CN109794252A - A kind of magnetism cerium zirconium compound oxide and the preparation method and application thereof - Google Patents
A kind of magnetism cerium zirconium compound oxide and the preparation method and application thereof Download PDFInfo
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Abstract
The present invention relates to a kind of magnetic cerium zirconium compound oxides and the preparation method and application thereof.The magnetism cerium zirconium compound oxide, includes: 20-70 parts of cerium oxide by weight percentage, and 20-60 parts of zirconium oxide, ferroso-ferric oxide or 20-50 parts of mangano-manganic oxide, 3-20 parts of any one or several rare earth oxides in addition to cerium.Magnetism cerium zirconium compound oxide of the invention, is rich in Fe3+/Fe2+Or Mn3+/Mn2+, the ability and rate of instantaneous storage oxygen are increased, the defect of lattice and structure is increased, increases the rate travel of static oxygen storage capacity and Lattice Oxygen；The temperature for reducing reduction increases the detergent power of the tail gas in cold-starting automobile stage.Present invention magnetism cerium zirconium compound oxide specific surface area with higher and Kong Rong, ageing resistance is strong, and service life is longer, and is conducive to the coating and separation of cerium zirconium based composite oxide.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, and in particular to a kind of magnetism cerium zirconium compound oxide and its preparation side
Method and application.
Background technique
With the increase of automobile quantity, the pollution of vehicle exhaust is very serious, has developed efficient tai-gas clean-up catalyst
Through becoming current research hotspot.Cerium zirconium compound oxide is the critical material of automobile three-way catalyst.Vehicle exhaust temperature becomes
Change larger, requirement highest of the tail gas clean-up of low-temperature space and high-temperature region to cerium zirconium compound oxide.Cerium zirconium compound oxide is necessary
Have the detergent power that higher oxygen storage capacity increases low-temperature space, while must have higher ageing resistance and increase high temperature
The detergent power in area and the service life of three-way catalyst.
Summary of the invention
It is an object of that present invention to provide a kind of magnetic cerium zirconium compound oxides and the preparation method and application thereof.
The study found that introduce lanthanide series metal in cerium zirconium compound oxide, alkali earth metal etc. can effectively increase it is anti-ageing
Change ability and storage put oxygen performance.Fe is introduced in cerium zirconium compound oxide3+/Fe2+Or Mn3+/Mn2+, not only can increase lattice defect
Oxygen storage capacity is further increased, and there is magnetism simultaneously.In magnetic cerium zirconium compound oxide due to containing transition metal iron and
Manganese has lower reduction temperature, increases the efficiency of cold-starting automobile stage vehicle maintenance service.Magnetic cerium-zirconium composite oxide
Object not only has high specific surface area, Kong Rong and the high oxygen storage capacity of traditional cerium zirconium compound oxide, and has magnetism, is easy to
The coating and separation of carrier.
Specifically, the present invention provides a kind of magnetic cerium zirconium compound oxide, include: by weight percentage
20-70 parts of cerium oxide,
20-60 parts of zirconium oxide,
Ferroso-ferric oxide or 20-50 parts of mangano-manganic oxide,
3-20 parts of any one or several rare earth oxides in addition to cerium.
Preferably, the magnetic cerium zirconium compound oxide includes: by weight percentage
20-50 parts of cerium oxide,
20-50 parts of zirconium oxide,
Ferroso-ferric oxide or 20-50 parts of mangano-manganic oxide,
3-20 parts of any one or several rare earth oxides in addition to cerium.
It is further preferred that the magnetism cerium zirconium compound oxide includes: by weight percentage
20-30 parts of cerium oxide,
20-30 parts of zirconium oxide,
Ferroso-ferric oxide or 25-35 parts of mangano-manganic oxide,
5-10 parts of lanthana,
5-10 parts of praseodymium oxide.
Rare earth element except cerium (Ce) of the present invention refer to lanthanum (La), praseodymium (Pr), neodymium (Nd), promethium (Pm), samarium (Sm),
Europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), yttrium (Y) and scandium (Sc).
The rare earth oxide in addition to cerium is preferably lanthana, praseodymium oxide, neodymia, yttrium oxide, samarium oxide
Any one or more of.It is demonstrated experimentally that when the rare earth oxide in addition to cerium is lanthana and praseodymium oxide, storage
Put oxygen and the performances such as anti-aging more preferably.
Specifically, the magnetic cerium zirconium compound oxide is by cerium oxide, zirconium oxide, ferroso-ferric oxide or four oxidations three
Manganese, and the rare earth oxide composition in addition to cerium, total amount are 100 parts.
In the specific embodiment of the invention, with weight, the magnetism cerium zirconium compound oxide is by following
Group is grouped as:
Cerium oxide 20%-50%,
Zirconium oxide 20%-50%,
Ferroso-ferric oxide 20%-50%,
One or more of lanthana, praseodymium oxide, neodymia, yttrium oxide 3%-20%.
Preferably, with weight, the magnetism cerium zirconium compound oxide is composed of the following components:
Cerium oxide 20%-30%,
Zirconium oxide 20%-30%,
Ferroso-ferric oxide 25%-35%,
Lanthana 5%-10%,
Praseodymium oxide 5%-10%.
Prepare zirconium source used in magnetic cerium zirconium compound oxide of the present invention can be selected from zirconium nitrate, zirconium sulfate, basic zirconium chloride,
Acetic acid zirconium etc..Consider preferred zirconium oxychloride as zirconium source from price angle.
Preparing cerium source used in magnetic cerium zirconium compound oxide of the present invention can be selected from cerous nitrate, cerium chloride, cerous carbonate, nitre
Sour cerium ammonium, Cericammoniumsulfate etc., preferably using ammonium ceric nitrate as cerium source.
Preparing source of iron used in magnetic cerium zirconium compound oxide of the present invention can be selected from ferric trichloride and ferrous chloride；It is used
Manganese source can be selected from manganic chloride and manganous chloride as manganese source.Rare earth element source used can be selected from its correspondingly nitrate or chlorination
Object.
Magnetism cerium zirconium compound oxide of the present invention has the property that
750 DEG C, BET specific surface is at least 80m2The hole /g, BJH holds in 0.55ml/g between 0.80ml/g, and aperture is presented
Diplopore distribution, based on mesoporous, distribution 2-5nm, 10-50nm；And/or
4h is calcined at 1100 DEG C, BET specific surface is at least 30m2/g；The hole BJH holds in 0.35ml/g between 0.50ml/g,
Diplopore distribution, based on mesoporous, distribution 2-3nm, 30-100nm is presented in aperture；And/or
The oxygen storage capacity of the composite oxides is in 500 μm of olO2/ g to 1200 μm of olO2Between/g；And/or
The composite oxides pass through temperature programmed reduction (H2- TPR) measurement highest reduction temperature be less than or equal to 500
℃；And/or
The composite oxides vibrate magnetic strength by sample and measure its B-H loop, and saturation magnetization is in 20emu/g
To 50emu/g.
Sol-gel self-combustion synthesis synthesis can be used in above-mentioned magnetism cerium zirconium compound oxide.Firstly, synthesis cerium zirconium iron and except cerium with
The colloidal sol of outer rare earth element is conducive to each component and is uniformly dispersed；Further hydrothermal synthesis advantageously form specific morphology and
The magnetic cerium zirconium compound oxide of high-specific surface area.The magnetic cerium zirconium compound oxide that sol-gel self-combustion synthesis generates overcomes tradition
The low disadvantage of the easy high temperature sintering of cerium zirconium based composite oxide and oxygen storage capacity of coprecipitation technology, and be easy to coat and divide with carrier
From the following application prospect is very wide.
Specifically, the present invention also provides the preparation methods of above-mentioned magnetic cerium zirconium compound oxide, comprising:
1) raw material for preparing each oxide is dissolved in water, mixed solution is made；Ammonium hydroxide is added (preferably into the mixed solution
Adjust pH to 10 or more), mixed hydroxides sediment is made；
2) polarity decentralized medium is added into mixed hydroxides made from step 1), dispersant nonpolar liquid is made；The pole
Property decentralized medium can be selected from ethyl alcohol, ethylene glycol isopolarity solvent, preferably ethylene glycol；
3) acid is added into dispersant nonpolar liquid made from step 2), adjusts pH to acidity, acid dispersion is made；Heating system
At mixed sols；
The acid for adjusting pH such as nitric acid commonly used in the art, sulfuric acid, hydrochloric acid can be used；
General heating temperature is 80 DEG C or so；
4) mixed sols prepared by step 3) is heated into aqueous medium reaction and composite oxides is made；Then calcining system
At the magnetic cerium zirconium compound oxide；General heating temperature is 180 DEG C or so；General calcination temperature is 750 DEG C or so, calcining
Time 4h or so.It can be calcined under the conditions of oxidizing atmosphere.
The invention also includes the magnetic cerium zirconium compound oxides of above method preparation.
The invention also includes application of the above-mentioned magnetic cerium zirconium compound oxide in tail gas denitration.The tail gas includes various
Nitrogen-containing oxide (NOx) tail gas, such as the motor-driven diesel exhaust of motor vehicle, ship, power plant, boiler and factory's combustion tail gas
Deng.
The raw materials used in the present invention is commercially available to buy, or prepares by conventional method in that art.
On the basis of common knowledge of the art, above-mentioned each optimum condition can be combined with each other each preferably to get the present invention
Example.
Magnetism cerium zirconium compound oxide of the invention, is rich in Fe3+/Fe2+Or Mn3+/Mn2+。Fe3+/Fe2+Or Mn3+/Mn2+Have
Compare Ce4+/Ce3+Lower oxidation-reduction potential increases the ability and rate of instantaneous storage oxygen, increases lattice and structure
Defect increases the rate travel of static oxygen storage capacity and Lattice Oxygen.Meanwhile the introducing of two kinds of transition metal elements of iron and manganese,
The temperature for reducing reduction increases the detergent power of the tail gas in cold-starting automobile stage.Magnetism cerium-zirconium composite oxide of the invention
Object specific surface area with higher and Kong Rong, ageing resistance is strong, and service life is longer, and is conducive to cerium zirconium based composite oxide
Coating and separation.The present invention utilizes sol-gel self-combustion synthesis synthesizing magnetic cerium zirconium based composite oxide, overcomes conventional coprecipitation work
The low disadvantage of the easy high temperature sintering of cerium zirconium based composite oxide and oxygen storage capacity of skill, is easy to industrial applications.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..It is not specified in embodiment specific
Technology or conditions person, described technology or conditions according to the literature in the art, or carried out according to product description.It is used
Production firm person is not specified in reagent or instrument, is the conventional products that can be commercially available by regular distributor.
Embodiment 1
A kind of magnetism cerium zirconium compound oxide, with weight, consisting of: cerium oxide 30%, zirconium oxide
30%, ferroso-ferric oxide 25%, lanthana 10%, praseodymium oxide 5%.
The present embodiment also provides the preparation method of above-mentioned magnetic cerium zirconium compound oxide, includes the following steps:
1) zirconium oxychloride needed for preparing ammonium ceric nitrate (cerium source) needed for preparing 300g cerium oxide, preparing 300g zirconium oxide
(zirconium source), prepare 250g ferroso-ferric oxide needed for iron chloride and frerrous chloride (the two molar ratio is 2:1, source of iron), preparation
Lanthanum nitrate needed for 100g lanthana (lanthanum source) and the corresponding praseodymium nitrate of 50g praseodymium oxide (praseodymium source)；It is dissolved in 2000mL ultrapure water,
Mixed solution is made, ammonium hydroxide is slowly added dropwise into the solution, adjusts pH value to 10 or more, obtains cerium hydroxide-zirconium hydroxide-
Iron hydroxide-ferrous hydroxide-lanthanum hydroxide-praseodymium hydroxide mixed hydroxides, filtration washing obtain mixed hydroxides
Sediment；
2) above-mentioned sediment is added in the ethylene glycol solution of 1500mL, dispersant nonpolar liquid is made.
3) nitric acid is slowly added dropwise into the dispersion of gained polarity, adjusts pH value to acidity, acid dispersion is made；It is heated to 80
DEG C keep 48h, cerium oxide-zirconium oxide-ferroso-ferric oxide-lanthana-praseodymium oxide mixed sols is made.
4) gained mixed sols is put into 10L autoclave, reacts 8h in 180 DEG C of aqueous mediums, oxidation is made
Cerium-zirconium oxide-ferroso-ferric oxide-lanthana-praseodymium oxide magnetic coupling oxide.By gained magnetism cerium-zirconium composite oxide
Object calcines 4h in 750 DEG C of oxidizing atmospheres, finally obtains fresh magnetic cerium zirconium compound oxide.
Embodiment 2
A kind of magnetism cerium zirconium compound oxide, with weight, consisting of: cerium oxide 30%, zirconium oxide
30%, mangano-manganic oxide 25%, lanthana 10%, praseodymium oxide 5%.
The present embodiment also provides the preparation method of above-mentioned magnetic cerium zirconium compound oxide, comprising: prepares preparation 300g oxidation
Ammonium ceric nitrate needed for cerium (cerium source), prepare 300g zirconium oxide needed for zirconium oxychloride (zirconium source), preparation 250g mangano-manganic oxide
Corresponding manganic chloride and manganous chloride (the two molar ratio is 2:1, manganese source), prepare 100g lanthana needed for lanthanum nitrate (lanthanum
Source) and the corresponding praseodymium nitrate of 50g praseodymium oxide (praseodymium source)；It is dissolved in 2000mL ultrapure water, mixed solution is made；Subsequent step and reality
It is identical to apply example 1.
Embodiment 3
A kind of magnetism cerium zirconium compound oxide, with weight, consisting of: cerium oxide 30%, zirconium oxide
20%, ferroso-ferric oxide 35%, lanthana 10%, praseodymium oxide 5%.
The present embodiment also provides the preparation method of above-mentioned magnetic cerium zirconium compound oxide, comprising: prepares preparation 300g oxidation
Ammonium ceric nitrate needed for cerium (cerium source), prepare 200g zirconium oxide needed for zirconium oxychloride (zirconium source), preparation 350g ferroso-ferric oxide
Required iron chloride and frerrous chloride (the two molar ratio is 2:1, source of iron), prepare 100g lanthana needed for lanthanum nitrate (lanthanum source)
And the corresponding praseodymium nitrate of 50g praseodymium oxide (praseodymium source)；It is dissolved in 2000mL ultrapure water, mixed solution is made；Subsequent step and implementation
Example 1 is identical.
Comparative example 1
A kind of cerium zirconium compound oxide, with weight, consisting of: zirconium oxide 40%, cerium oxide 40%, oxygen
Change lanthanum 10%, praseodymium oxide 10%.
The preparation method of this comparative example cerium zirconium compound oxide, comprising: oxychlorination needed for preparation prepares 400g zirconium oxide
Zirconium (zirconium source), prepare 400g cerium oxide needed for ammonium ceric nitrate (cerium source), prepare 100g lanthana needed for lanthanum nitrate (lanthanum source)
And the corresponding praseodymium nitrate of 100g praseodymium oxide (praseodymium source)；It is dissolved in 2000mL ultrapure water, mixed solution is made；Subsequent step and implementation
Example 1 is identical.
Experimental example 1
Respectively to the carry out physical and chemical performance test of cerium zirconium compound oxide prepared by embodiment 1-3 and comparative example 1, as a result
As shown in table 1 below.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | |
| 750 DEG C of specific surface (m2/g) | 108 | 100 | 95 | 103 |
| 750 DEG C of holes hold (mL/g) | 0.66 | 0.63 | 0.58 | 0.65 |
| 750 DEG C of apertures (nm) | 25 | 27 | 23 | 27 |
| 1100 DEG C of specific surface (m2/g) | 32 | 35 | 30 | 31 |
| 1100 DEG C of holes hold (mL/g) | 0.20 | 0.23 | 0.18 | 0.19 |
| 1100 DEG C of apertures (nm) | 34 | 30 | 32 | 35 |
| Magnetic intensity (emu/g) | 25 | 23 | 30 | 0 |
Experimental example 2
Respectively to the carry out application performance test of cerium zirconium compound oxide prepared by embodiment 1-3 and comparative example 1.
Experimental method:
1, the preparation of catalyst: preparation catalyst is used.It respectively will be provided by embodiment 1-3 and comparative example 1
Cerium zirconium compound oxide, that is, catalyst carrier (i.e. catalyst carrier) is impregnated into H2PdCl4Impregnate 18h in aqueous solution, wherein Pd
Load capacity is 0.5%, is washed with deionized after hydrazine hydrate reduction processing, roasts in 100 DEG C of dry 6h, 480 DEG C of air atmospheres
2h is burnt, fresh catalyst is obtained.
2, the catalytic effect evaluation of catalyst: the evaluation of catalyst uses self-built micro-reaction device.Simulate gas ingredient NO
(1000ppm)、NO2(300ppm)、C3H6(670ppm)、CO(7500ppm)、O2With Ar (Balance Air).During evaluating catalyst
Use T50And T90Indicate catalyst to the catalytic activity of specified reactant.T50To specify the reaction temperature that reactant is 50%, T90For
The reaction temperature that specified reaction-ure conversion-age is 90%.Control λ={ 2 [O2]+[ON]+2[NO2]/{ 9 [CH]+[CO] }, air speed
43000h-1。
Test result is as follows shown in table 2.
Table 2
The aging specific surface that the above test result shows magnetic cerium zirconium sosoloid not only and has traditional cerium zirconium sosoloid high
Product, and its efficiency for purifying vehicle exhaust is very high.Magnetic cerium zirconium sosoloid has magnetism, is easy to the coating and separation of carrier,
Have the advantages that conventional cerium zirconium sosoloid is incomparable.
Although above the present invention is described in detail with a general description of the specific embodiments,
On the basis of the present invention, it can be made some modifications or improvements, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements, fall within the scope of the claimed invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. a kind of magnetism cerium zirconium compound oxide, which is characterized in that include: by weight percentage
20-70 parts of cerium oxide,
20-60 parts of zirconium oxide,
Ferroso-ferric oxide or 20-50 parts of mangano-manganic oxide,
3-20 parts of any one or several rare earth oxides in addition to cerium；
Preferably, the magnetic cerium zirconium compound oxide includes: by weight percentage
20-50 parts of cerium oxide,
20-50 parts of zirconium oxide,
Ferroso-ferric oxide or 20-50 parts of mangano-manganic oxide,
3-20 parts of any one or several rare earth oxides in addition to cerium.
2. magnetism cerium zirconium compound oxide according to claim 1, which is characterized in that include: by weight percentage
20-30 parts of cerium oxide,
20-30 parts of zirconium oxide,
Ferroso-ferric oxide or 25-35 parts of mangano-manganic oxide,
5-10 parts of lanthana,
5-10 parts of praseodymium oxide.
3. magnetism cerium zirconium compound oxide according to claim 1 or 2, which is characterized in that by cerium oxide, zirconium oxide, four
Fe 3 O or mangano-manganic oxide, and the rare earth oxide composition in addition to cerium；It is preferred that its total amount is 100 parts.
4. magnetism cerium zirconium compound oxide according to claim 1-3, which is characterized in that described in addition to cerium
Rare earth oxide is lanthana, praseodymium oxide, neodymia, yttrium oxide or samarium oxide.
5. a kind of magnetism cerium zirconium compound oxide, which is characterized in that composed of the following components with weight:
Cerium oxide 20%-50%,
Zirconium oxide 20%-50%,
Ferroso-ferric oxide 20%-50%,
One or more of lanthana, praseodymium oxide, neodymia, yttrium oxide 3%-20%；
Preferably, with weight, the magnetism cerium zirconium compound oxide is composed of the following components:
Cerium oxide 20%-30%,
Zirconium oxide 20%-30%,
Ferroso-ferric oxide 25%-35%,
Lanthana 5%-10%,
Praseodymium oxide 5%-10%.
6. the preparation method of any one of the claim 1-5 magnetic cerium zirconium compound oxide characterized by comprising
1) raw material for preparing each oxide is dissolved in water, mixed solution is made；Ammonium hydroxide is added into the mixed solution, mixing is made
Hydroxide sediment；
2) polarity decentralized medium is added into mixed hydroxides made from step 1), dispersant nonpolar liquid is made；
3) acid is added into dispersant nonpolar liquid made from step 2), adjusts pH to acidity, acid dispersion is made；Heating is made mixed
Close colloidal sol；
4) mixed sols prepared by step 3) is heated into aqueous medium reaction and composite oxides is made；Then institute is made in calcining
State magnetic cerium zirconium compound oxide.
7. preparation method according to claim 6, which is characterized in that step 1) by be added ammonium hydroxide adjust pH to 10 with
On；And/or
Step 2) the polarity decentralized medium is ethyl alcohol or ethylene glycol；And/or
Step 3) the heating temperature is 180 DEG C or so；And/or calcination temperature is 750 DEG C or so.
8. claim 6 or the magnetic cerium zirconium compound oxide of 7 the methods preparation.
9. claim 1-5,8 described in any item magnetic cerium zirconium compound oxides, which is characterized in that have the property that
750 DEG C, BET specific surface is at least 80m2The hole /g, BJH holds in 0.55ml/g between 0.80ml/g, and diplopore point is presented in aperture
Cloth, based on mesoporous, distribution 2-5nm, 10-50nm；And/or
4h is calcined at 1100 DEG C, BET specific surface is at least 30m2/g；The hole BJH holds in 0.35ml/g between 0.50ml/g, aperture
Diplopore distribution, based on mesoporous, distribution 2-3nm, 30-100nm is presented；And/or
The oxygen storage capacity of the composite oxides is in 500 μm of olO2/ g to 1200 μm of olO2Between/g；And/or
The composite oxides pass through temperature programmed reduction (H2- TPR) measurement highest reduction temperature be less than or equal to 500 DEG C；
And/or
The composite oxides vibrate magnetic strength by sample and measure its B-H loop, saturation magnetization 20emu/g extremely
50emu/g。
10. application of any one of claim 1-5,8, the 9 magnetic cerium zirconium compound oxide in tail gas denitration.
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| CN114364460A (en) * | 2019-09-10 | 2022-04-15 | 三井金属矿业株式会社 | Powder of composite oxide containing cerium element and zirconium element, exhaust gas purifying catalyst composition using same, and method for producing same |
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