CN105668606B - A kind of preparation method of square nano-sheet cerium oxide - Google Patents
A kind of preparation method of square nano-sheet cerium oxide Download PDFInfo
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- CN105668606B CN105668606B CN201610137854.3A CN201610137854A CN105668606B CN 105668606 B CN105668606 B CN 105668606B CN 201610137854 A CN201610137854 A CN 201610137854A CN 105668606 B CN105668606 B CN 105668606B
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- 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
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- 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
- C01P2004/36—Spheres fragmented
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
It is raw material that a kind of preparation method of square nano-sheet cerium oxide of the present invention uses cerous nitrate, enuatrol, and absolute ethyl alcohol, n-hexane and water are solvent, and magnetic agitation is heated to 60 DEG C, and reaction prepares oleic acid cerium precursor；Then the high boiling organic solvents such as oleic acid cerium and oleic acid, oleyl amine and trioctylamine are mixed, magnetic agitation, N2Protection, is heated to 360 370 DEG C, is incubated 60 90min, and reaction uses absolute ethanol washing, centrifugation, obtains final product square nano-sheet cerium oxide, its thickness about 2nm, the 23nm of the length of side 10 after terminating.Equipment needed for this method for preparing square platy cerium oxide is simple, short preparation period, controllability are good, and the shape dependence to studying nano ZnO is significant, while having application value very high in storage oxygen and catalytic field.
Description
Technical field
The present invention relates to a kind of preparation method of square nano-sheet cerium oxide, nano material preparation technology is particularly belonged to
Field.
Background technology
Cerium oxide is led in purifying vehicle exhaust, photochemical catalyst, mechanical polishing, ultraviolet radiation absorption, fuel-cell electrolyte etc.
Domain has broad application prospects.Therefore, the research to cerium oxide nano materials is relatively more, and relatively deeply.Prepare at present and receive
The method of rice cerium oxide has a lot, mainly there is the precipitation method, electrostatic spinning, water（Solvent）Hot method, sol-gal process, combustion method, heat
Decomposition method etc..Using these methods, people have successfully been obtained the cerium oxide nano materials of many different-shapes, such as：China
Patent CN201310307042.5 with six water cerous nitrates, enuatrol be raw material, with Tween-80 as surfactant, with hydroxide
Sodium is precipitating reagent, and 170-190 DEG C is reacted 24h in a kettle., obtains oil solubility nanometer ceria；Patent
CN20141002673 is raw material with six water cerous nitrates, enuatrol, and with CTAB as surfactant, NaOH is precipitating reagent,
180 DEG C of reaction kettle for reaction, obtain excellent oil-soluble ceria superfine powder, and particle diameter distribution is uniform, good dispersion.Patent
With cerous nitrate as raw material, ammonium hydrogen carbonate is precipitating reagent to CN201410192456.2,0-50 DEG C of reaction, aged, filtering, washing,
Annealing obtains flake nano cerium oxide；Patent CN201310194946.1 with cerous nitrate or cerium chloride as raw material, at -10 ~ 20 DEG C
Excessive ammonia is added dropwise, reaction kettle for reaction obtains platy cerium oxide, thickness 10-30nm.Surface-active is added in above-mentioned patent
Agent, the pattern heterogeneity of gained nano-cerium oxide, crystallinity is not high；And the thickness of flake nano cerium oxide is more than 10nm,
Specific surface area is small, has had a strong impact on its performance and application.
In recent years, researchers have found that super-thin sheet-shaped cerium oxide has specific surface area high, and surface-active is high, shows excellent
Different storage oxygen and catalytic performance, application prospect are very tempting.Therefore, it is necessary to develop it is a kind of it is novel easy prepare particle diameter it is small,
The method of the big cerium oxide of single dispersing, super-thin sheet-shaped, specific surface area.
The content of the invention
It is an object of the invention to provide a kind of preparation method of square nano-sheet cerium oxide, especially by following skill
Art scheme is realized.
A kind of preparation method of square nano-sheet cerium oxide of the present invention, comprises the following steps：
（1）Six water cerous nitrate 0.217g, enuatrol 0.457g are placed in conical flask, 2ml absolute ethyl alcohols, 3.5ml is added
N-hexane and 20ml deionized waters, magnetic agitation are simultaneously heated to 60 DEG C, insulation 4h；0- is put into after product is cooled into room temperature
3 DEG C of refrigerator cold-storage 2h, surplus liquid in conical flask is poured out, then is rinsed 3 times with absolute ethyl alcohol, obtains oleic acid cerium precursor thing；Its
In six water cerous nitrates, enuatrol mol ratio be 1:3.
（2）In step（1）In obtained oleic acid cerium precursor thing, 1-1.5ml oleic acid, 1-1.5ml oleyl amines and 6-9ml tri- are added
Octylame, is passed through N2Gas, magnetic agitation, reactant mixture is heated to 120 DEG C, after insulation 30-35min, is heated rapidly to 360-
370 DEG C, and it is incubated 60-90min；Then after product naturally cools to room temperature, absolute ethanol washing is added, then through being centrifuged
Filter obtains filter cake；Use absolute ethanol washing filter cake again, and through centrifugal treating filter cake after, be dispersed in n-hexane,
Obtain square nano-sheet cerium oxide；Wherein oleic acid, oleyl amine, the volume ratio of trioctylamine are 1:1:6.
The beneficial effects of the invention are as follows：
Preparation method of the invention need not add Morphological control agent or dispersant, required equipment is simple, short preparation period,
Controllability is good.The nano-cerium oxide pattern rule of production, good dispersion, size uniformity, thickness are about 2nm, length of side 10-23nm.
Shape dependence to studying nano ZnO is significant, at the same storage oxygen and catalytic field have it is very high should
With value.
Brief description of the drawings
Fig. 1 is the TEM photos of the products therefrom of the embodiment of the present invention 1；Fig. 2 shines for the TEM of the products therefrom of the embodiment of the present invention 2
Piece.
Specific embodiment
Embodiment 1
A kind of preparation method of square nano-sheet cerium oxide, comprises the following steps：
（1）Weigh cerous nitrate（Ce(NO3)3.6H2O）0.217g, enuatrol 0.457g are placed in conical flask, add 2ml without
Water-ethanol, 3.5ml n-hexanes and 20ml deionized waters, are placed in magnetic agitation in oil bath, and be heated to 60 °C, insulation by conical flask
4h；Conical flask is taken out after completion of the reaction is cooled to room temperature, be put into 0-3 °C of refrigerator cold-storage 2h, superfluous water in conical flask is poured out,
Rinsed 3 times with absolute ethyl alcohol again, obtain oleic acid cerium precursor thing.
（2）By step（1）In the oleic acid cerium that obtains move into there-necked flask, add 1ml oleic acid, 1ml oleyl amines and 6ml tri- pungent
Amine, magnetic agitation is passed through N2Gas, with electric jacket heated solution to 120 °C, is incubated 30min；Then rapid heated solution is extremely
360-370 °C, and 90min is incubated, then naturally cool to room temperature.To absolute ethyl alcohol is added in product, through centrifugal filtration
Filter cake is obtained, again with absolute ethanol washing, then be dispersed in filter cake in n-hexane by centrifugal treating, obtains length of side 15-
The square nano-sheet cerium oxide of 23nm, thickness about 2nm.
Embodiment 2
A kind of preparation method of square nano-sheet cerium oxide, comprises the following steps：
（1）Weigh cerous nitrate（Ce(NO3)3.6H2O）0.217g, enuatrol 0.457g are placed in conical flask, add 2ml without
Water-ethanol, 3.5ml n-hexanes and 20ml deionized waters, are placed in magnetic agitation in oil bath, and be heated to 60 °C, insulation by conical flask
4h；Conical flask is taken out after completion of the reaction is cooled to room temperature, be put into 0-3 °C of refrigerator cold-storage 2h, superfluous water in conical flask is poured out,
Rinsed 3 times with absolute ethyl alcohol again, obtain oleic acid cerium precursor thing.
（2）By step（1）In the oleic acid cerium that obtains move into there-necked flask, add 1.5ml oleic acid, 1.5ml oleyl amines and 9ml tri-
Octylame, magnetic agitation is passed through N2Gas, with electric jacket heated solution to 120 °C, is incubated 30min；Then rapid heated solution is extremely
360-370 °C, and 60min is incubated, then naturally cool to room temperature.To absolute ethyl alcohol is added in product, through centrifugal filtration
Filter cake is obtained, again with absolute ethanol washing, then be dispersed in filter cake in n-hexane by centrifugal treating, obtains length of side 10-
The square nano-sheet cerium oxide of 13nm, thickness about 2nm.
Claims (1)
1. a kind of preparation method of square nano-sheet cerium oxide, it is characterised in that：Described preparation method includes following step
Suddenly：
（1）Six water cerous nitrate 0.217g, enuatrol 0.457g are placed in conical flask, add 2ml absolute ethyl alcohols, 3.5ml just oneself
Alkane and 20ml deionized waters, magnetic agitation are simultaneously heated to 60 DEG C, insulation 4h；0-3 DEG C is put into after product is cooled into room temperature
Refrigerator cold-storage 2h, surplus liquid in conical flask is poured out, then is rinsed 3 times with absolute ethyl alcohol, obtains oleic acid cerium precursor thing；Wherein six
Water cerous nitrate, the mol ratio of enuatrol are 1:3；
（2）In step（1）In obtained oleic acid cerium precursor thing, add 1-1.5ml oleic acid, 1-1.5ml oleyl amines and 6-9ml tri- pungent
Amine, is passed through N2Gas, magnetic agitation, reactant mixture is heated to 120 DEG C, after insulation 30-35min, is heated rapidly to 360-370
DEG C, and it is incubated 60-90min；Then after product naturally cools to room temperature, absolute ethanol washing is added, then through centrifugal filtration
Obtain filter cake；Use absolute ethanol washing filter cake again, and through centrifugal treating filter cake after, be dispersed in n-hexane, obtain
To square nano-sheet cerium oxide；Wherein oleic acid, oleyl amine, the volume ratio of trioctylamine are 1:1:6.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107335416A (en) * | 2017-06-08 | 2017-11-10 | 浙江工业大学 | A kind of catalyst nanoparticles dispersion liquid and preparation method and application |
| CN108190937A (en) * | 2018-03-23 | 2018-06-22 | 中国科学院化学研究所 | A kind of method that oil-soluble cerium oxide nanoparticles are quickly prepared in oleyl amine solvent |
| CN111662764A (en) * | 2020-06-10 | 2020-09-15 | 江苏凯瑞德润滑技术有限公司 | Method for preparing calcium-based lubricating grease by using waste rapeseed oil and triazine-modified lanthanum oxide |
| CN112919523B (en) * | 2021-03-16 | 2022-01-28 | 厦门稀土材料研究所 | Preparation method of hexagonal flaky rare earth cerium oxide |
Citations (4)
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| CN101282910A (en) * | 2005-10-08 | 2008-10-08 | 首尔国立大学工业基金会 | Process for producing cerium oxide nanocrystals |
| US7867463B2 (en) * | 2005-10-08 | 2011-01-11 | Taeg-Hwan Hyeon | Process for producing cerium oxide nanocrystals |
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| CN103387257A (en) * | 2013-07-19 | 2013-11-13 | 东华大学 | Method for preparing nano cerium dioxide material by utilizing tween-80 as surfactant |
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2016
- 2016-03-11 CN CN201610137854.3A patent/CN105668606B/en not_active Expired - Fee Related
Patent Citations (4)
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| CN101282910A (en) * | 2005-10-08 | 2008-10-08 | 首尔国立大学工业基金会 | Process for producing cerium oxide nanocrystals |
| US7867463B2 (en) * | 2005-10-08 | 2011-01-11 | Taeg-Hwan Hyeon | Process for producing cerium oxide nanocrystals |
| CN102936033A (en) * | 2012-12-04 | 2013-02-20 | 九江学院 | Method for preparing monodisperse zinc oxide ultrathin nanosheets |
| CN103387257A (en) * | 2013-07-19 | 2013-11-13 | 东华大学 | Method for preparing nano cerium dioxide material by utilizing tween-80 as surfactant |
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| Controlled Synthesis of Monodisperse CeO2 Nanoplates Developed from Assembled Nanoparticles;Haruo Imagawa等;《The Journal of Physical Chemistry C》;20120103;第116卷;第2761-2765页 * |
| Large-Scale Nonhydrolytic Sol–Gel Synthesis of Uniform-Sized Ceria Nanocrystals with Spherical,Wire, and Tadpole Shapes;Taekyung Yu等;《Angew. Chem.》;20051231;第117卷;第7577-7580页 * |
| Mineralizer-Assisted Shape-Control of Rare Earth Oxide Nanoplates;Dianyuan Wang等;《Chemistry of Materials》;20141103;第26卷;第6328 −6332页 * |
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