CN110526272A - A kind of micro-nano structure CeCO3The preparation process of OH - Google Patents
A kind of micro-nano structure CeCO3The preparation process of OH Download PDFInfo
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- CN110526272A CN110526272A CN201910804777.6A CN201910804777A CN110526272A CN 110526272 A CN110526272 A CN 110526272A CN 201910804777 A CN201910804777 A CN 201910804777A CN 110526272 A CN110526272 A CN 110526272A
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- 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
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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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/34—Spheres hollow
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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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a kind of micro-nano structure CeCO3The preparation process of OH is that the CeCO of almond type or hollow sphere structure is synthetically prepared by hydro-thermal method using cerium salt as presoma3OH superfine powdery material.The present invention has CeCO3OH pattern is adjustable, of uniform size, good dispersion, the simple feature of preparation process.
Description
Technical field
The present invention relates to a kind of CeCO3The preparation process of OH, especially a kind of micro-nano structure CeCO3The preparation process of OH.
Background technique
Ce elements are the rare earth elements that reserves are most in the earth's crust, and the chemical combination of Ce elements has preferable functionalized application way
Diameter.Cerous carbonate hydroxide (CeCO3It OH is) a kind of important functional material, it, which is provided not only, is different from structure and pattern
Relevant unique optical properties and there is novel electronic property and chemical property, and CeCO3OH microstructure is excellent in
Electrochemical reversibility, this be it is many application (such as lithium ion battery) important feature.Specifically CeCO3OH different structures
There is different performances to can be used for different applications, and the CeCO of different-shape with pattern3OH can be by simply thermally decomposing guarantor
Hold pattern it is constant in the case where prepare CeO2If nano Ce CO may be implemented3The control of OH crystal structure and pattern synthesizes, just
It is likely to occur more applications and new functional material.
In recent years, the nano Ce CO of different-shape has been synthesized using different methods3OH, such as self assembly, sonochemistry, water
Hot and microwave-assisted hydro-thermal method.In all preparation methods, hydro-thermal method is because its synthesis temperature is low, high powdered reaction and diversification
The advantages of pattern controls is considered as a kind of preparation method of efficient and cost-effective.It is most of about nanometer in hydrothermal system
CeCO3The report of OH Opacity in lens is using CO (NH2)2Alkali and carbon source, and surfactant or template are added to adjust
CeCO3It is prepared by the nucleation of OH particle and crystal growth.This makes process complicated, and the cost of raw material is higher.
Report preparation CeCO in domestic and foreign literature at present3The pattern of OH mainly has needle-shaped, rodlike, triangle etc., and apricot
Benevolence shape and spherical shape CeCO3The preparation of OH has not been reported, and pattern is to CeCO3OH, and to the CeO that decomposition obtains2Performance it is equal
There is important influence.
In addition, China is rare earth big country, a large amount of rare earth resources export to after exploitation, refinement and are dealt into country, added
Work becomes high added value rare-earth products.Rare earth resources develop the preparation process of high added value rare-earth products as important resource
It is most important to current China with product.And CeCO3OH is as a kind of important potential rare-earth products of tool, high-quality
CeCO3The Study on Preparation of OH is also of great significance to the comprehensive technological development of China's rare-earth trade and deposit.
Therefore, the present invention develops a kind of micro-nano structure CeCO3The technique of preparation and the regulation of OH, prepared CeCO3OH
Pattern, of uniform size, dispersion performance is good, and preparation process simply has preferable prospects for commercial application.
Summary of the invention
The object of the present invention is to provide a kind of micro-nano structure CeCO3The preparation process of OH.The present invention has CeCO3OH shape
Looks are adjustable, of uniform size, good dispersion, the simple feature of preparation process.
A kind of technical solution of the present invention: micro-nano structure CeCO3The preparation process of OH is led to using cerium salt as presoma
Cross the CeCO that hydro-thermal method is synthetically prepared almond type or hollow sphere structure3OH superfine powdery material.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the specific steps are as follows:
1) cerium salt is dissolved in distilled water, stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and dehydrated alcohol is added, stirring obtains B product to clear solution is formed；
3) A product and B product are mixed, stirring then proceedes to stirring slurry 0.1-1h, obtain C to white " milky " slurries are formed
Product；
4) C product are put into autoclave sealing, and pressurized, heated is handled, after treatment cooled to room temperature obtains D
Product；
5) it will be filtered after the washing of D product, and white depositions be obtained, up to CeCO after white depositions are dried3OH superfine powder
Material.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the step 1) cerium salt are Ce (NO3)3·6H2O or
CeCl3·7H2O。
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the molar ratio of step 2) ammonium hydrogen carbonate and dehydrated alcohol
For 3:0.1-0.5.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, when step 3) the A product and B product mix, in A product cerium salt with
The molar ratio of ammonium hydrogen carbonate is 0.1-1:3 in B product.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, step 3) the white " milky " slurries use magnetic agitation.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, when step 4) the heating pressurized treatments, pressure 0.5-
3MPa, temperature are 80-180 DEG C, handle time 12-48h.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the step 5) washing is using distilled water and dehydrated alcohol
Alternately wash.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, step 5) is described dry using vacuum drying, and drying temperature is
30-40 DEG C, time 10-15h.
Micro-nano structure CeCO above-mentioned3The preparation process of OH, the CeCO3The average-size of OH superfine powdery material is
0.2-1.5μm。
Beneficial effects of the present invention
1, CeCO can be realized on the basis of regulating and controlling different technological parameters by same set of technique in the present invention3OH shape
The CeCO of almond type or hollow sphere structure is prepared in the adjusting of looks3OH superfine powdery material, extends CeCO3OH superfine powder
Material morphology structure type, pattern remains unchanged after roasting, has filled up amygdaloidal, hollow sphere CeCO3The preparation of OH micro-nano structure
Technological gap, to China's rare earth material exploitation and high added value rare-earth products exploitation all have significance；
2, CeCO produced by the present invention3OH superfine powdery material is of uniform size, and between 0.2-1.5 μm, dispersion performance is good；
3, the present invention uses hydro-thermal law technology, and method is simple, easy to operate, has the characteristics that mass production and advantage.
Detailed description of the invention
Attached drawing 1 is amygdaloidal CeCO produced by the present invention3The SEM of OH superfine powdery material schemes；
Attached drawing 2 is amygdaloidal CeCO produced by the present invention3The XRD diagram of OH superfine powdery material；
Attached drawing 3 is the CeCO of hollow sphere produced by the present invention3The SEM of OH superfine powdery material schemes；
Attached drawing 4 is the CeCO of hollow sphere produced by the present invention3The XRD diagram of OH superfine powdery material.
It can be seen that produced by the present invention amygdaloidal and hollow sphere CeCO from Fig. 1 and Fig. 33OH superfine powdery material
Shape and size more uniformly, dispersibility preferably.And its corresponding crystal phase can be seen that by Fig. 2 and Fig. 4.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1: micro-nano structure CeCO3The preparation process of OH, the specific steps are as follows:
1) by Ce (NO3)3·6H2O is dissolved in distilled water, and stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and be added dehydrated alcohol (molar ratio of ammonium hydrogen carbonate and dehydrated alcohol be 3:
0.3), stirring obtains B product to clear solution is formed；
3) A product and B product are mixed to (Ce (NO in A product3)3·6H2The molar ratio of O and ammonium hydrogen carbonate in B product is 0.3:3), it stirs
It mixes to white " milky " slurries are formed, then proceedes to magnetic agitation stirring slurry 0.5h, obtain C product；
4) C product are put into autoclave sealing, handle 30h at 2MPa, 130 DEG C, after treatment naturally cools to
Room temperature obtains D product；
5) it is filtered after alternately washing D product distilled water and dehydrated alcohol, white depositions is obtained, by white depositions 35
DEG C vacuum drying 12h to get CeCO3OH superfine powdery material.
CeCO made from the present embodiment3The pattern of OH superfine powdery material is amygdaloidal.
Embodiment 2: micro-nano structure CeCO3The preparation process of OH, the specific steps are as follows:
1) by Ce (NO3)3·6H2O is dissolved in distilled water, and stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and be added dehydrated alcohol (molar ratio of ammonium hydrogen carbonate and dehydrated alcohol be 3:
0.1), stirring obtains B product to clear solution is formed；
3) A product and B product are mixed to (Ce (NO in A product3)3·6H2The molar ratio of O and ammonium hydrogen carbonate in B product is 0.1:3), it stirs
It mixes to white " milky " slurries are formed, then proceedes to magnetic agitation stirring slurry 0.1h, obtain C product；
4) C product are put into autoclave sealing, handle 12h at 0.5MPa, 80 DEG C, after treatment naturally cools to
Room temperature obtains D product；
5) it is filtered after alternately washing D product distilled water and dehydrated alcohol, white depositions is obtained, by white depositions 30
DEG C vacuum drying 10h to get CeCO3OH superfine powdery material.
CeCO made from the present embodiment3The pattern of OH superfine powdery material is amygdaloidal.
Embodiment 3: micro-nano structure CeCO3The preparation process of OH, the specific steps are as follows:
1) by CeCl3·7H2O is dissolved in distilled water, and stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and be added dehydrated alcohol (molar ratio of ammonium hydrogen carbonate and dehydrated alcohol be 3:
0.5), stirring obtains B product to clear solution is formed；
3) A product and B product are mixed to (CeCl in A product3·7H2The molar ratio of O and ammonium hydrogen carbonate in B product is 0.5:3), stirring
To white " milky " slurries are formed, magnetic agitation stirring slurry 1h is then proceeded to, C product are obtained；
4) C product are put into autoclave sealing, handle 48h at 3MPa, 180 DEG C, after treatment naturally cools to
Room temperature obtains D product；
5) it is filtered after alternately washing D product distilled water and dehydrated alcohol, white depositions is obtained, by white depositions 40
DEG C vacuum drying 15h to get CeCO3OH superfine powdery material.
CeCO made from the present embodiment3The pattern of OH superfine powdery material is amygdaloidal.
Embodiment 4: micro-nano structure CeCO3The preparation process of OH, the specific steps are as follows:
1) by Ce (NO3)3·6H2O is dissolved in distilled water, and stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and be added dehydrated alcohol (molar ratio of ammonium hydrogen carbonate and dehydrated alcohol be 3:
0.3), stirring obtains B product to clear solution is formed；
3) A product and B product are mixed to (Ce (NO in A product3)3·6H2The molar ratio of O and ammonium hydrogen carbonate in B product is 0.9:3), it stirs
It mixes to white " milky " slurries are formed, then proceedes to magnetic agitation stirring slurry 0.5h, obtain C product；
4) C product are put into autoclave sealing, handle 30h at 2MPa, 130 DEG C, after treatment naturally cools to
Room temperature obtains D product；
5) it is filtered after alternately washing D product distilled water and dehydrated alcohol, white depositions is obtained, by white depositions 35
DEG C vacuum drying 12h to get CeCO3OH superfine powdery material.
CeCO made from the present embodiment3The pattern of OH superfine powdery material is hollow sphere.
Embodiment 5: micro-nano structure CeCO3The preparation process of OH, the specific steps are as follows:
1) by Ce (NO3)3·6H2O is dissolved in distilled water, and stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and be added dehydrated alcohol (molar ratio of ammonium hydrogen carbonate and dehydrated alcohol be 3:
0.1), stirring obtains B product to clear solution is formed；
3) A product and B product are mixed to (Ce (NO in A product3)3·6H2The molar ratio of O and ammonium hydrogen carbonate in B product is 0.8:3), it stirs
It mixes to white " milky " slurries are formed, then proceedes to magnetic agitation stirring slurry 0.1h, obtain C product；
4) C product are put into autoclave sealing, handle 12h at 0.5MPa, 80 DEG C, after treatment naturally cools to
Room temperature obtains D product；
5) it is filtered after alternately washing D product distilled water and dehydrated alcohol, white depositions is obtained, by white depositions 30
DEG C vacuum drying 10h to get CeCO3OH superfine powdery material.
CeCO made from the present embodiment3The pattern of OH superfine powdery material is hollow sphere.
Embodiment 6: micro-nano structure CeCO3The preparation process of OH, the specific steps are as follows:
1) by CeCl3·7H2O is dissolved in distilled water, and stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and be added dehydrated alcohol (molar ratio of ammonium hydrogen carbonate and dehydrated alcohol be 3:
0.5), stirring obtains B product to clear solution is formed；
3) A product and B product are mixed to (CeCl in A product3·7H2The molar ratio of O and ammonium hydrogen carbonate in B product is 1:3), stirring is extremely
White " milky " slurries are formed, magnetic agitation stirring slurry 1h is then proceeded to, obtains C product；
4) C product are put into autoclave sealing, handle 48h at 3MPa, 180 DEG C, after treatment naturally cools to
Room temperature obtains D product；
5) it is filtered after alternately washing D product distilled water and dehydrated alcohol, white depositions is obtained, by white depositions 40
DEG C vacuum drying 15h to get CeCO3OH superfine powdery material.
CeCO made from the present embodiment3The pattern of OH superfine powdery material is hollow sphere.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not
It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention
The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the invention protection scope it
It is interior.
Claims (10)
1. a kind of micro-nano structure CeCO3The preparation process of OH, it is characterised in that: be to be closed using cerium salt as presoma by hydro-thermal method
At the CeCO for preparing almond type or hollow sphere structure3OH superfine powdery material.
2. micro-nano structure CeCO according to claim 13The preparation process of OH, which is characterized in that specific step is as follows:
1) cerium salt is dissolved in distilled water, stirring obtains A product to clear solution is formed；
2) ammonium hydrogen carbonate is dissolved in distilled water, and dehydrated alcohol is added, stirring obtains B product to clear solution is formed；
3) A product and B product are mixed, stirring then proceedes to stirring slurry 0.1-1h, obtain C product to white " milky " slurries are formed；
4) C product are put into autoclave sealing, and pressurized, heated is handled, after treatment cooled to room temperature obtains D product；
5) it will be filtered after the washing of D product, and white depositions be obtained, up to CeCO after white depositions are dried3OH superfine powdery material.
3. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: cerium salt described in step 1) is
Ce(NO3)3·6H2O or CeCl3·7H2O。
4. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: bicarbonate described in step 2
The molar ratio of ammonium and dehydrated alcohol is 3:0.1-0.5.
5. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: A product and B described in step 3)
When product mix, cerium salt and the molar ratio of ammonium hydrogen carbonate in B product are 0.1-1:3 in A product.
6. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: the cream of white described in step 3)
Shape slurries use magnetic agitation.
7. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: heating described in step 4) adds
When pressure processing, pressure 0.5-3MPa, temperature are 80-180 DEG C, handle time 12-48h.
8. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: washing described in step 5) is
It is alternately washed using distilled water and dehydrated alcohol.
9. micro-nano structure CeCO according to claim 23The preparation process of OH, it is characterised in that: drying described in step 5) is adopted
With vacuum drying, drying temperature is 30-40 DEG C, time 10-15h.
10. micro-nano structure CeCO according to claim 1 or 23The preparation process of OH, it is characterised in that: the CeCO3OH
The average-size of superfine powdery material is 0.2-1.5 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113332976A (en) * | 2021-05-18 | 2021-09-03 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
| CN115490257A (en) * | 2022-08-31 | 2022-12-20 | 贵州大学 | N-doped submicron spherical Y 2 O 3 Preparation method of (1) |
| CN116741549A (en) * | 2023-08-14 | 2023-09-12 | 新乡学院 | Ce-based composite electrode material and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115490257A (en) * | 2022-08-31 | 2022-12-20 | 贵州大学 | N-doped submicron spherical Y 2 O 3 Preparation method of (1) |
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| CN116741549B (en) * | 2023-08-14 | 2023-10-24 | 新乡学院 | Ce-based composite electrode material and preparation method thereof |
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