CN105948098A - Spherical lanthanum oxide - Google Patents
Spherical lanthanum oxide Download PDFInfo
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- CN105948098A CN105948098A CN201610260597.2A CN201610260597A CN105948098A CN 105948098 A CN105948098 A CN 105948098A CN 201610260597 A CN201610260597 A CN 201610260597A CN 105948098 A CN105948098 A CN 105948098A
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- Prior art keywords
- lanthanum
- spherical alumina
- ethylene glycol
- spherical
- water
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- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 title abstract description 66
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 60
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 19
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 19
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 15
- 150000007524 organic acids Chemical class 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 150000002603 lanthanum Chemical class 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 29
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000005352 clarification Methods 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 3
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- 229910002422 La(NO3)3·6H2O Inorganic materials 0.000 claims description 2
- 229910002249 LaCl3 Inorganic materials 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- ICAKDTKJOYSXGC-UHFFFAOYSA-K lanthanum(iii) chloride Chemical compound Cl[La](Cl)Cl ICAKDTKJOYSXGC-UHFFFAOYSA-K 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 2
- 238000002425 crystallisation Methods 0.000 abstract 1
- 230000008025 crystallization Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000004005 microsphere Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000001788 irregular Effects 0.000 description 4
- 239000003981 vehicle Substances 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 2
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 239000004141 Sodium laurylsulphate Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- -1 when it is prepared Chemical compound 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007210 heterogeneous catalysis Methods 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a spherical lanthanum oxide. The average particle size of spherical lanthanum oxide is 150 nm-1.2 mum, the specific surface area after roasting at 1000 DEG C is 1-7 m<2>/g, and the specific surface area after roasting at 500 DEG C is 120-144 m<2>/g. The invention also discloses a preparation method of the spherical lanthanum oxide, and the method includes the following steps: (1) mixing lanthanum salt, hydrous ethylene glycol, polyvinylpyrrolidone, and short-chain organic acid, stirring the mixture, dissolving the mixture, and performing a hydrothermal reaction; and (2) subjecting the mixture to the reaction for 1-8 hours at 160-240 DEG C, cooling the mixture to obtain the precipitate, and drying the precipitate to obtain the spherical lanthanum oxide. The lanthanum oxide prepared by the invention is spherical, has uniform morphology, good degree of crystallization, good dispersibility, high heat stability, and big specific surface area, and is suitable for the application on the motor vehicle exhaust.
Description
Technical field
The invention belongs to micro Nano material synthesis field, be specifically related to a kind of spherical alumina lanthanum.
Background technology
Rare earth element has the 4f electron orbit of uniqueness, and in track, the motion mode of electronics makes rare earth element have and is different from other yuan
Optics, electricity and the magnetic property of element.Lanthana is as the one in light rare earth oxide, at precision optics glass, fluorescence
The aspects such as material, solid electrolyte battery, ceramic capacitor and gas sensor have important application.It addition, lanthana is same
Sample is good catalysis material, is widely used in heterogeneous catalysis field.In Vehicle Exhaust Gas Cleaning Catalysts, lanthana with
Cerium oxide all as auxiliary agent, can improve the dispersion of noble metal, the growth of suppression noble metal crystal grain, carries high catalytic activity；Lanthanum
Based perovskite type oxide produces Lacking oxygen due to fault of construction, the most just has and is well catalyzed activity.
The method of synthesis lanthana is various, and the lanthana of traditional sedimentation method and sol-gal process synthesis mostly is amorphous, exists
Poor heat stability, the deficiency such as high temperature easy-sintering, application in high temperature environments is limited.The La that traditional method obtains2O3Generally
Amorphous, degree of crystallinity is low, poor heat stability, typically comes increasing specific surface area and heat stability by doping, through 1000 DEG C of roastings
After burning, specific surface is less than 1m2/ g, is applied to motor-vehicle tail-gas catalytic efficiency low.
CN200910089538.3 discloses a kind of lanthana microsphere as dimension standard material, and described lanthana microsphere is nothing
Machine one organic hybrid microsphere, is made up of with polyvinylpyrrolidonemolecules molecules lanthana, wherein lanthana and polyvinylpyrrolidone
Weight ratio be 11-16:1, this inorganic organic hybrid microsphere is polycrystalline structure, belongs to cubic system, and crystal structure is fluorite
Type, structure cell is face-centred cubic structure, and microsphere form factor is less than 1.2, and size range is 90nm-450nm, the phase of size value
To uncertainty less than 5}0.Twice Hydrothermal Synthesis of the need of said method, operational approach is loaded down with trivial details, and the lanthana microsphere obtained exists
After 1000 DEG C of high-temperature roastings, its specific surface area is less than 1m2/ g, is applied to motor-vehicle tail-gas catalytic efficiency the lowest.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that a kind of better crystallinity degree, good dispersion, have more uniform
The spherical alumina lanthanum of pattern.
For reaching above-mentioned purpose, present invention employs following technical proposals:
A kind of spherical alumina lanthanum, the mean diameter of spherical alumina lanthanum is 150nm～1.2 μm, ratio table after roasting at 1000 DEG C
Area is 1-7m2/g。
Preferably, at 500 DEG C, specific surface area after roasting is 120-144m2/g。
Preferably, the preparation method of described spherical alumina lanthanum comprises the steps:
(1) mixing lanthanum salt, water and ethylene glycol, polyvinylpyrrolidone and short chain organic acid, carry out hydro-thermal anti-after stirring and dissolving
Should；
(2) react 1-8 hour at 160-240 DEG C；Being centrifuged after cooling and be precipitated thing, dry sediment obtains spherical alumina
Lanthanum.
Preferably, in described step (1), the volume ratio of water and ethylene glycol is 6-10:50-80.
Preferably, lanthanum salt and polyvinylpyrrolidone mol ratio be (200-270): 1, short chain organic acid and water and ethylene glycol it
The volume ratio of sum is 1:50-88, and lanthanum salt is 4-8:63-92 with the mass ratio of water and ethylene glycol sum.
Preferably, lanthanum salt is first dissolved in water and ethylene glycol in (1) by described step, is subsequently adding polyvinylpyrrolidone and stirs
Mix the solution to transparent clarification, after adding short chain organic acid, stir the solution to transparent clarification.
Preferably, described lanthanum salt is La (NO3)3·6H2O or LaCl3·7H2O。
Preferably, described short chain organic acid is selected from glacial acetic acid, propanoic acid, n-butyric acie and n-caproic acid.
The spherical alumina lanthanum of the present invention application in motor-vehicle tail-gas.
Compared with prior art, there is advantages that
1, the present invention prepares that the lanthana reacted time is short, easy and simple to handle, easy to control, easily repeats, use suitable organic acid and
Its consumption, the lanthana pattern globulate of synthesis and have more uniform pattern, better crystallinity degree, good dispersion, heat stability high,
Specific surface area is big.
2, the present invention uses ethylene glycol to be solvent, and ethylene glycol can occur stronger coordination with lanthanum so that it is in synthesis phase control
Make nanocrystalline growth.Additionally, the viscosity of ethylene glycol is high, it is possible to decrease nucleation and growth rate so as to get product morphology more
Uniformly, rule.The spherical secondary structure with relatively low-surface-energy can also be formed so that the spherical alumina lanthanum heat of preparation is steady simultaneously
Qualitative height.
The addition of water have adjusted viscosity, it is to avoid spheroidal particle sticks together.Meanwhile, the present invention uses PVP as surface activity
Agent, and with water and ethylene glycol in the range of proper ratio, it is spherical for not only preparing lanthana, and it has more uniform
Pattern, better crystallinity degree, good dispersion, heat stability are high, specific surface area is big.
Additionally, the addition of PVP and short chain organic acid has regulated and controled pattern, PVP is adsorbed in spherical surface, limits the size of particle diameter
And prevent the adhesion between spheroidal particle；Short chain organic acid affects the size of spheroidal particle, short chain organic acid due to exist carboxyl and
Alkyl, the carboxyl of one end can and La3+Coordination, the alkyl of the other end can be modified nanoparticle and affect between nanoparticle
Interact.
Accompanying drawing explanation
The X ray diffracting spectrum of lanthana in Fig. 1 embodiment 1
Lanthana SEM Electronic Speculum figure after 750 DEG C of roastings in Fig. 2 embodiment 1
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is entered
Row further describes, but the scope of protection of present invention is not limited to the scope that embodiment is expressed.
The composition of raw materials used that each embodiment and comparative example prepare lanthana is as follows:
Embodiment 1
A kind of spherical alumina lanthanum of preparation, has and comprises the steps:
(1) La (NO is weighed3)3·6H2O is dissolved in the mixed liquor of deionized water and ethylene glycol, stirs to being completely dissolved,
Add polyvinylpyrrolidone (PVP, molecular weight M=58000), stir about 1h, obtain the solution of transparent clarification, add
Propanoic acid, continues stirring 0.5h；
(2) mixed liquor obtaining transparent clarification proceeds to, in 100ml polytetrafluoroethyllining lining, put into stainless steel cauldron, 200 DEG C
Reaction 200min；
(3), after question response still is cooled to room temperature, product is centrifuged 5min with the rotating speed of 10000r/min, is precipitated thing,
Again with deionized water and ethanol alternately washing 3 times, obtain lanthana in 80 DEG C of dry 12h subsequently.
Test prepares: lanthana prepared by embodiment 1 is dried by (1), and becomes fine powder with mortar grinder, by wherein one
Half, in 500 DEG C of roasting 1h, 2 DEG C/min of heating rate, obtains carbonic acid dioxy lanthanum；Will wherein second half in 1000 DEG C of roasting 4h,
3 DEG C/min of heating rate, the lanthanum oxide powder obtained.
(2) XRD test: lanthana embodiment 1 prepared carries out XRD test and obtains X ray diffracting spectrum, such as figure
Shown in 1, result shows that the lanthana prepared is hexagonal crystal phase.
(3) SEM test: lanthana embodiment 1 prepared carries out SEM sem test, its pattern such as Fig. 2 institute
Show, figure it is seen that the lanthana of embodiment 1 preparation be particle diameter 150～300nm spherical.
Comparative example 1-1
A kind of spherical alumina lanthanum, is provided without the polyvinylpyrrolidone that molecular weight is 58000, remaining raw material and system when it is prepared
Preparation Method and each performance test are with embodiment 1.
Comparative example 1-2
A kind of spherical alumina lanthanum, when it is prepared, deionized water and ethylene glycol is not in OK range, remaining raw material and preparation method
And respectively test with embodiment 1.
Comparative example 1-3
A kind of spherical alumina lanthanum, when it is prepared, deionized water and ethylene glycol and polyvinylpyrrolidone three be not the most in OK range
In, remaining raw material and preparation method and test are with embodiment 1.
Comparative example 1-4
A kind of spherical alumina lanthanum, uses sodium lauryl sulphate to replace polyvinylpyrrolidone, remaining raw material and system when it is prepared
Preparation Method and test are with embodiment 1.
The test result of all above embodiment and comparative example such as following table:
Data above shows, comparative example 1-1 is provided without polyvinylpyrrolidone that molecular weight is 58000 as surfactant,
Relative to the lanthana of embodiment 1 preparation, the bigger pattern of its mean diameter is irregular and agglomeration occurs, through 500 DEG C, 1000 DEG C
After roasting, heat stability is worse relative to embodiment 1, and after especially 1000 DEG C roastings, its specific surface area is lower, relatively
In embodiment 1, it is not suitable for vehicle exhaust gas systems.
Comparative example 1-2 deionized water and ethylene glycol is not in OK range, and relative to the lanthana of embodiment 1 preparation, it is put down
All the bigger pattern of particle diameter is irregular and agglomeration occurs, through 500 DEG C, after 1000 DEG C of roastings, heat stability is relative to enforcement
Example 1 is worse, and after especially 1000 DEG C roastings, its specific surface area is lower, and relative to embodiment 1, it is not suitable for motor-driven vehicle
Gas catalyst.
Comparative example 1-3 deionized water and ethylene glycol and polyvinylpyrrolidone, not in OK range, are made relative to embodiment 1
Standby lanthana, the bigger pattern of its mean diameter is irregular and agglomeration occurs, through 500 DEG C, after 1000 DEG C of roastings, heat is steady
Qualitative property is worse relative to embodiment 1, and after especially 1000 DEG C roastings, its specific surface area is lower, relative to embodiment 1 its
It is not suitable for vehicle exhaust gas systems.
Comparative example 1-4 uses sodium lauryl sulphate to replace polyvinylpyrrolidone, relative to the lanthana of embodiment 1 preparation,
The bigger pattern of its mean diameter is irregular and agglomeration occurs, through 500 DEG C, after 1000 DEG C of roastings, heat stability relative to
Embodiment 1 is worse, and after especially 1000 DEG C roastings, its specific surface area is lower, and relative to embodiment 1, it is not suitable for motor-driven
Tail gas catalyst.
The announcement of book and teaching according to the above description, above-mentioned embodiment can also be become by those skilled in the art in the invention
More and amendment.Therefore, the invention is not limited in detailed description of the invention disclosed and described above, some of the present invention are repaiied
Change and change in the scope of the claims that should also be as falling into the present invention.Although additionally, this specification employing
Specific term, but these terms are merely for convenience of description, and the present invention does not constitute any restriction.
Claims (9)
1. a spherical alumina lanthanum, it is characterised in that the mean diameter of spherical alumina lanthanum is 150nm～1.2 μm, at 1000 DEG C
Specific surface area after lower roasting is 1-7m2/g。
2. spherical alumina lanthanum as claimed in claim 1, it is characterised in that the specific surface area after roasting is at 500 DEG C
120-144m2/g。
3. spherical alumina lanthanum as claimed in claim 1 or 2, it is characterised in that the preparation method bag of described spherical alumina lanthanum
Include following steps:
(1) mixing lanthanum salt, water and ethylene glycol, polyvinylpyrrolidone and short chain organic acid, carry out hydro-thermal anti-after stirring and dissolving
Should；
(2) react 1-8 hour at 160-240 DEG C；Being centrifuged after cooling and be precipitated thing, dry sediment obtains spherical alumina
Lanthanum.
4. spherical alumina lanthanum as claimed in claim 3, it is characterised in that water and the body of ethylene glycol in described step (1)
Long-pending ratio is 6-10:50-80.
5. spherical alumina lanthanum as claimed in claim 3, it is characterised in that lanthanum salt with polyvinylpyrrolidone mol ratio is
(200-270): 1, the volume ratio of short chain organic acid and water and ethylene glycol sum is 1:50-88, lanthanum salt and water and ethylene glycol it
The mass ratio of sum is 4-8:63-92.
6. spherical alumina lanthanum as claimed in claim 3, it is characterised in that lanthanum salt is first dissolved in (1) by described step
In water and ethylene glycol, it is subsequently adding the solution of polyvinylpyrrolidone stirring extremely transparent clarification, stirs after adding short chain organic acid
Mix the solution to transparent clarification.
7. the spherical alumina lanthanum as described in any one of claim 3-6, it is characterised in that described lanthanum salt is La (NO3)3·6H2O
Or LaCl3·7H2O。
8. the spherical alumina lanthanum as described in any one of claim 3-6, it is characterised in that described short chain organic acid is selected from ice second
Acid, propanoic acid, n-butyric acie and n-caproic acid.
9. spherical alumina lanthanum application in motor-vehicle tail-gas described in claim 1 or 2.
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|---|---|---|---|
| CN201610260597.2A CN105948098B (en) | 2016-04-22 | 2016-04-22 | A kind of spherical lanthana |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610260597.2A CN105948098B (en) | 2016-04-22 | 2016-04-22 | A kind of spherical lanthana |
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| CN105948098A true CN105948098A (en) | 2016-09-21 |
| CN105948098B CN105948098B (en) | 2017-11-14 |
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| CN113087729A (en) * | 2021-04-01 | 2021-07-09 | 山东大学 | Lanthanum complex precursor, lanthanum oxide fiber and preparation method and application of lanthanum zirconate fiber derived from lanthanum oxide fiber |
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| CN113891924A (en) * | 2020-02-27 | 2022-01-04 | 碧德·奧利珍股份有限公司 | Spherical inorganic particles with surface bumps and preparation method thereof |
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| CN115231605A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
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| CN110790297B (en) * | 2018-07-31 | 2022-01-18 | 盛和资源(江苏)稀土有限公司 | Production process of lanthanum oxide |
| CN110359043A (en) * | 2019-07-27 | 2019-10-22 | 西北师范大学 | Dielectric soaks the preparation method of the titanium-based lanthana nano flower film of low-voltage response |
| CN110359043B (en) * | 2019-07-27 | 2021-03-26 | 西北师范大学 | Preparation method of titanium-based lanthanum oxide nanoflower film with dielectric wetting low-voltage response |
| CN114728807A (en) * | 2019-10-23 | 2022-07-08 | 新性能材料(新加坡)私人有限公司 | Moderately dispersed Dy2O3Granules |
| CN111017980A (en) * | 2019-12-26 | 2020-04-17 | 宣城晶瑞新材料有限公司 | Preparation method of high-purity nano lanthanum oxide material |
| CN113891924A (en) * | 2020-02-27 | 2022-01-04 | 碧德·奧利珍股份有限公司 | Spherical inorganic particles with surface bumps and preparation method thereof |
| CN113891924B (en) * | 2020-02-27 | 2023-03-31 | 碧德·奧利珍股份有限公司 | Spherical inorganic particles with surface bumps and preparation method thereof |
| CN113087729A (en) * | 2021-04-01 | 2021-07-09 | 山东大学 | Lanthanum complex precursor, lanthanum oxide fiber and preparation method and application of lanthanum zirconate fiber derived from lanthanum oxide fiber |
| CN113651351A (en) * | 2021-08-16 | 2021-11-16 | 广东工业大学 | Samarium oxide and preparation and application thereof |
| CN115231605A (en) * | 2022-07-26 | 2022-10-25 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
| CN115231605B (en) * | 2022-07-26 | 2024-02-06 | 宣城市晶和环保新材料科技有限公司 | Preparation method of high-purity nano lanthanum oxyfluoride |
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