CN110526272B - Micro-nano structure CeCO3Preparation process of OH - Google Patents
Micro-nano structure CeCO3Preparation process of OH Download PDFInfo
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- CN110526272B CN110526272B CN201910804777.6A CN201910804777A CN110526272B CN 110526272 B CN110526272 B CN 110526272B CN 201910804777 A CN201910804777 A CN 201910804777A CN 110526272 B CN110526272 B CN 110526272B
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/34—Spheres hollow
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
Abstract
The invention discloses a micro-nano structure CeCO3The preparation process of OH is characterized in that cerium salt is used as a precursor, and the CeCO with the almond type or hollow spherical structure is synthesized and prepared by a hydrothermal method3OH superfine powder material. The invention has CeCO3The OH has the characteristics of adjustable appearance, uniform size, good dispersibility and simple preparation process.
Description
Technical Field
The invention relates to a CeCO3OH preparation process, in particular to a micro-nano structure CeCO3And (3) a preparation process of OH.
Background
The cerium element is the rare earth element with the largest reserve in the earth crust, and the combination of the cerium element has a better functional application approach. Cerium carbonate hydroxide (CeCO)3OH) is an important functional material that not only provides unique optical properties related to its different structures and morphologies but also has novel electronic and chemical properties, and CeCO3The OH microstructure exhibits excellent electrochemical reversibility, an important feature for many applications, such as lithium ion batteries. In particular CeCO3Different structures and morphologies of OH have different properties and can be used for different applications, and CeCO with different morphologies3Preparation of CeO by simple thermal decomposition of OH under the condition of keeping the shape unchanged2If the nano CeCO can be realized3The controlled synthesis of the crystal structure and the appearance of OH can lead to more applications and new functional materials.
In recent years, different methods are adopted to synthesize the nano CeCO with different shapes3OH, such as self-assembly, sonochemistry, hydrothermal and microwave-assisted hydrothermal processes.Among all preparation methods, the hydrothermal method is considered to be an effective and economical preparation method due to its advantages of low synthesis temperature, high powder reactivity and diversified morphology control. In hydrothermal systems, most are about nanoco3The OH crystal synthesis is reported to use CO (NH)2)2Alkali and carbon source, and addition of surfactant or template to modulate CeCO3Nucleation and crystal growth of OH particles. This makes the process complicated and the raw material cost higher.
The preparation of CeCO is reported in the literature at home and abroad at present3The OH shapes mainly include needle, rod, triangle, etc., while the almond and spherical CeCO shapes3The preparation of OH has not been reported, but the morphology is to CeCO3OH and CeO obtained by decomposition2All have important influences on the performance of the catalyst.
In addition, China is a big rare earth country, and a large amount of rare earth resources are exported to the country after being mined and refined and are processed into rare earth products with high added values. The rare earth resource is used as an important resource, and the development of a preparation process of a high value-added rare earth product and the product are of great importance to China at present. And CeCO3OH as an important potential rare earth product, high quality CeCO3The research on the preparation process of OH is also of great significance to the comprehensive technical development and storage of the rare earth industry in China.
Therefore, the invention develops a micro-nano structure CeCO3Preparation and regulation process of OH and prepared CeCO3The OH has uniform appearance and size, good dispersibility, simple preparation process and good industrial application prospect.
Disclosure of Invention
The invention aims to provide a micro-nano structure CeCO3And (3) a preparation process of OH. The invention has CeCO3The OH has the characteristics of adjustable appearance, uniform size, good dispersibility and simple preparation process.
The technical scheme of the invention is as follows: micro-nano structure CeCO3The preparation process of OH is characterized in that cerium salt is used as a precursor, and the CeCO with the almond type or hollow spherical structure is synthesized and prepared by a hydrothermal method3OH superfine powder material.
The micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) dissolving cerium salt in distilled water, and stirring to form transparent solution to obtain product A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol, and stirring to obtain transparent solution B;
3) mixing product A and product B, stirring to form white milky slurry, and stirring for 0.1-1 hr to obtain product C;
4) sealing the product C in a high-pressure reaction kettle, pressurizing and heating, and naturally cooling to room temperature after the treatment is finished to obtain a product D;
5) washing the product D, filtering to obtain white precipitate, and drying to obtain CeCO3OH superfine powder material.
The micro-nano structure CeCO3The preparation process of OH comprises the step 1) that the cerium salt is Ce (NO)3)3·6H2O or CeCl3·7H2O。
The micro-nano structure CeCO3The preparation process of OH comprises the step 2) of preparing the ammonium bicarbonate with absolute ethyl alcohol according to a molar ratio of 3: 0.1-0.5.
The micro-nano structure CeCO3And (3) when the product A and the product B are mixed in the step 3), the molar ratio of the cerium salt in the product A to the ammonium bicarbonate in the product B is 0.1-1: 3.
The micro-nano structure CeCO3And (3) a preparation process of OH, wherein the white milky slurry in the step 3) is stirred by magnetic force.
The micro-nano structure CeCO3The preparation process of OH comprises the step 4) of heating and pressurizing treatment, wherein the pressure is 0.5-3MPa, the temperature is 80-180 ℃, and the treatment time is 12-48 h.
The micro-nano structure CeCO3The OH preparation process and the washing in the step 5) adopt distilled water and absolute ethyl alcohol to wash alternately.
The micro-nano structure CeCO3And 5) drying in vacuum at 30-40 ℃ for 10-15 h.
The micro-nano structure CeCO3Process for the preparation of OH, the CeCO3The average size of the OH superfine powder material is 0.2-1.5 mu m.
The invention has the advantages of
1. The invention can realize CeCO by the same process on the basis of regulating and controlling different process parameters3Regulating OH shape to prepare the almond or hollow spherical CeCO3OH ultrafine powder material, expanded CeCO3The shape and structure of the OH superfine powder material are kept unchanged after roasting, and the shape and structure of the material are filled with the almond-shaped hollow spherical CeCO3The technical blank of the preparation of the OH micro-nano structure has important significance for the development of rare earth materials and the development of rare earth products with high added values in China;
2. the CeCO prepared by the invention3The size of the OH superfine powder material is uniform and is between 0.2 and 1.5 mu m, and the dispersibility is good;
3. the invention adopts a hydrothermal method technology, has the characteristics and advantages of simple method, convenient operation and mass production.
Drawings
FIG. 1 shows the almond-shaped CeCO prepared by the present invention3SEM image of OH superfine powder material;
FIG. 2 shows the almond-shaped CeCO prepared by the present invention3XRD pattern of OH superfine powder material;
FIG. 3 shows the hollow spherical CeCO prepared by the present invention3SEM image of OH superfine powder material;
FIG. 4 shows the hollow spherical CeCO prepared by the present invention3XRD pattern of OH ultrafine powder material.
As can be seen from FIGS. 1 and 3, the almond-shaped and hollow spherical CeCO prepared by the present invention3The shape and the size of the OH superfine powder material are uniform, and the dispersibility is good. While the corresponding crystalline phases can be seen in fig. 2 and 4.
Detailed Description
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
Examples of the invention
Example 1: micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) adding Ce (NO)3)3·6H2Dissolving O in distilled water, and stirring to obtain transparent solution A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol (molar ratio of ammonium bicarbonate to anhydrous ethanol is 3:0.3), and stirring to obtain transparent solution B;
3) mixing product A and product B (Ce (NO) in product A)3)3·6H2The molar ratio of O to ammonium bicarbonate in the product B is 0.3:3), stirring to form white milky serous fluid, and then continuing stirring the serous fluid by magnetic force for 0.5h to obtain a product C;
4) sealing the product C in a high-pressure reaction kettle, treating at 130 deg.C under 2MPa for 30h, and naturally cooling to room temperature to obtain product D;
5) washing product D with distilled water and anhydrous ethanol alternately, filtering to obtain white precipitate, and vacuum drying at 35 deg.C for 12 hr to obtain CeCO3OH superfine powder material.
The CeCO obtained in this example3The shape of the OH superfine powder material is almond.
Example 2: micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) adding Ce (NO)3)3·6H2Dissolving O in distilled water, and stirring to obtain transparent solution A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol (molar ratio of ammonium bicarbonate to anhydrous ethanol is 3:0.1), and stirring to obtain transparent solution B;
3) mixing product A and product B (Ce (NO) in product A)3)3·6H2The molar ratio of O to ammonium bicarbonate in the product B is 0.1:3), stirring to form white milky serous fluid, and then continuing stirring the serous fluid by magnetic stirring for 0.1h to obtain a product C;
4) sealing the product C in a high-pressure reaction kettle, treating at 80 deg.C under 0.5MPa for 12 hr, and naturally cooling to room temperature to obtain product D;
5) washing product D with distilled water and anhydrous ethanol alternately, filtering to obtain white precipitate, and vacuum drying at 30 deg.C for 10 hr to obtain CeCO3OH superfine powder material.
The CeCO obtained in this example3The shape of the OH superfine powder material is almond.
Example 3: micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) reacting CeCl3·7H2Dissolving O in distilled water, and stirring to obtain transparent solution A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol (molar ratio of ammonium bicarbonate to anhydrous ethanol is 3:0.5), and stirring to obtain transparent solution B;
3) mixing product A and product B (CeCl in product A)3·7H2The molar ratio of O to ammonium bicarbonate in the product B is 0.5:3), stirring to form white milky slurry, and then continuing to stir the slurry for 1h by magnetic stirring to obtain a product C;
4) sealing the product C in a high-pressure reaction kettle, treating at 3MPa and 180 ℃ for 48h, and naturally cooling to room temperature after the treatment is finished to obtain a product D;
5) washing product D with distilled water and anhydrous ethanol alternately, filtering to obtain white precipitate, and vacuum drying at 40 deg.C for 15 hr to obtain CeCO3OH superfine powder material.
The CeCO obtained in this example3The shape of the OH superfine powder material is almond.
Example 4: micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) adding Ce (NO)3)3·6H2Dissolving O in distilled water, and stirring to obtain transparent solution A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol (molar ratio of ammonium bicarbonate to anhydrous ethanol is 3:0.3), and stirring to obtain transparent solution B;
3) mixing product A and product B (Ce (NO) in product A)3)3·6H2The molar ratio of O to ammonium bicarbonate in the product B is0.9:3) stirring until white milky serous fluid is formed, and then continuing stirring the serous fluid by magnetic force for 0.5h to obtain a product C;
4) sealing the product C in a high-pressure reaction kettle, treating at 130 deg.C under 2MPa for 30h, and naturally cooling to room temperature to obtain product D;
5) washing product D with distilled water and anhydrous ethanol alternately, filtering to obtain white precipitate, and vacuum drying at 35 deg.C for 12 hr to obtain CeCO3OH superfine powder material.
The CeCO obtained in this example3The shape of the OH superfine powder material is hollow spherical.
Example 5: micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) adding Ce (NO)3)3·6H2Dissolving O in distilled water, and stirring to obtain transparent solution A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol (molar ratio of ammonium bicarbonate to anhydrous ethanol is 3:0.1), and stirring to obtain transparent solution B;
3) mixing product A and product B (Ce (NO) in product A)3)3·6H2The molar ratio of O to ammonium bicarbonate in the product B is 0.8:3), stirring to form white milky serous fluid, and then continuing stirring the serous fluid by magnetic stirring for 0.1h to obtain a product C;
4) sealing the product C in a high-pressure reaction kettle, treating at 80 deg.C under 0.5MPa for 12 hr, and naturally cooling to room temperature to obtain product D;
5) washing product D with distilled water and anhydrous ethanol alternately, filtering to obtain white precipitate, and vacuum drying at 30 deg.C for 10 hr to obtain CeCO3OH superfine powder material.
The CeCO obtained in this example3The shape of the OH superfine powder material is hollow spherical.
Example 6: micro-nano structure CeCO3The preparation process of OH comprises the following specific steps:
1) reacting CeCl3·7H2Dissolving O in distilled water, and stirring to obtain transparent solution A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol (molar ratio of ammonium bicarbonate to anhydrous ethanol is 3:0.5), and stirring to obtain transparent solution B;
3) mixing product A and product B (CeCl in product A)3·7H2The molar ratio of O to ammonium bicarbonate in the product B is 1:3), stirring to form white milky slurry, and then continuing stirring the slurry by magnetic force for 1h to obtain a product C;
4) sealing the product C in a high-pressure reaction kettle, treating at 3MPa and 180 ℃ for 48h, and naturally cooling to room temperature after the treatment is finished to obtain a product D;
5) washing product D with distilled water and anhydrous ethanol alternately, filtering to obtain white precipitate, and vacuum drying at 40 deg.C for 15 hr to obtain CeCO3OH superfine powder material.
The CeCO obtained in this example3The shape of the OH superfine powder material is hollow spherical.
The above description is only for the purpose of illustrating the present invention and the appended claims, and the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (6)
1. Micro-nano structure CeCO3The preparation process of OH is characterized by comprising the following steps: adopts cerium salt as a precursor, and prepares the almond-type or hollow spherical CeCO by hydrothermal synthesis3OH superfine powder material; the method comprises the following specific steps:
1) dissolving cerium salt in distilled water, and stirring to form transparent solution to obtain product A;
2) dissolving ammonium bicarbonate in distilled water, adding anhydrous ethanol, and stirring to obtain transparent solution B; the molar ratio of the ammonium bicarbonate to the absolute ethyl alcohol is 3: 0.1-0.5;
3) mixing product A and product B, stirring to form white milky slurry, and stirring for 0.1-1 hr to obtain product C; when the product A and the product B are mixed, the molar ratio of the cerium salt in the product A to the ammonium bicarbonate in the product B is 0.1-1: 3;
4) sealing the product C in a high-pressure reaction kettle, pressurizing and heating, and naturally cooling to room temperature after the treatment is finished to obtain a product D; the pressure is 0.5-3MPa, the temperature is 80-180 ℃, and the treatment time is 12-48 h;
5) washing the product D, filtering to obtain white precipitate, and drying to obtain CeCO3OH superfine powder material.
2. Micro-nano structure CeCO according to claim 13The preparation process of OH is characterized by comprising the following steps: step 1) the cerium salt is Ce (NO)3)3·6H2O or CeCl3·7H2O。
3. Micro-nano structure CeCO according to claim 13The preparation process of OH is characterized by comprising the following steps: and 3) magnetically stirring the white milky slurry.
4. Micro-nano structure CeCO according to claim 13The preparation process of OH is characterized by comprising the following steps: and step 5), washing is alternately washing by using distilled water and absolute ethyl alcohol.
5. Micro-nano structure CeCO according to claim 13The preparation process of OH is characterized by comprising the following steps: and 5) drying in vacuum at 30-40 ℃ for 10-15 h.
6. Micro-nano structure CeCO according to claim 13The preparation process of OH is characterized by comprising the following steps: the CeCO3The average size of the OH superfine powder material is 0.2-1.5 mu m.
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| CN113332976B (en) * | 2021-05-18 | 2022-06-07 | 贵州大学 | CeCO3OH nanosphere wrapped MnCO3Preparation method and application of microsphere composite material |
| CN115490257B (en) * | 2022-08-31 | 2023-06-27 | 贵州大学 | N-doped submicron spherical Y 2 O 3 Is prepared by the preparation method of (2) |
| 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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| CN103172101A (en) * | 2012-12-13 | 2013-06-26 | 浙江海洋学院 | Preparation method of alkali-type cerous carbonate |
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