CN104492414B - Preparation method of cerium-zirconium based solid solution - Google Patents
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Abstract
The invention discloses a preparation method of a cerium-zirconium based solid solution. The preparation method comprises the following sequential steps: (1) preparation of Ce<4+>; (2) preparation of active ingredient solution; (3) precipitation reaction; (4) surface modification; (5) roasting. The Ce<4+> is prepared firstly and then mixed with other rare earth ions and positively quadrivalent zirconium ions to obtain a mixed metal nitrate solution; as the mixed metal nitrate solution contains an organic complexing agent, the precipitation speed in the precipitation reaction process is controlled by virtue of complexing coordination of the organic complexing agent and the rare earth and zirconium ions, so that a precursor uniform and stable in particle size is obtained; the surface treatment is performed on the precipitate precursor by use of polyacrylic acid, and therefore, the agglomeration problem of particles in the roasting process is solved, and the pore diameter and the pore volume of the roasted product are increased, and consequently, the cerium-zirconium based solid solution catalytic material excellent in heat stability is obtained. The preparation method is suitable for the preparation of the solid solutions.
Description
Technical field
The invention belongs to catalyst field, it is related to a kind of preparation method of motor vehicle vent gas purification catalysis material, specifically relates to
And a kind of preparation method of cerium zirconium based solid solution.
Background technology
Reduce automobile exhaust pollution, environment protection quality, realize ecological environment and the sustainable development of society, be mesh
One of important topic of China environmental protection in front and following long duration.
In order to reduce pollution it is necessary to from raising gasoline quality, improving engine combustion state and increase exhaust purification catalytic
Efficiency three aspect is broken through.Up to the present, using cleaning catalyst for tail gases of automobiles be most effective approach be exactly pass through ternary
Catalytic unit is reducing the content of tri- kinds of toxic gas of hc, co and nox in tail gas, and cerium zirconium based solid solution catalysis material is ternary
Important component part in catalytic convention design, it plays the effect adjusting atmosphere during tail gas clean-up, when atmosphere is in
During lean burn condition, cerium zirconium based solid solution catalysis material will absorb unnecessary oxygen, and when atmosphere is in fuel-rich state, cerium zirconium base is solid
Solution catalysis material releases oxygen, so that three kinds of gases is effectively converted.Therefore, the storage oxygen of cerium zirconium based solid solution catalysis material
The quality of performance directly affects the transformation efficiency of tail gas.Cerium zirconium based solid solution catalysis material can effective stabilizing active component simultaneously
Dispersion, therefore has big specific surface area, larger pore volume and suitable pore-size distribution, and has good high-temperature aging resisting
Performance, the cerium zirconium based oxygen storage material of excellent low-temperature catalyzed performance become the critical material of new three-way catalyst.
Due to simple ceo2Being susceptible to sintering, particle growth at high temperature, leading to specific surface area to reduce, thus reducing
Until losing oxygen storage capacity.1987, m.ozawa et al. began through interpolation zirconium oxide to improve ceo2Heat stability.With
Pure ceo2Compare, high-performance rare-earth hydrogen-storing material technology of preparing has become the core skill of Advanced Automotive Exhaust Catalyst
Art and source technology, do not have high-performance rare-earth hydrogen-storing material, will prepare the purifying vehicle exhaust catalysis with the market competitiveness
Agent is impossible.
By zro2It is added to ceo2In, ceo can be formed2-zro2Solid solution and improve ceo2Body phase characteristic, beneficial to body phase oxygen
The migration of atom and diffusion, make body phase course of reaction become active, it is possible to increase ceo2Oxygen storage capacity and high-temperature stability.With
When, the addition of the rare earth such as pr, nd, y, nb, la and ba and alkaline earth element can further enhance cerium zirconium based solid solution catalysis material
High-temperature aging resisting, improves its oxygen storage capacity.
China Patent No. is that the patent of invention of zl200510115874.2 discloses a kind of high-ratio surface cerium-zirconium composite oxide
Thing solid solution composition and preparation method thereof, adds surfactant or amine salt or nothing by being added in the suspension being settled out
Machine ammonium salt or ethanol, and high temperature crystallization, after crystallization, product is through washing with alcohol, high-temperature roasting.But, above-mentioned complicated process of preparation,
It is common liquid-phase precipitation when passing through high temperature crystallization, washing with alcohol simultaneously, be unfavorable for commercial production, and precipitating, particle is larger.
China Patent Publication No. be cn101637721b patent of invention disclose a kind of porous yttrium-cerium-zirconium solid solution and its
Preparation method, by adding protective agent, norium saline solution and active polystyrene microsphere emulsion, room temperature precipitates, 80-
100 DEG C of ageings, collection precipitate, washing, drying, roasting obtain target product.But in above-mentioned preparation method, polystyrene microsphere
Emulsion cannot be mixed homogeneously with metal salt solution, is easily reduced 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
ce0.6zr0.3y0.1o2Solid solution preparation, is used as surface activity by adding cetyl trimethylammonium bromide.United States Patent (USP)
Number it is the patent of invention of us 5,747,401 and patent of invention that U.S. patents number are us 5,723,101 discloses employing
Hydrothermal decomposition method or coprecipitation obtain mixed sediment altogether, are then washed with alkyl oxide solution or impregnate, obtain
Solid solution has high-ratio surface, uniform particle distribution and high oxygen storage power.Cerium solution used (can be by electrolytic oxidation, nitre for tetravalence
Sour cerium ammonium or dissolving carbonate add hydrogen peroxide and obtain), ce+4Concentration is more than 85%, and 900 DEG C, 6 hours, specific surface area was 51.7m2/
g.But, above-mentioned preparation method passes through hydrothermal treatment consists, needs high pressure equipment, is unfavorable for industrialization production.
It is accordingly required in particular to a kind of cerium zirconium based solid solution and preparation method thereof, to solve above-mentioned existing problem.
Content of the invention
The technical problem to be solved in the present invention, is to provide a kind of preparation method of cerium zirconium based solid solution, prepared cerium
The features such as zirconio solid solution has that specific surface area is big, high temperature ageing resistance is good, to store oxygen ability high.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
A kind of preparation method of cerium zirconium based solid solution, it is sequentially carried out in accordance with the following steps:
(1)ce4+Preparation: by cerous nitrate dissolving and water, be heated to 70～80 DEG C, under agitation, use mass concentration
Ammonia precipitation process for 10～15% is 5～6 to ph, adds the dioxygen of the mass concentration 30% of 0.6～0.7 times of cerous nitrate quality
Water, then proceeding to ammonia precipitation process to ph is 8.5～9.0, boils insulation 1.5～2.0h；After filter press, obtain total amount of rare earth
Cerium hydroxide wet cake for 25～30%；Cerium hydroxide wet cake and pure water are pulled an oar according to the ratio of mass ratio 1:5, is adjusted with nitric acid
Section ph is 1.5～2.5, after standing 3～5h, vacuum filtration, and obtain ce4+Settled solution a；
(2) preparation of active component solution: in ce4+Settled solution a in, add except cerium other rare earth oxides
Nitrate, zirconyl nitrate, add organic complexing agent, obtain active component solution b；
(3) precipitation: active component solution b is heated to 70～80 DEG C, under agitation, is slowly added to quality dense
Spend the ammonia for 10～15%, be 8.5～9 to precipitation terminal ph, be incubated 2～4h；After standing 12h, extract the supernatant, must consolidate
Liquid mixed serum c；
(4) surface modification: in solid-liquid mixed serum c add molecular weight be 4000～7000 polyacrylic acid, stirring 1～
2h, obtains the material d of surface modification；
(5) roasting: roasting 4～6h, the finally prepared cerium zirconium base solid solution at 700～750 DEG C by the material d of surface modification
Body.
As one kind restriction of the present invention, in described step (1) cerous nitrate quality account for cerous nitrate and water gross mass 25～
35%.
As the another kind restriction of the present invention, in described step (2), described other rare earth oxides of except cerium
Nitrate, is two or three of lanthana, yittrium oxide, praseodymium oxide and the corresponding nitrate of Dineodymium trioxide.
As the restriction further of above-mentioned restriction, other rare earth oxides of described except cerium in mass, addition
For cerous nitrate consumption 0.3～0.32 times.
As the third restriction of the present invention, in described step (2), the addition of described zirconyl nitrate, in mass,
For cerous nitrate consumption 1.17～1.53 times.
As the 4th kind of restriction of the present invention, in described step (2), described organic complexing agent is hydroxycarboxylic acid chemical combination
Thing.
As the restriction further of above-mentioned restriction, described hydroxy carboxylic acids are alpha-hydroxybutyric dehydrogenase, lactic acid, α-
One of hydroxacetic acid or two kinds.
As the further restriction of above-mentioned restriction, the addition of described hydroxy carboxylic acids, in mass, it is nitre
The 10～20% of sour cerium consumption.
As the 5th kind of present invention restriction, in described step (4), described polyacrylic acid, in mass, addition is
The 1～2% of cerous nitrate consumption.
The present invention also have a kind of limit, obtained cerium zirconium based solid solution is by cerium oxide, zirconium oxide and in addition to cerium zirconium
The composite oxides composition of other rare earth oxide compositions, its percentage by weight is as follows: cerium oxide: 40～50%, and remove cerium zirconium
Other rare earth oxides in addition: 12～13%, remaining is zirconium oxide.
Preparation method due to existing cerium zirconium based solid solution has many kinds, mainly liquid phase method, including coprecipitation, molten
Sol-gel, masterplate method, microemulsion method etc..And coprecipitation is as conventional preparation method, it is that precipitant is added to metal
Saline solution in, the component of solubility is converted into slightly solubility component, obtains target through steps such as filtration, washing, drying, roastings
Compound, but roasting can lead to the decline of specific surface area at high temperature, in addition can relate to during precipitation, drying, roasting etc.
And grow up to aggregation of particles, the reasonable selection of aperture pore volume etc..Technology in therefore involved in present invention preparation method
The index of the product cerium zirconium based solid solution for final preparation for the parameter has significant impact.In addition, in preparation process feed liquid
Concentration, the temperature of chemical reaction, the control of the concentration of precipitant, the screening of various additives and addition etc. are all material systems
Standby key factor, this is related to sedimentary granularity, uniformity, dispersibility, settleability etc., also relates to the poly- of target product
Collection property, pattern, solid solubility, aperture pore volume etc..
Due to employing above-mentioned technical scheme, compared with prior art, acquired technological progress is the present invention:
(1) first prepare ce4+, then mix with the zirconium ion of other rare earth ions and+4 valencys, obtain hybrid metal nitrate
Solution, the present invention contains organic complexing agent by hybrid metal nitrate solution, by organic complexing agent and rare earth and zirconium ion
Complex coordination, control precipitation during settling velocity, obtained uniform particle diameter, stable presoma.
(2) selected from the high rare earth ion of the hydroxy carboxylic acid strong with rare-earth ion coordination and valence state and zirconium ion, on the one hand, make
For the rare earth ion of hard acid class, charge number is bigger, and electrostatic attraction is big, and coordination ability is strong, increased rare earth ion and complex
Complexing power, improves the stability of complex；On the other hand, promote rare earth ion and zirconium ion solid solution ability, really
Protect the solid solution phase that target product has had, even if still there is no split-phase under 1000 DEG C of high temperature ageing.
(3) it is surface-treated in precipitate presoma by polyacrylic acid, on the one hand, solve granule in roasting process
Agglomeration traits；On the other hand, by the roasting of Organic substance, improve aperture, the pore volume of product of roasting, obtain good thermal stability
Cerium zirconium based solid solution catalysis material.
(4) selected by hybrid metal feed liquid and the selection of concentration, precipitant and concentration, the screening of additive and addition
Control, the suitable selection of the condition of association reaction, roasting condition etc. and control, it is little to have obtained having granule, specific surface area is big,
High temperature ageing resistance and active high the advantages of cerium zirconium based solid solution catalysis material.
The present invention is applied to the preparation of cerium zirconium based solid solution, is particularly suited for Vehicle Exhaust Gas Cleaning Catalysts, organic waste
Gas eliminates carriers for catalysts and auxiliary agent with the waste gas purifications such as natural gas catalytic combustion or catalysis burning.
The present invention is described in further detail with specific embodiment below in conjunction with Figure of description.
Brief description
Fig. 1 is the xrd schematic diagram that embodiments of the invention 1 prepare cerium zirconium based solid solution.
Fig. 2 is the xrd schematic diagram that embodiments of the invention 1 prepare 1000 DEG C of roasting 4h of cerium zirconium based solid solution.
Fig. 3 is the xrd schematic diagram of comparative example 1 preparation 1000 DEG C of roasting 4h of cerium zirconium based solid solution of the present invention.
Specific embodiment
A kind of preparation method of cerium zirconium based solid solution of embodiment 1
A kind of preparation method of cerium zirconium based solid solution, it is sequentially carried out in accordance with the following steps:
(1)ce4+Preparation: by 105kg cerous nitrate dissolving mix with 315kg water, be heated to 70 DEG C, under agitation,
The ammonia precipitation process being 10% with mass concentration is 5 to ph, adds the hydrogen peroxide of 63kg mass concentration 30%, then proceedes to use ammonia
Being precipitated to ph is 9.0, boils insulation 2.0h；After filter press, obtain cerium hydroxide wet cake 160kg (total amount of rare earth is 25%)；
160kg cerium hydroxide wet cake is pulled an oar with 800kg pure water, adjusting ph with nitric acid is 1.5, after standing 3h, vacuum filtration, obtain ce+4
Settled solution a；
(2) preparation of active component solution: in ce4+Settled solution a in add 15.7kg Lanthanum (III) nitrate, 15.7kg nitric acid
Yttrium, 240kg zirconyl nitrate, 10.5kg alpha-hydroxybutyric dehydrogenase, obtain active component solution b；
(3) precipitation: active component solution b is heated to 70 DEG C, under agitation, being slowly added to mass concentration is
10% ammonia, is 8.5 to precipitation terminal, is incubated 2h；After standing 12h, extract the supernatant, obtain solid-liquid mixed serum c；
(4) surface modification: add the polyacrylic acid that 1.05kg molecular weight is 4000 in solid-liquid mixed serum c, stir 1h,
Obtain the material d of surface modification；
(5) roasting: by the material d of surface modification in 700 times roasting 6h, obtain described dilute cerium zirconium based solid solution.Cerium zirconium base
Solid solution consist of cerium oxide 40%, zirconium oxide 48%, 6% lanthana, 6% yittrium oxide.
The specific surface area of the cerium zirconium based solid solution obtaining is 92.5m2/ g, through xrd analysis, is shown in Fig. 1；This catalysis material exists
Specific surface area after 1000 DEG C of roasting 4h is 56.2m2/ g, through xrd analysis, is shown in Fig. 2；Specific surface area after 1050 DEG C of roasting 12h
For 34.5m2/g.
The preparation method of embodiment 2-6 cerium zirconium based solid solution
Embodiment 2-6 is respectively a kind of preparation method of cerium zirconium based solid solution, and its method is similar to Example 1, difference
Place is only that wherein involved technical parameter is different, shown in table specific as follows:
Comparative example 1
By 105kg cerous nitrate, 15.7kg Lanthanum (III) nitrate, 15.7kg Yttrium trinitrate, 240kg zirconyl nitrate, it is added to 1831kg's
In pure water, dissolving clarification, after obtaining the solution of clear, it is heated to 70 DEG C of solution a obtaining clear；Under agitation,
It is slowly added to 10% ammonia toward in solution a, be 9.0 to ph.Then under agitation, after insulation 2h, after standing 12h, take out
Take the supernatant, obtain solid-liquid mixed serum, then proceed in saggar, in 700 times roasting 6h, obtain described cerium zirconium based solid solution.
Cerium zirconium based solid solution consist of cerium oxide 40%, zirconium oxide 48%, 6% lanthana, 6% yittrium oxide.
The specific surface area of the cerium zirconium based solid solution obtaining is 80.5m2/ g, ratio after 1000 DEG C of roasting 4h for this catalysis material
Surface area is 21.2m2/ g, the specific surface area after 1050 DEG C of roasting 12h is 8.5m2/g.Through xrd analysis, see Fig. 3,1000 DEG C of roastings
Under after 4h, product, compared with embodiment 1 (Fig. 2), occurs in that obvious split-phase, and specific surface area all has substantially compared with embodiment 1-6
Fall.
Comparative example 2
By 105kg cerous nitrate, 15.7kg Lanthanum (III) nitrate, 15.7kg Yttrium trinitrate, 240kg zirconyl nitrate, it is added to 1831kg's
In pure water, dissolving clarification, after obtaining the solution of clear, it is heated to 70 DEG C of solution a obtaining clear；Under agitation,
It is slowly added to 10% ammonia toward in solution a, be 9.0 to ph.Then under agitation, after insulation 2h, after standing 12h, take out
Take the supernatant, obtain solid-liquid mixed serum.Add the polyacrylic acid that 1.05kg molecular weight is 4000, stirring in solid-liquid mixed serum
1h, proceeds in saggar, in 700 times roasting 6h, obtains described cerium zirconium based solid solution.Cerium zirconium based solid solution consist of cerium oxide
40%, zirconium oxide 48%, 6% lanthana, 6% yittrium oxide.
The specific surface area of the cerium zirconium based solid solution obtaining is 80.5m2/ g, ratio after 1000 DEG C of roasting 4h for this catalysis material
Surface area is 28.2m2/ g, the specific surface area after 1050 DEG C of roasting 12h is 13.5m2/g.The cerium zirconium base being worth compared with embodiment 1-6
The specific surface area in 1000 DEG C and 1050 DEG C of solid solution has all declined.
Comparative example 3
The dissolving of 105kg cerous nitrate is mixed with 315kg water, is heated to 70 DEG C, under agitation, with mass concentration is
10% ammonia precipitation process is 5 to ph, adds the hydrogen peroxide of 63kg mass concentration 30%, and then proceeding to ammonia precipitation process to ph is 9,
Boil insulation 2h；After filter press, obtain cerium hydroxide wet cake 160kg (total amount of rare earth is 25%)；Will be wet for 160kg cerium hydroxide
Cake is pulled an oar with 800kg pure water, and adjusting ph with nitric acid is 1.5, after standing 3h, vacuum filtration, and obtain settled solution a；
In settled solution a, add 15.7kg Lanthanum (III) nitrate, 15.7kg Yttrium trinitrate, 240kg zirconyl nitrate, obtain active component
Solution b；
Active component solution b is heated to 70 DEG C, under agitation, is slowly added to the ammonia that mass concentration is 10%,
It is 8.5 to precipitation terminal, be incubated 2h；After standing 12h, extract the supernatant, obtain solid-liquid mixed serum c.
Add the polyacrylic acid that 1.05kg molecular weight is 4000 in solid-liquid mixed serum c, stir 1h, proceed in saggar,
In 700 times roasting 6h, obtain described cerium zirconium based solid solution.Cerium zirconium based solid solution consist of cerium oxide 40%, zirconium oxide 48%,
6% lanthana, 6% yittrium oxide.
The specific surface area of the cerium zirconium based solid solution obtaining is 92.5m2/ g, ratio after 1000 DEG C of roasting 4h for this catalysis material
Surface area is 26.2m2/ g, the specific surface area after 1050 DEG C of roasting 12h is 14.5m2/ g, the cerium zirconium base being worth compared with embodiment 1-6
The specific surface area in 1000 DEG C and 1050 DEG C of solid solution has all declined.
The above, be only presently preferred embodiments of the present invention, is not the restriction that the present invention is made with other forms, appoints
What those skilled in the art is changed as enlightenment possibly also with above-mentioned technology contents or is modified as equivalent variations
Equivalent embodiments.But every without departing from technical solution of the present invention content, according to the present invention technical spirit to above example
Done simple modification, equivalent variations and remodeling, still falls within the protection domain of the claims in the present invention.
Claims (6)
1. a kind of preparation method of cerium zirconium based solid solution is it is characterised in that it is sequentially carried out in accordance with the following steps:
(1)ce4+Preparation: cerous nitrate is dissolved in water, is heated to 70～80 DEG C, under agitation, with mass concentration be 10
～15% ammonia precipitation process is 5～6 to ph, adds the hydrogen peroxide of the mass concentration 30% of 0.6～0.7 times of cerous nitrate quality, so
Continuation ammonia precipitation process is 8.5～9.0 to ph afterwards, boils insulation 1.5～2.0h；After filter press, obtaining total amount of rare earth is 25-
30% cerium hydroxide wet cake；Cerium hydroxide wet cake and pure water are pulled an oar according to the ratio of mass ratio 1:5, adjusting ph with nitric acid is
1.5～2.5, after standing 3～5h, vacuum filtration, obtain ce4+Settled solution a；
(2) preparation of active component solution: in ce4+Settled solution a in, add except cerium other rare earth oxides nitre
Hydrochlorate, zirconyl nitrate, add organic complexing agent, obtain active component solution b；Other rare earth oxides of described except cerium
Nitrate, is two or three of lanthana, yittrium oxide, praseodymium oxide and the corresponding nitrate of Dineodymium trioxide；Described organic network
Mixture is hydroxy carboxylic acids；The addition of described hydroxy carboxylic acids, in mass, is the 10 of cerous nitrate consumption
～20%；
(3) precipitation: active component solution b is heated to 70～80 DEG C, under agitation, being slowly added to mass concentration is
10～15% ammonia, is 8.5～9 to precipitation terminal ph, is incubated 2～4h；After standing 12h, extract the supernatant, obtain solid-liquid and mix
Close serosity c；
(4) surface modification: add the polyacrylic acid that molecular weight is 4000～7000 in solid-liquid mixed serum c, stir 1～2h,
Obtain the material d of surface modification；Described polyacrylic acid, in mass, addition is the 1～2% of cerous nitrate consumption；
(5) roasting: by the material d of surface modification at 700～750 DEG C roasting 4～6h, finally be obtained cerium zirconium based solid solution.
2. cerium zirconium based solid solution according to claim 1 preparation method it is characterised in that: nitric acid in described step (1)
Cerium quality accounts for the 25～35% of cerous nitrate and water gross mass.
3. cerium zirconium based solid solution according to claim 1 preparation method it is characterised in that: described except cerium its
In mass, addition is 0.3～0.32 times of cerous nitrate consumption for his rare earth oxide.
4. cerium zirconium based solid solution according to claim 1 preparation method it is characterised in that: in described step (2), described
Zirconyl nitrate addition, in mass, be 1.17～1.53 times of cerous nitrate consumption.
5. cerium zirconium based solid solution according to claim 1 preparation method it is characterised in that: described hydroxycarboxylic acid
Compound is one of alpha-hydroxybutyric dehydrogenase, lactic acid, Alpha-hydroxy acetic acid or two kinds.
6. cerium zirconium based solid solution according to claim 1 preparation method it is characterised in that: obtained cerium zirconium base solid solution
Body is made up of the composite oxides that cerium oxide, zirconium oxide and the other rare earth oxides in addition to cerium zirconium form, its weight percent
Than as follows: cerium oxide: 40～50%, and other rare earth oxides in addition to cerium zirconium: 12～13%, remaining is zirconium oxide.
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| CN1449863A (en) * | 2003-04-28 | 2003-10-22 | 华东理工大学 | Nano Cerium-zirconium base compound oxide and preparation process thereof |
| CN102247826A (en) * | 2011-05-27 | 2011-11-23 | 济南大学 | Cubic phase cerium and zirconium based composite oxide with high specific surface area and preparation method thereof |
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| CN103127925A (en) * | 2011-11-23 | 2013-06-05 | 上海华明高纳稀土新材料有限公司 | Cerium-zirconium-based solid solution rare earth oxygen-storage material and preparation method thereof |
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| CN1449863A (en) * | 2003-04-28 | 2003-10-22 | 华东理工大学 | Nano Cerium-zirconium base compound oxide and preparation process thereof |
| CN102247826A (en) * | 2011-05-27 | 2011-11-23 | 济南大学 | Cubic phase cerium and zirconium based composite oxide with high specific surface area and preparation method thereof |
| CN102513085A (en) * | 2011-11-07 | 2012-06-27 | 上海华明高纳稀土新材料有限公司 | Cerium oxide-zirconium oxide-based composite oxide and preparation method thereof |
| CN103127925A (en) * | 2011-11-23 | 2013-06-05 | 上海华明高纳稀土新材料有限公司 | Cerium-zirconium-based solid solution rare earth oxygen-storage material and preparation method thereof |
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