CN105948098A - Spherical lanthanum oxide - Google Patents

Spherical lanthanum oxide Download PDF

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Publication number
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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CN201610260597.2A
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CN105948098B (en
Inventor
余林
杨润农
赵向云
范群
萧剑鸣
杨晓波
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WAYGREEN TECHNOLOGIES Inc
Guangdong University of Technology
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WAYGREEN TECHNOLOGIES Inc
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/206Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/30Particle morphology extending in three dimensions
    • C01P2004/32Spheres
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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  • 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

A kind of spherical alumina lanthanum
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.
CN201610260597.2A 2016-04-22 2016-04-22 A kind of spherical lanthana Expired - Fee Related CN105948098B (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
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
CN110790297A (en) * 2018-07-31 2020-02-14 中铝稀土(江苏)有限公司 Production process of lanthanum oxide
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
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
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
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
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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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110790297A (en) * 2018-07-31 2020-02-14 中铝稀土(江苏)有限公司 Production process of lanthanum oxide
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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