CN108585017A - A kind of preparation method of rare earth oxide ceria - Google Patents
A kind of preparation method of rare earth oxide ceria Download PDFInfo
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- CN108585017A CN108585017A CN201810821762.6A CN201810821762A CN108585017A CN 108585017 A CN108585017 A CN 108585017A CN 201810821762 A CN201810821762 A CN 201810821762A CN 108585017 A CN108585017 A CN 108585017A
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- Prior art keywords
- oil
- water
- rare earth
- earth oxide
- ceria
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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
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Abstract
The invention discloses a kind of preparation methods of rare earth oxide ceria, include the following steps, surfactant selects, base oil is directly emulsified using 10 emulsifiers of OP, the more difficult dispersion in water of obtained oil emulsion, the emulsion that cannot stablize, this is because the HLB value required by the HLB value of emulsifier and the oil being emulsified is not suitable for, surfactant is used as using OP 10, the selection of oil phase and cosurfactant, use normal octane for oil phase, the stable emulsifiable base oil of 10 emulsifiers of OP, suitable water is added to be diluted, ensure the stability of whole solution.The present invention prepares ceria using OP 10 as surfactant, hydro-thermal method obtains product by improvement, it is at low cost, product purity height is obtained, gained ceria is in normal structure, and sample surfaces are coarse, sample size dispersion is more uniform, impurity content is few, is subsequently not necessarily to the processing of a large amount of chemicals, reduces pollution.
Description
Technical field
The present invention relates to rare earth oxide technical field more particularly to a kind of preparation sides of rare earth oxide ceria
Method.
Background technology
Rare earth oxide refers to 15 kinds of lanthanide oxides that period of element atom ordinal number is 57 to 71,
And scandium similar with lanthanide series chemical property（Sc）And yttrium（Y）The oxide of totally 17 kinds of elements, rare earth element oil,
The fields such as chemical industry, metallurgy, weaving, ceramics, glass, permanent-magnet material, which are obtained for, to be widely applied, and with advances in technology and is answered
It will be increasing with the value of the continuous breakthrough of technology, rare earth oxide.Existing ceria be all by water sedimentation method or
Prepared by person's combustion method, the impurity content for the product that a large amount of polluted gas is will produce in preparation process, and is obtained is high, needs
The processing of chemicals is subsequently carried out, cost is higher.
Invention content
Technical problems based on background technology, the present invention propose a kind of preparation side of rare earth oxide ceria
Method.
A kind of preparation method of rare earth oxide ceria proposed by the present invention, includes the following steps：
S1：Surfactant selects：Base oil is directly emulsified using OP-10 emulsifiers, obtained oil emulsion is more difficult in water
Dispersion is to get less than stable emulsion, this is because the HLB value required by the HLB value of emulsifier and the oil being emulsified is uncomfortable
It closes, using OP-10 as surfactant；
S2：The selection of oil phase and cosurfactant：Use normal octane for oil phase, the stable emulsifiable basis of OP-10 emulsifiers
Oil is added suitable water and is diluted, and ensures the stability of whole solution, n-butanol is cosurfactant, can change surface
The surface-active and hydrophile-lipophile balance of activating agent, participation form micella, the polarity of adjustment water and oil, and water-soluble alcohol can reduce
The polarity of water, oil-soluble alcohol can increase the polarity of oil, to influence the phase of system and the micro emulsion ingredient of phase property；
S3：Water phase selects：Use cerous nitrate for water phase, cerous nitrate is soluble easily in water, is dissolved in ethyl alcohol, acetone, is to produce in lotion
One of raw material of cerium salt, arranging in pairs or groups when in use above, urea mixed solution and oil solution are mixed；
S4：Reaction：Passing through different processing modes, is being reacted in input to reaction kettle, obtain product product；
S5：Wash separation product：By the product in reaction kettle through adequately washing, changed through superheated water, alcohol and the multiple village of distilled water
Washing is centrifugally separating to obtain the higher product of purity, and ideal ceria material is obtained after drying.
Preferably, the oily mixed solution content accounting of OP-10 is 13.6%-15%, the oil mixing of n-butanol in described S1, S2
Solution content accounting is 13.6%-15%, and the oily mixed solution content accounting of normal octane is 70%-72.7%.
Preferably, the 0.30-0.32mol/L cerous nitrates that content is 3g-3.5g are taken in the S3, the content of urea is
0.08-0.10g。
Preferably, the first processing mode in the S4 is to be placed in mixed liquor instead to clarifying with magnetic stirrer
It answers in kettle, is put into 110 DEG C of high-temperature baking case 24 hours.
Preferably, the second processing mode in the S4 is that mixed liquor is heated to 80 DEG C of holding 20min, is placed in reaction kettle
In, it is put into 150 DEG C -180 DEG C of high-temperature baking case 24 hours.
Having the beneficial effect that in the present invention：Ceria is prepared as surfactant using OP-10, hydro-thermal method is by changing
Into the washing separation product of nanoscale ceria is obtained, easy to operate, at low cost, obtained product purity is high, gained dioxy
It is in normal structure to change cerium, and sample surfaces are coarse, and sample size dispersion is more uniform, and size is：It is about 1 μm, thickness is about
600nm, impurity content is few, is subsequently not necessarily to the processing of a large amount of chemicals, reduces pollution.
Description of the drawings
Fig. 1 is a kind of preparation flow figure of the preparation method of rare earth oxide ceria proposed by the present invention.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
Referring to Fig.1, a kind of preparation method of rare earth oxide ceria, includes the following steps：
S1：Surfactant selects：Base oil is directly emulsified using OP-10 emulsifiers, obtained oil emulsion is more difficult in water
Dispersion is to get less than stable emulsion, this is because the HLB value required by the HLB value of emulsifier and the oil being emulsified is uncomfortable
It closes, using OP-10 as surfactant；
S2：The selection of oil phase and cosurfactant：Use normal octane for oil phase, the stable emulsifiable basis of OP-10 emulsifiers
Oil is added suitable water and is diluted, and ensures the stability of whole solution, n-butanol is cosurfactant, can change surface
The surface-active and hydrophile-lipophile balance of activating agent, participation form micella, the polarity of adjustment water and oil, and water-soluble alcohol can reduce
The polarity of water, oil-soluble alcohol can increase the polarity of oil, to influence the phase of system and the micro emulsion ingredient of phase property；
S3：Water phase selects：Use cerous nitrate for water phase, cerous nitrate is soluble easily in water, is dissolved in ethyl alcohol, acetone, is to produce in lotion
One of raw material of cerium salt, arranging in pairs or groups when in use above, urea mixed solution and oil solution are mixed；
S4：Reaction：Passing through different processing modes, is being reacted in input to reaction kettle, obtain product product；
S5：Wash separation product：By the product in reaction kettle through adequately washing, changed through superheated water, alcohol and the multiple village of distilled water
Washing is centrifugally separating to obtain the higher product of purity, and ideal ceria material is obtained after drying.
In the present invention, the oily mixed solution content accounting of OP-10 is 13.6%-15% in S1, S2, and the oil mixing of n-butanol is molten
Liquid hold-up accounting is 13.6%-15%, and the oily mixed solution content accounting of normal octane is 70%-72.7%, and it is 3g- that content is taken in S3
The content of the 0.30-0.32mol/L cerous nitrates of 3.5g, urea is 0.08-0.10g, and the first processing mode in S4 is to use magnetic force
Blender stirs to clarify, and mixed liquor is placed in reaction kettle, is put into 110 DEG C of high-temperature baking case 24 hours, and in S4
Two processing modes are that mixed liquor is heated to 80 DEG C of holding 20min, are placed in reaction kettle, are put into 150 DEG C -180 DEG C of high temperature and dry
24 hours in oven.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of rare earth oxide ceria, which is characterized in that include the following steps：
S1：Surfactant selects：Base oil is directly emulsified using OP-10 emulsifiers, obtained oil emulsion is more difficult in water
Dispersion is to get less than stable emulsion, this is because the HLB value required by the HLB value of emulsifier and the oil being emulsified is uncomfortable
It closes, using OP-10 as surfactant；
S2：The selection of oil phase and cosurfactant：Use normal octane for oil phase, the stable emulsifiable basis of OP-10 emulsifiers
Oil is added suitable water and is diluted, and ensures the stability of whole solution, n-butanol is cosurfactant, can change surface
The surface-active and hydrophile-lipophile balance of activating agent, participation form micella, the polarity of adjustment water and oil, and water-soluble alcohol can reduce
The polarity of water, oil-soluble alcohol can increase the polarity of oil, to influence the phase of system and the micro emulsion ingredient of phase property；
S3：Water phase selects：Use cerous nitrate for water phase, cerous nitrate is soluble easily in water, is dissolved in ethyl alcohol, acetone, is to produce in lotion
One of raw material of cerium salt, arranging in pairs or groups when in use above, urea mixed solution and oil solution are mixed；
S4：Reaction：Passing through different processing modes, is being reacted in input to reaction kettle, obtain product product；
S5：Wash separation product：By the product in reaction kettle through adequately washing, changed through superheated water, alcohol and the multiple village of distilled water
Washing is centrifugally separating to obtain the higher product of purity, and ideal ceria material is obtained after drying.
2. a kind of preparation method of rare earth oxide ceria according to claim 1, which is characterized in that the S1,
The oily mixed solution content accounting of OP-10 is 13.6%-15% in S2, and the oily mixed solution content accounting of n-butanol is 13.6%-
15%, the oily mixed solution content accounting of normal octane is 70%-72.7%.
3. a kind of preparation method of rare earth oxide ceria according to claim 1, which is characterized in that in the S3
The 0.30-0.32mol/L cerous nitrates that content is 3g-3.5g are taken, the content of urea is 0.08-0.10g.
4. a kind of preparation method of rare earth oxide ceria according to claim 1, which is characterized in that in the S4
The first processing mode be with magnetic stirrer to clarify, mixed liquor is placed in reaction kettle, be put into 110 DEG C high temperature dry
24 hours in oven.
5. a kind of preparation method of rare earth oxide ceria according to claim 1, which is characterized in that in the S4
Second processing mode be by mixed liquor be heated to 80 DEG C holding 20min, be placed in reaction kettle, be put into 150 DEG C -180 DEG C of height
24 hours in warm baking box.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891236A (en) * | 2010-07-16 | 2010-11-24 | 扬州大学 | Method for synthesizing monodisperse samarium-doped rare earth cerium oxide nanocrystal |
| CN102303882A (en) * | 2011-08-16 | 2012-01-04 | 桂林理工大学 | Method for preparing alpha-Al2O3 powder from microemulsion |
| CN102390852A (en) * | 2011-08-16 | 2012-03-28 | 桂林理工大学 | Method for preparing high-purity superfine Alpha-Al2O3 powder from microemulsion |
| CN103084174A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | Methanation catalyst for carbon oxide removing, preparation method and applications thereof |
| CN103084172A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | C2 fraction selective hydrogenation catalyst, preparation method and applications thereof |
| CN103084169A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | Unsaturated hydrocarbon hydrogenation catalyst, preparation method and applications thereof |
| CN103084173A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | C4 fraction selective hydrogenation catalyst, preparation method and applications thereof |
| 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 |
| CN103754922A (en) * | 2014-01-03 | 2014-04-30 | 东华大学 | Method for preparing oil-soluble nano cerium dioxide fluorescent powder by using CTAB (cetyltrimethyl ammonium bromide) as surfactant |
-
2018
- 2018-07-24 CN CN201810821762.6A patent/CN108585017A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891236A (en) * | 2010-07-16 | 2010-11-24 | 扬州大学 | Method for synthesizing monodisperse samarium-doped rare earth cerium oxide nanocrystal |
| CN102303882A (en) * | 2011-08-16 | 2012-01-04 | 桂林理工大学 | Method for preparing alpha-Al2O3 powder from microemulsion |
| CN102390852A (en) * | 2011-08-16 | 2012-03-28 | 桂林理工大学 | Method for preparing high-purity superfine Alpha-Al2O3 powder from microemulsion |
| CN103084174A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | Methanation catalyst for carbon oxide removing, preparation method and applications thereof |
| CN103084172A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | C2 fraction selective hydrogenation catalyst, preparation method and applications thereof |
| CN103084169A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | Unsaturated hydrocarbon hydrogenation catalyst, preparation method and applications thereof |
| CN103084173A (en) * | 2011-10-28 | 2013-05-08 | 中国石油化工股份有限公司 | C4 fraction selective hydrogenation catalyst, preparation method and applications thereof |
| 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 |
| CN103754922A (en) * | 2014-01-03 | 2014-04-30 | 东华大学 | Method for preparing oil-soluble nano cerium dioxide fluorescent powder by using CTAB (cetyltrimethyl ammonium bromide) as surfactant |
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Application publication date: 20180928 |