate is raw material, with the ammonium hydrogencarbonate is precipitating reagent, through preparations such as chemical reaction, drying, roasting have high-specific surface area and high oxygen storage power based on cerium oxide and zirconic a kind of Ce-Zr based composite oxide, it was 500 ℃ of roastings 2 hours, specific area is 40～50m
2/ g.This method products obtained therefrom specific area is less.
Patent USP6255242 discloses a kind of preparation method of Ce-Zr based composite oxide.Improve oxygen storage capacity by introducing sulfate ion, it is at 3 hours specific area＞10m of 1100 ℃ of roastings
2/ g.This method has been introduced element sulphur, and the catalyst poisoning of using in many reactions is lost activity.
(Journal of Molecular Catalysis, 2000,14: the cerium zirconium sosoloid that 81) makes though operating procedure is simple, is 40.6m through the specific area of 600 ℃ of roastings after 5 hours to improved sol-gel process
2/ g.
Patent CN1387943A discloses a kind of preparation technology based on cerium oxide and zirconic composite oxide solid solution.Mix in proportion after alkali precipitation, filtration, sedimentary heat treatment, oven dry, calcining by rare-earth sol that contains cerium and zirconium colloidal sol and to make.This method operating procedure complexity, the cost height.
Summary of the invention
Technical problem to be solved by this invention provides a kind of based on cerium oxide and zirconic composite oxides and preparation method thereof, further improves specific area, oxygen storage capacity and the heat endurance of particle.
The general structure of Ce-Zr based composite oxide of the present invention is:
Ce
1-x-yZr
xB
yO
2-δ
Wherein: x=0.10～0.75, y=0.00～0.10, δ=0.00～0.30.
In optimized technical scheme of the present invention, comprise the CeO of 10～90% (weight)
2ZrO with 10～90% (weight)
2, 4nm≤size of microcrystal≤80nm;
In optimized technical scheme of the present invention, also comprise other element of 0.01～10% of described Ce-Zr based composite oxide gross weight in the described Ce-Zr based composite oxide, this other element is selected from one or more in the elements such as rare earth element, silicon, aluminium, barium, strontium or calcium.The performance of introducing the nano cerium zirconium based compound oxide of the present invention behind above-mentioned these elements is more excellent.
Described rare earth element comprises that period of element atom ordinal number is 57 to 71 element, yttrium or scandium element.
The preparation method of Ce-Zr based composite oxide of the present invention comprises the steps:
According to stoichiometric proportion, the nitrate of Ce, Zr and metallic element B (wherein B is Ca or Sr or Ba or Mn or Al or Si or the arbitrary rare earth element except that Ce) is water-soluble, make the solution that concentration is 20～50wt% (I); Get the water-soluble solution that concentration is 40～60wt% (II) of making of excessive hydrogen peroxide and ammoniacal liquor; Under vigorous stirring, drip solution (I) and solution (II) in ammonia spirit, control solution (I): solution (II) is that 1: 1～1: 2 (weight ratio) and pH value are 9.5-10.5, static ageing 5～30 hours under the room temperature after stirring 0.5-1 hour again, with the precipitation of hydroxide suction filtration after the static ageing, then after 100～110 ℃ of following dryings of still air, roasting is 2～6 hours in 500～1000 ℃ of scopes, can get Ce-Zr based composite oxide.
Preparation method's of the present invention advantage is: the nitrate of Ce in precipitation process can and hydrogen peroxide react, oxygen gas generation is arranged, stop sedimentary reunion, the solid sample that makes has that crystal grain is little, specific area is big, oxygen storage capacity is high and Heat stability is good.
The nano cerium zirconium based compound oxide that makes with the inventive method is a kind of multicomponent composite oxide of novel solid solution type, has higher specific surface area and heat endurance, through 900 ℃ of following roastings after 6 hours specific area still greater than 30m
2/ g.
Nano cerium zirconium based compound oxide of the present invention has the excellent in chemical activity, higher specific surface area, high storage/put oxygen ability and high high-temp stability, in cleaning catalyst for tail gases of automobiles, catalyst for catalytic combustion and other catalyst, purposes is widely arranged.
Description of drawings
(it consists of Ce to Fig. 1 for the prepared a kind of nanometer cerium zirconium oxide of the inventive method
0.5Zr
0.5O
2) X ray diffracting spectrum.
Fig. 2 is for (it consists of Ce with the prepared a kind of cerium zirconium compound oxide of conventional method
0.5Zr
0.5O
2) temperature programmed reduction (TPR) collection of illustrative plates.
(it consists of Ce to Fig. 3 for the prepared a kind of nanometer cerium zirconium oxide of the inventive method
0.5Zr
0.5O
2) H
2-temperature programmed reduction (TPR) collection of illustrative plates.
The specific embodiment
The present invention is not limited by following examples.
Embodiment 1
Get 24.8gZr (NO
3)
45H
2O, 25.1gCe (NO
3)
36H
2Make solution (I) after O and the 100ml deionized water heating for dissolving, getting 60ml ammoniacal liquor is dissolved in 60ml water and makes solution (II), put some ammoniacal liquor in advance at drag, control pH value is at 9.5-10.5, under vigorous stirring, drip solution (I) and solution (II) simultaneously to flask, generation purple precipitation, at room temperature stirred after 0.5-1 hour static ageing 24 hours, with the precipitation of hydroxide suction filtration after the static ageing, after 110 ℃ of dryings, 550 ℃ of roastings 5 hours, can get single cerium zirconium compound oxide, specific area is 68.6m
2/ g, 900 ℃ of roastings after 6 hours specific area be 21.4m
2/ g.
Embodiment 2
Get 24.8g Zr (NO
3)
45H
2O, 25.1g Ce (NO
3)
36H
2Make solution (I) after O and the 100ml deionized water heating for dissolving, getting 15ml hydrogen peroxide and 60ml ammoniacal liquor is dissolved in 60ml water and makes solution (II), put some ammoniacal liquor in advance at drag, control pH value is at 9.5-10.5, in vigorous stirring and drip down solution (I) and solution (II) simultaneously to flask, generate yellow mercury oxide, at room temperature stirred after 0.5-1 hour static ageing 24 hours, with the precipitation of hydroxide suction filtration after the static ageing, after 110 ℃ of dryings, 550 ℃ of roastings 5 hours, can get single cerium zirconium compound oxide, specific area is 107.4 m
2/ g, 900 ℃ of roastings after 6 hours specific area be 32.2m
2/ g.
Embodiment 3
Get 24.8g Zr (NO
3)
45H
2O, 25.1g Ce (NO
3)
36H
2O, 4.8gLa (NO
3)
3NH
2Make solution (I) after O and the 100ml deionized water heating for dissolving, getting 15ml hydrogen peroxide and 60ml ammoniacal liquor is dissolved in 60ml water and makes solution (II), put some ammoniacal liquor in advance at drag, control pH value is at 9.5-10.5, under vigorous stirring, drip solution (I) and solution (II) simultaneously, generate yellow mercury oxide, at room temperature stirred after 0.5-1 hour static ageing 24 hours, with the precipitation of hydroxide suction filtration after the static ageing, after 110 ℃ of dryings, 550 ℃ of roastings 5 hours, can get cerium zirconium lanthanium complex oxide, specific area is 92.4m
2/ g, 900 ℃ of roastings after 6 hours specific area be 38.2m
2/ g.
Claims (10)
1. a nano cerium zirconium based compound oxide is characterized in that, general structure is:
Ce
1-x-yZr
xB
yO
2-δ
Wherein: x=0.10～0.75, y=0.00～0.10, δ=0.00～0.30;
4nm≤size of microcrystal≤80nm.
2. a nano cerium zirconium based compound oxide is characterized in that, comprises the CeO of 10～90% (weight)
2ZrO with 10～90% (weight)
2, 4nm size of microcrystal 80nm.
3. nano cerium zirconium based compound oxide according to claim 1 and 2, it is characterized in that, also comprise other element of 0.01～10% of described Ce-Zr based composite oxide gross weight, this other element is selected from one or more in the elements such as rare earth element, silicon, aluminium, barium, strontium or calcium.
4. nano cerium zirconium based compound oxide according to claim 3 is characterized in that, described rare earth element comprises that period of element atom ordinal number is 57 to 71 element, yttrium and scandium element.
5. according to the preparation method of each described nano cerium zirconium based compound oxide of claim 1～4, it is characterized in that comprising the steps:
The nitrate of Ce, Zr and metallic element B (wherein B is Ca or Sr or Ba or Mn or Al or Si or the arbitrary rare earth element except that Ce) is water-soluble, make solution (I); Get the water-soluble solution (II) of making of excessive hydrogen peroxide and ammoniacal liquor; Solution (I) and solution (II) are joined in the ammonia spirit, and control pH value is at 9.5-10.5, reacts after 0.5-1 hour static ageing 5～30 hours, and after filtration, after the drying, roasting is 2～6 hours in 500～1000 ℃ of scopes, can get Ce-Zr based composite oxide.
6. the preparation method of nano cerium zirconium based compound oxide according to claim 5 is characterized in that, solution (I): solution (II)=1: 1～1: 2 (weight ratio).
7. the preparation method of nano cerium zirconium based compound oxide according to claim 5, it is characterized in that, according to stoichiometric proportion, that the nitrate of Ce, Zr and one or more metallic elements B (wherein B is Ca or Sr or Ba or Mn or Al or Si or the arbitrary rare earth element except that Ce) is soluble in water.
8. the preparation method of nano cerium zirconium based compound oxide according to claim 5 is characterized in that, the concentration of solution (I) is 20～50wt%.
9. the preparation method of nano cerium zirconium based compound oxide according to claim 5 is characterized in that, gets the water-soluble solution that concentration is 40～60wt% (II) of making of excessive hydrogen peroxide and ammoniacal liquor.
10. the preparation method of nano cerium zirconium based compound oxide according to claim 5 is characterized in that, solution (I) and solution (II) are added ammonia spirit simultaneously, and control pH value is at 9.5-10.5, reacts after 0.5-1 hour static ageing 5～30 hours.
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