CN103127925B - Cerium-zirconium-based solid solution rare earth oxygen-storage material and preparation method thereof - Google Patents
Cerium-zirconium-based solid solution rare earth oxygen-storage material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cerium-zirconium-based solid solution rare earth oxygen-storage material and a preparation method thereof. The cerium-zirconium-based solid solution rare earth oxygen-storage material has a specific surface area equal to or greater than 90m<2>.g<-1>, has a specific surface area equal to or greater than 30m<2>.g<-1> after being calcined at a temperature of 1000 DEG C for 4 hours, and has a specific surface area equal to or greater than 20m<2>.g<-1> after being calcined at a temperature of 1050 DEG C for 12 hours. Compared with the prior art, the preparation method has the advantages that before precipitation, a mixed metal salt solution is added with a certain amount of an organic acid so that acidity of the mixed metal salt solution is improved or the mixed metal salt solution forms sol; a reaction rate is inhibited and a precipitation rate is controlled so that a stable precursor having the uniform grain size is obtained; and the precipitate precursor surface treatment is carried out by a surfactant so that the aperture size and the aperture volume of a calcination product are improved and the cerium-zirconium-based solid solution rare earth oxygen-storage material having good heat stability is prepared. The cerium-zirconium-based solid solution rare earth oxygen-storage material has the advantages of small granule size, large specific surface area, high temperature aging resistance and high activity.
Description
Technical field
The present invention relates to a kind of rare earth oxygen storage material and preparation method thereof, particularly a kind ofly to eliminate for purifying vehicle exhaust, organic exhaust gas and the cerium zirconium based solid solution rare earth oxygen storage material and preparation method thereof of the waste gas purification such as natural gas catalytic combustion or catalytic combustion.
Background technology
Reduce automobile exhaust pollution, environment protection quality, realizing the sustainable development of ecological environment and society, is one of important topic of China environmental protection in the current and following long duration.
In order to decreasing pollution, must break through from improving gasoline quality, improving engine combustion state and increasing exhaust purification catalytic efficiency three aspect.Up to the present, using cleaning catalyst for tail gases of automobiles to be most effective way is exactly reduced the content of HC, CO and NOx tri-kinds of toxic gases in tail gas by three-way catalytic apparatus, and hydrogen-storing material is the important component part in three way catalytic conversion device, it plays the effect regulating atmosphere in tail gas clean-up process, when atmosphere is in lean burn condition, hydrogen-storing material by absorbing unnecessary oxygen, when atmosphere is in fuel-rich state, hydrogen-storing material releases oxygen, and three kinds of gases are effectively transformed.Therefore, the quality of the Oxygen storage capacity of hydrogen-storing material directly affects the transformation efficiency of tail gas.Simultaneously hydrogen-storing material can the dispersion of effective stabilizing active component, therefore there is large specific area, larger pore volume and suitable pore-size distribution, and there is good high-temperature aging resisting performance, the cerium zirconium based oxygen storage material of excellent low-temperature catalyzed performance becomes the critical material of new three-way catalyst.
ZrO
2add CeO to
2in, can CeO be formed
2-ZrO
2solid solution and improve CeO
2body phase behaviour, be beneficial to migration and the diffusion of body phase oxygen atom, make body phase reaction process become active, can CeO be improved
2oxygen storage capacity and high-temperature stability.Meanwhile, the rare earths such as Pr, Nd, Y, Nb, La and Ba and alkaline earth element add the high-temperature aging resisting that can strengthen hydrogen-storing material further, improve its oxygen storage capacity.
The Chinese patent patent No. is that the patent of invention of ZL200510115874.2 discloses a kind of solid solution composition of cerium zirconium compound oxide with high specific surface and preparation method thereof, surfactant or amine salt or inorganic ammonium salt or ethanol is added by being added in the suspension that is settled out, and high temperature crystallization, after crystallization, product washs through ethanol, high-temperature roasting.
But above-mentioned complicated process of preparation, simultaneously by high temperature crystallization, ethanol washs, and is unfavorable for industrial production, and is common liquid-phase precipitation during precipitation, and particle is larger.
China Patent Publication No. is that the patent of invention of CN101637721B discloses a kind of porous yttrium-cerium-zirconium solid solution and preparation method thereof; by adding protective agent, norium salting liquid and active polystyrene microballoon emulsion; normal temperature precipitates; 80-100 DEG C of ageing, collecting precipitation thing, washing, drying, roasting obtain target product.
In above-mentioned preparation method, polystyrene microsphere emulsion cannot mix with metal salt solution, easily causes the stable homogeneous of product.
China Patent Publication No. is that the patent of invention of CN100496745C discloses a kind of wire or rod-like polycrystal Ce
0.6zr
0.3y
0.1o
2solid solution preparation method, by adding softex kw as surfactant, obtain presoma by hydrothermal treatment consists, calcination obtains target product.
Above-mentioned preparation method, by hydrothermal treatment consists, needs high-tension apparatus, is unfavorable for that industrialization is produced.
Therefore, a kind of cerium zirconium based solid solution rare earth oxygen storage material of special needs and preparation method thereof, has solved above-mentioned existing Problems existing.
Summary of the invention
The object of the present invention is to provide a kind of cerium zirconium based solid solution rare earth oxygen storage material and preparation method thereof, overcome prior art and there is above-mentioned problem, the cerium zirconium based solid solution rare earth oxygen storage material of preparation, have that particle is little, specific area be large, high-temperature aging resisting and active high, meet business to production cost and the requirement to environment restriction that day by day increases.
To achieve these goals, technical scheme of the present invention is as follows:
A first aspect of the present invention provides a kind of cerium zirconium based solid solution rare earth oxygen storage material, it is characterized in that, its specific surface>=90m
2g
-1, specific surface>=30m after 1000 DEG C of roasting 4h
2g
-1, specific surface>=20m after 1050 DEG C of roasting 12h
2g
-1.
A second aspect of the present invention provides a kind of preparation method of cerium zirconium based solid solution rare earth oxygen storage material, and it is characterized in that, it comprises the steps:
(1) preparation of hybrid metal nitrate solution: form and the weight of target product according to material component, determine the content of cerium oxide, zirconia and other rare earth oxides except cerium, be converted into the weight content of corresponding raw material, by water-soluble to cerous nitrate, other rare earth soluble nitrate except cerium and zirconium nitrate, add certain organic acid, obtain hybrid metal nitrate solution;
(2) preparation of cerium zirconium based solid solution rare earth oxygen storage material presoma: the industrial ammonia with 36% and the mixed precipitating reagent of pure water 1: 1, slowly join in the hybrid metal nitrate solution of 50-70 DEG C, be 3-4, add Ce to pH
3+/ Ce
4+transform the stoichiometry 1.2-1.5 hydrogen peroxide doubly needed, continuing to add precipitating reagent to pH is 9, insulation 2-5h, and washing, dehydration, obtain cerium zirconium based solid solution rare earth oxygen storage material presoma;
(3) surface treatment of cerium zirconium based solid solution rare earth oxygen storage material presoma: cerium zirconium based solid solution rare earth oxygen storage material presoma and certain surfactant are sheared and disperses;
(4) roasting: by surface treated cerium zirconium based solid solution rare earth oxygen storage material presoma roasting 4-8h at 450-800 DEG C, obtain described cerium zirconium based solid solution rare earth oxygen storage material.
In one embodiment of the invention, described other rare earth soluble nitrate except cerium are selected from the combination of one or more in lanthanum nitrate, yttrium nitrate, praseodymium nitrate or neodymium nitrate.
In one embodiment of the invention, described other rare earth soluble nitrate except cerium are selected from nitric acid and react to lanthana, yittrium oxide, praseodymium oxide or neodymia and generate corresponding nitrate solution.
In one embodiment of the invention, in described hybrid metal nitrate solution, the ratio of each nitrate is:
Cerous nitrate 20-70%
Zirconium nitrate 20-70%
Other rare earth soluble nitrate 5-15% except cerium.
In one embodiment of the invention, described organic acid is one or more combination in acetic acid, formic acid or citric acid, and described organic acid addition accounts for the 5-20% of nitrate weight in mixed salt solution by weight.
In one embodiment of the invention, described surface conditioning agent to be selected from laurate, stearic acid or alkenyl succinic anhydride one or more combination, and the addition of described surface conditioning agent counts 30-50% with the weight of described cerium zirconium based solid solution rare earth oxygen storage material.
Cerium zirconium based solid solution rare earth oxygen storage material of the present invention and preparation method thereof, compared with existing product, certain organic acid is added in mixed salt solution before precipitation, improve the acidity of mixed salt solution or form colloidal sol, suppress the speed of reaction, control settling velocity, to obtaining uniform particle diameter, stable presoma; And carry out surface treatment by surfactant at sediment presoma, improve the aperture of product of roasting, pore volume, obtain the cerium zirconium based solid solution rare earth oxygen storage material of good thermal stability, it is little that the cerium zirconium based solid solution rare earth oxygen storage material prepared has particle, specific area is large, high temperature ageing resistance and active advantages of higher, realizes object of the present invention.
The detailed description and obtaining that feature of the present invention can consult the graphic and following better embodiment of this case is well understood to.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the XRD contrast of the cerium zirconium based solid solution rare earth oxygen storage material of embodiments of the invention 1.
Detailed description of the invention
The technological means realized to make the present invention, creation characteristic, reaching object and effect is easy to understand, setting forth the present invention further below in conjunction with specific embodiment.
Cerium zirconium based solid solution rare earth oxygen storage material of the present invention, its specific surface>=90m
2g
-1, specific surface>=30m after 1000 DEG C of roasting 4h
2g
-1, specific surface>=20m after 1050 DEG C of roasting 12h
2g
-1.
The preparation method of cerium zirconium based solid solution rare earth oxygen storage material of the present invention, it comprises the steps:
(1) preparation of hybrid metal nitrate solution: form and the weight of target product according to material component, determine the content of cerium oxide, zirconia and other rare earth oxides except cerium, be converted into the weight content of corresponding raw material, by water-soluble to cerous nitrate, other rare earth soluble nitrate except cerium and zirconium nitrate, add certain organic acid, obtain hybrid metal nitrate solution;
(2) preparation of cerium zirconium based solid solution rare earth oxygen storage material presoma: the industrial ammonia with 36% and the mixed precipitating reagent of pure water 1: 1, slowly join in the hybrid metal nitrate solution of 50-70 DEG C, be 3-4, add Ce to pH
3+/ Ce
4+transform the stoichiometry 1.2-1.5 hydrogen peroxide doubly needed, continuing to add precipitating reagent to pH is 9, insulation 2-5h, and washing, dehydration, obtain cerium zirconium based solid solution rare earth oxygen storage material presoma;
(3) surface treatment of cerium zirconium based solid solution rare earth oxygen storage material presoma: cerium zirconium based solid solution rare earth oxygen storage material presoma and certain surfactant are sheared and disperses;
(4) roasting: by surface treated cerium zirconium based solid solution rare earth oxygen storage material presoma roasting 4-8h at 450-800 DEG C, obtain described cerium zirconium based solid solution rare earth oxygen storage material.
In above-mentioned steps (1), described other rare earth soluble nitrate except cerium are selected from the combination of one or more in lanthanum nitrate, yttrium nitrate, praseodymium nitrate or neodymium nitrate; Described other rare earth soluble nitrate except cerium are selected from nitric acid and react to lanthana, yittrium oxide, praseodymium oxide or neodymia and generate corresponding nitrate solution.
In described hybrid metal nitrate solution, the ratio of each nitrate is:
Cerous nitrate 20-70%
Zirconium nitrate 20-70%
Other rare earth soluble nitrate 5-15% except cerium.
Described organic acid is one or more combination in acetic acid, formic acid or citric acid, and described organic acid addition accounts for the 5-20% of nitrate weight in mixed salt solution by weight.
In above-mentioned steps (3), described surface conditioning agent to be selected from laurate, stearic acid or alkenyl succinic anhydride one or more combination, and the addition of described surface conditioning agent counts 30-50% with the weight of described cerium zirconium based solid solution rare earth oxygen storage material.
Embodiment 1
70g cerous nitrate, 20g zirconium nitrate, 5g lanthanum nitrate, 5g yttrium nitrate is dissolved in 1900g deionized water, adds 5g acetic acid, is heated to 50 DEG C, obtains hybrid metal nitrate solution; Mixed with mass ratio 1: 1 with pure water by industrial ammonia, obtain precipitating reagent, precipitating reagent slowly being added to obtain hybrid metal nitrate solution, is 3 to pH value, and after adding 11.6g hydrogen peroxide, continuing to add precipitating reagent to pH value is 9, insulation 5h; Washing, dehydration; Mixed with 11g laurate by cerium zirconium based solid solution rare earth oxygen storage material presoma after dehydration, shear dispersion, roasting 4h at 600 DEG C, obtains described cerium zirconium based solid solution rare earth oxygen storage material.
The specific surface of described cerium zirconium based solid solution rare earth oxygen storage material is 100.55m
2g
-1, particle size is that 90nm, XRD schematic diagram is see Fig. 1.Getting cerium zirconium based solid solution rare earth oxygen storage material specific surface after 1000 DEG C of roasting 4h is 45.32m
2g
-1, after 1050 DEG C of roasting 12h, specific surface is 25.32m
2g
-1.
Embodiment 2
21g cerous nitrate, 133g zirconium nitrate, 5.5g neodymium nitrate, 1.5g yttrium nitrate is dissolved in 1900g deionized water, adds 32g citric acid, is heated to 70 DEG C, obtains hybrid metal nitrate solution; Mixed with mass ratio 1: 1 with pure water by industrial ammonia, obtain precipitating reagent, precipitating reagent slowly being added to obtain hybrid metal nitrate solution, is 3 to pH value, and after adding 4.4g hydrogen peroxide, continuing to add precipitating reagent to pH value is 9, insulation 2h; Washing, dehydration; By the cerium zirconium based solid solution rare earth oxygen storage material presoma after dehydration and 30g alkenyl succinic anhydride, shear dispersion, roasting 8h at 450 DEG C, obtains described cerium zirconium based solid solution rare earth oxygen storage material.
The specific surface of described cerium zirconium based solid solution rare earth oxygen storage material is 120.18m
2g
-1, getting cerium zirconium based solid solution rare earth oxygen storage material specific surface after 1000 DEG C of roasting 4h is 35.86m
2g
-1, after 1050 DEG C of roasting 12h, specific surface is 27.38m
2g
-1.
Embodiment 3
By 5g lanthana, 5g yittrium oxide nitric acid dissolve, adds 100g cerous nitrate after obtaining clear transparent solutions, and 72g zirconium nitrate adds deionized water to 2000g, adds 20g formic acid, is heated to 70 DEG C; Obtain hybrid metal nitrate solution; Mixed with mass ratio 1: 1 with pure water by industrial ammonia, obtain precipitating reagent, precipitating reagent slowly being added to obtain hybrid metal nitrate solution, is 3 to pH value, and after adding 20g hydrogen peroxide, continuing to add precipitating reagent to pH value is 9, insulation 4h; Washing, dehydration; By the cerium zirconium based solid solution rare earth oxygen storage material presoma after dehydration and 30g stearic acid, shear dispersion, roasting 4h at 800 DEG C, obtains described cerium zirconium based solid solution rare earth oxygen storage material.
The specific surface of described cerium zirconium based solid solution rare earth oxygen storage material is 100.02m
2g
-1, getting cerium zirconium based solid solution rare earth oxygen storage material specific surface after 1000 DEG C of roasting 4h is 31.28m
2g
-1, after 1050 DEG C of roasting 12h, specific surface is 23.12m
2g
-1.
Embodiment 4
By 7g praseodymium oxide, 7g neodymia nitric acid dissolve, adds 76g cerous nitrate after obtaining clear transparent solutions, and 145g zirconium nitrate adds deionized water to 2000g, adds 20g formic acid, is heated to 70 DEG C; Obtain hybrid metal nitrate solution; Mixed with mass ratio 1: 1 with pure water by industrial ammonia, obtain precipitating reagent, precipitating reagent slowly being added to obtain hybrid metal nitrate solution, is 4 to pH value, and after adding 20g hydrogen peroxide, continuing to add precipitating reagent to pH value is 9, insulation 4h; Washing, dehydration; By the cerium zirconium based solid solution rare earth oxygen storage material presoma after dehydration and 30g laurate, shear dispersion, roasting 5h at 600 DEG C, obtains described cerium zirconium based solid solution rare earth oxygen storage material.
The specific surface of described cerium zirconium based solid solution rare earth oxygen storage material is 120.02m
2g
-1, getting cerium zirconium based solid solution rare earth oxygen storage material specific surface after 1000 DEG C of roasting 4h is 32.28m
2g
-1, after 1050 DEG C of roasting 12h, specific surface is 24.12m
2g
-1.
More than show and describe general principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; the just principle of the present invention described in above-described embodiment and description; the present invention also has various changes and modifications without departing from the spirit and scope of the present invention, and these changes and improvements all fall in claimed scope of the present invention.The protection domain of application claims is defined by appending claims and equivalent thereof.
Claims (6)
1. a cerium zirconium based solid solution rare earth oxygen storage material, is characterized in that, its specific surface>=90m
2g
-1, specific surface>=30m after 1000 DEG C of roasting 4h
2g
-1, specific surface>=20m after 1050 DEG C of roasting 12h
2g
-1;
Its preparation method, comprises the steps:
(1) preparation of hybrid metal nitrate solution: form and the weight of target product according to material component, determine the content of cerium oxide, zirconia and other rare earth oxides except cerium, be converted into the weight content of corresponding raw material, by water-soluble to cerous nitrate, other rare earth soluble nitrate except cerium and zirconium nitrate, add certain organic acid, obtain hybrid metal nitrate solution;
(2) preparation of cerium zirconium based solid solution rare earth oxygen storage material presoma: the industrial ammonia with 36% and the mixed precipitating reagent of pure water 1:1, slowly join in the hybrid metal nitrate solution of 50-70 DEG C, be 3-4, add Ce to pH
3+/ Ce
4+transform the stoichiometry 1.2-1.5 hydrogen peroxide doubly needed, continuing to add precipitating reagent to pH is 9, insulation 2-5h, and washing, dehydration, obtain cerium zirconium based solid solution rare earth oxygen storage material presoma;
(3) surface treatment of cerium zirconium based solid solution rare earth oxygen storage material presoma: cerium zirconium based solid solution rare earth oxygen storage material presoma and certain surfactant are sheared and disperses;
(4) roasting: by surface treated cerium zirconium based solid solution rare earth oxygen storage material presoma roasting 4-8h at 450-800 DEG C, obtain described cerium zirconium based solid solution rare earth oxygen storage material.
2. cerium zirconium based solid solution rare earth oxygen storage material according to claim 1, is characterized in that, described other rare earth soluble nitrate except cerium are selected from the combination of one or more in lanthanum nitrate, yttrium nitrate, praseodymium nitrate or neodymium nitrate.
3. cerium zirconium based solid solution rare earth oxygen storage material according to claim 1, is characterized in that, described other rare earth soluble nitrate except cerium are selected from nitric acid and react to lanthana, yittrium oxide, praseodymium oxide or neodymia and generate corresponding nitrate solution.
4. cerium zirconium based solid solution rare earth oxygen storage material according to claim 1, is characterized in that, in described hybrid metal nitrate solution, the ratio of each nitrate is:
Cerous nitrate 20-70%
Zirconium nitrate 20-70%
Other rare earth soluble nitrate 5-15% except cerium.
5. cerium zirconium based solid solution rare earth oxygen storage material according to claim 1, it is characterized in that, described organic acid is one or more combination in acetic acid, formic acid or citric acid, and described organic acid addition accounts for the 5-20% of nitrate weight in mixed salt solution by weight.
6. cerium zirconium based solid solution rare earth oxygen storage material according to claim 1, it is characterized in that, described surface conditioning agent to be selected from laurate, stearic acid or alkenyl succinic anhydride one or more combination, and the addition of described surface conditioning agent counts 30-50% with the weight of described cerium zirconium based solid solution rare earth oxygen storage material.
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| CN104437458B (en) * | 2014-11-12 | 2017-05-17 | 诺轩化学科技（上海）有限公司 | Cerium-zirconium-based composite oxide catalytic material and preparation method thereof |
| CN104492415B (en) * | 2014-12-02 | 2017-05-17 | 上海华明高纳稀土新材料有限公司 | Preparation method of cerium-zirconium based solid solution catalytic material |
| CN104492414B (en) * | 2014-12-02 | 2017-01-25 | 上海华明高纳稀土新材料有限公司 | Preparation method of cerium-zirconium based solid solution |
| CN104525180B (en) * | 2014-12-30 | 2017-02-22 | 长沙矿冶研究院有限责任公司 | Preparation method for cerium-zirconium-aluminum-lanthanum-based oxygen storage material of mesoporous structure |
| CN105080530A (en) * | 2015-05-26 | 2015-11-25 | 华东理工大学 | Preparation method for cerium-zirconium composite oxide with high performance |
| CN105013457B (en) * | 2015-06-19 | 2018-04-17 | 云南中烟工业有限责任公司 | A kind of high oxygen storage capacity cerium zirconium sosoloid prepared using tobacco plant as template and preparation method thereof |
| EP3398678A1 (en) * | 2017-05-05 | 2018-11-07 | SASOL Germany GmbH | Nox trap catalyst support material composition |
| CN110026174B (en) * | 2018-12-12 | 2020-09-08 | 四川大学 | High thermal stability CeO2-ZrO2Oxygen-storing material and its preparation |
| CN110560033B (en) | 2019-08-09 | 2020-10-23 | 山东国瓷功能材料股份有限公司 | Stable cerium-zirconium solid solution and preparation method and application thereof |
| CN115403393B (en) * | 2022-08-25 | 2023-05-16 | 宜兴瑞泰耐火材料有限公司 | Zirconium mullite brick for high-salt incinerator and preparation method thereof |
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| US7964527B2 (en) * | 2006-02-17 | 2011-06-21 | Rhodia Operations | Catalytic compositions comprising the oxides of zirconium, cerium, yttrium, lanthanum and other rare earths |
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| CN1241988A (en) * | 1996-12-27 | 2000-01-19 | 阿南化成株式会社 | Composite zirconium-cerium oxide, process for the preparation thereof, and cocatalyst for cleaning exhaust gas |
| CN1403376A (en) * | 2002-10-15 | 2003-03-19 | 清华大学 | Cerium-base quaternary nano level composite RE oxide and its prepn process |
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Denomination of invention: Cerium zirconium based Solid solution rare earth oxygen storage material and its preparation method Effective date of registration: 20230627 Granted publication date: 20150325 Pledgee: Industrial Bank Co.,Ltd. Shanghai Songjiang sub branch Pledgor: SHANGHAI HUAMING GONA RARE EARTH NEW MATERIALS Co.,Ltd. Registration number: Y2023310000314 |
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