CN108862362B - Preparation method of micron-sized cerium oxide powder - Google Patents
Preparation method of micron-sized cerium oxide powder Download PDFInfo
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- CN108862362B CN108862362B CN201811084598.1A CN201811084598A CN108862362B CN 108862362 B CN108862362 B CN 108862362B CN 201811084598 A CN201811084598 A CN 201811084598A CN 108862362 B CN108862362 B CN 108862362B
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- C01—INORGANIC CHEMISTRY
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- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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Abstract
The invention discloses a preparation method of micron-sized cerium oxide powder, which comprises the following steps: adding a cerium-containing compound into an acidic solution to prepare a cerium salt solution; adding a cerium salt solution into a mixed solution of ethylene glycol and water, fully stirring, adding a surfactant, uniformly stirring and mixing, and adjusting the pH value to 8-10 by using ammonia water; and adding the solution into a hydrothermal kettle for hydrothermal reaction for 6-10h to generate a precipitate, and then filtering, drying and roasting to obtain the product. The invention takes the mixed solution of glycol and water as the solvent, and develops a simple and low-cost method for preparing the polyhydric alcohol of cerium oxide powder; the invention prevents the agglomeration of particles by adding a surface active agent (CTAB/CTAC), and performs modification and morphology control; the cerium oxide powder prepared by the invention has uniform particle distribution and controllable size, the size of the cerium oxide powder can be controlled within the range of 0.1-25 mu m, and the cerium oxide powder is suitable for large-scale production.
Description
Technical Field
The invention relates to the field of preparation of rare earth oxides, in particular to a preparation method of micron-sized cerium oxide powder.
Background
Cerium oxide is a light rare earth oxide which is inexpensive and has a wide range of applications, and has been used in the fields of catalysts, chemical mechanical polishing, electrochemistry, steel industry, and the like. As a catalyst, cerium oxide has been widely used in automobile exhaust gas purification catalysts; the polishing solution taking cerium oxide as polishing particles is widely applied to polishing of various precision glasses, polishing of semiconductor substrates, polishing of monocrystalline silicon wafers and polishing of intermediate dielectric layers of integrated circuits; in electrochemistry, cerium oxide-based composite oxide is used as electrolyte, and the cation current density can be high enough at medium temperature; in the steel industry, cerium oxide can be used as a trace additive in materials such as steel, cast iron, titanium, aluminum, nickel, tungsten, key and the like, so as to improve the thermal stability, corrosion resistance and the like of the alloy.
The performance of cerium oxide is closely related to the physicochemical properties thereof, the average particle diameter, the dispersion, the particle size, and the like. Therefore, it is necessary to select a proper method to prepare cerium oxide with a certain morphology and controllable size. The invention patent CN 16999282 proposes a preparation method of monodisperse spherical cerium oxide, the particle size of the obtained cerium oxide is single (about 300 nm), and the preparation process is complex; chinese patent CN101898787A discloses a method for synthesizing submicron cerium oxide by using cerium chloride solution as a raw material, the method takes cerium chloride solution as a cerium source, ammonium bicarbonate as a precipitator and a small amount of surfactant as a dispersing agent, the submicron cerium oxide with D50 of 0.1-0.2 mu m is synthesized by a liquid phase precipitation method, the size of the prepared cerium oxide is single, and the size can not be regulated and controlled according to requirements.
Disclosure of Invention
In view of the above problems in the prior art, it is an object of the present invention to provide a method for preparing cerium oxide powder having a controlled size and uniform particle size.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of micron-sized cerium oxide powder comprises the following steps:
(1) adding a cerium-containing compound into an acidic solution to prepare a cerium salt solution;
(2) adding the cerium salt solution into a mixed solution of ethylene glycol and water, fully stirring, adding a surfactant, and uniformly stirring and mixing;
(3) adjusting the pH value of the solution obtained in the step (2) to 8-10 by using ammonia water;
(4) adding the solution obtained in the step (3) into a hydrothermal kettle for hydrothermal reaction for 6-10h to generate a precipitate;
(5) filtering, drying and roasting to obtain a product;
wherein, the cerium-containing compound in the step (1) is at least one of cerium oxide and cerium carbonate;
the volume mixing ratio of the ethylene glycol and the water in the step (2) is 10 (1-3);
in the step (2), the surfactant is one of Cetyl Trimethyl Ammonium Bromide (CTAB) and Cetyl Trimethyl Ammonium Chloride (CTAC).
Further, the acidic solution in the step (1) is one of hydrochloric acid, nitric acid and sulfuric acid, and the concentration of the acidic solution is 0.6-2.0 mol/L.
Further, the concentration of the cerium salt solution in the step (1) is 0.5-1.5 mol/L.
Further, the final concentration of each component in the system in the step (2) is as follows: surfactant (b): 0.05-0.2mol/L, cerium salt: 0.1-0.5 mol/L.
Further, the ammonia-containing mass concentration of the ammonia water in the step (3) is 20-28%.
Further, the temperature of the hydrothermal reaction in the step (4) is 100-140 ℃.
Further, the drying temperature in the step (5) is 120-160 ℃, the drying time is 4-8h, the roasting temperature is 320-450 ℃, and the roasting time is 4-8 h.
Further, a method for preparing micron-sized cerium oxide powder, comprising the steps of:
adding cerium oxide into 0.6mol/L hydrochloric acid to prepare a cerium chloride salt solution with the concentration of 0.5 mol/L; adding a cerium salt solution into a mixed solution of ethylene glycol and water (the volume mixing ratio of the ethylene glycol to the water is 10:1), fully stirring, adding a surfactant (CTAB), stirring and mixing uniformly, wherein the concentration of the surfactant in a final system is 0.05mol/L, and the concentration of the cerium salt is 0.1 mol/L; adjusting the pH value of the solution to 9 by using ammonia water with the mass concentration of 28%; adding the solution into a hydrothermal kettle, carrying out hydrothermal reaction for 8 hours at 120 ℃, generating precipitates in the system, then filtering, and drying for 8 hours at 140 ℃; finally roasting for 4 hours at 450 ℃ to obtain cerium oxide powder.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
the invention takes the mixed solution of glycol and water as the solvent, and develops a simple and low-cost method for preparing the polyhydric alcohol of cerium oxide powder; the surfactant (CTAB/CTAC) used in the invention can be used as a stabilizer firstly, so that a reaction system is uniformly dispersed, agglomeration among particles is prevented, and on the other hand, the crystal face of cerium oxide can be modified and the morphology and size can be controlled, and the growth speed of different crystal faces can be controlled by different concentrations of the surfactant, so that the size of cerium oxide powder can be well controlled by the amount of the surfactant, and the size of the cerium oxide powder can be controlled within the range of 0.1-25 mu m; the cerium oxide powder prepared by the method has uniform particle distribution and controllable size, and is suitable for large-scale production.
Detailed Description
The present invention will be further described with reference to examples, but the present invention is not limited to these examples.
Example 1
Adding cerium oxide into 0.6mol/L hydrochloric acid to prepare a cerium chloride solution with the concentration of 0.5 mol/L; adding a cerium chloride solution into a mixed solution of ethylene glycol and water (the volume mixing ratio of the ethylene glycol to the water is 10:1), fully stirring, adding a surfactant CTAB, stirring and mixing uniformly, wherein the concentration of the surfactant in a final system is 0.05mol/L, and the concentration of cerium chloride is 0.1 mol/L; adjusting the pH value of the solution to 9 by using ammonia water with the mass concentration of 28%; adding the solution into a hydrothermal kettle, carrying out hydrothermal reaction for 8 hours at 120 ℃, generating precipitates in the system, then filtering, and drying for 8 hours at 140 ℃; finally roasting for 4 hours at 450 ℃ to obtain cerium oxide powder.
Example 2
Adding cerium oxide into a 1.0mol/L nitric acid solution to prepare a cerium nitrate solution with the concentration of 0.8 mol/L; adding a cerium nitrate solution into a mixed solution of ethylene glycol and water (the volume mixing ratio of the ethylene glycol to the water is 10:2), fully stirring, adding a surfactant CTAC, stirring and mixing uniformly, wherein the concentration of the surfactant in a final system is 0.1mol/L, and the concentration of cerium nitrate is 0.5 mol/L; adjusting the pH value of the solution to 8 by using ammonia water with the mass concentration of 20%; adding the solution into a hydrothermal kettle, carrying out hydrothermal reaction for 6h at 100 ℃, generating precipitates in the system, then filtering, and drying for 6h at 160 ℃; finally roasting for 6h at 400 ℃ to obtain cerium oxide powder.
Example 3
Adding cerium carbonate into 1.5mol/L sulfuric acid solution to prepare 1.0mol/L cerium sulfate solution; adding a cerium sulfate solution into a mixed solution of ethylene glycol and water (the volume mixing ratio of the ethylene glycol to the water is 10:3), fully stirring, adding a surfactant CTAB, stirring and mixing uniformly, wherein the concentration of the surfactant in a final system is 0.15mol/L, and the concentration of cerium sulfate is 0.25 mol/L; adjusting the pH value of the solution to 10 by using ammonia water with the mass concentration of 25%; adding the solution into a hydrothermal kettle, carrying out hydrothermal reaction for 10 hours at 140 ℃, generating precipitates in the system, then filtering, and drying for 4 hours at 130 ℃; finally roasting at 350 ℃ for 8h to obtain cerium oxide powder.
Example 4
Adding cerium carbonate into a nitric acid solution of 2.0mol/L to prepare a cerium nitrate solution with the concentration of 1.5 mol/L; adding a cerium nitrate solution into a mixed solution of ethylene glycol and water (the volume mixing ratio of the ethylene glycol to the water is 10:2), fully stirring, adding a surfactant CTAC, stirring and mixing uniformly, wherein the concentration of the surfactant in a final system is 0.2mol/L, and the concentration of cerium nitrate is 0.4 mol/L; adjusting the pH value of the solution to 9 by using ammonia water with the mass concentration of 26%; adding the solution into a hydrothermal kettle, carrying out hydrothermal reaction for 8 hours at 110 ℃, generating precipitates in the system, then filtering, and drying for 7 hours at 150 ℃; finally roasting at 320 ℃ for 7h to obtain cerium oxide powder.
Example 5
Cerium oxide was prepared in the same manner as in example 1, except that the concentration of the surfactant in the system after adding the surfactant CTAB was 0.1 mol/L.
Example 6
Cerium oxide was prepared in the same manner as in example 1, except that the concentration of the surfactant in the system after adding the surfactant CTAB was 0.15 mol/L.
Example 7
Cerium oxide was prepared in the same manner as in example 1, except that the concentration of the surfactant in the system after adding the surfactant CTAB was 0.2 mol/L.
Comparative example 1
Cerium oxide was prepared in the same manner as in example 1, except that no surfactant was added during the preparation.
Comparative example 2
Cerium oxide was prepared in the same manner as in example 1, except that the cerium salt solution was added to the ethylene glycol solution.
The following table (table 1) is a table of particle size data of cerium oxide powder prepared by the methods of the above examples and comparative examples.
TABLE 1 particle size data table of cerium oxide powder prepared by the methods of examples and comparative examples
| Experimental protocol | D10/μm | D50/μm | D90/μm |
| Example 1 | 23.01 | 24.08 | 25.47 |
| Example 2 | 16.37 | 17.64 | 18.85 |
| Example 3 | 11.09 | 12.49 | 13.73 |
| Example 4 | 3.77 | 4.50 | 5.67 |
| Example 5 | 11.18 | 11.99 | 12.86 |
| Example 6 | 1.01 | 1.27 | 1.49 |
| Example 7 | 0.09 | 0.10 | 0.12 |
| Comparative example 1 | 50.93 | 86.32 | 98.40 |
| Comparative example 2 | 0.03 | 0.05 | 0.06 |
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention; those skilled in the art can make various changes, modifications and alterations without departing from the scope of the invention, and all equivalent changes, modifications and alterations to the disclosed technology are equivalent embodiments of the present invention; meanwhile, any changes, modifications, and evolutions of the equivalent changes of the above embodiments according to the actual techniques of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (2)
1. A preparation method of micron-sized cerium oxide powder is characterized by comprising the following steps:
(1) adding a cerium-containing compound into an acidic solution to prepare a cerium salt solution;
(2) adding the cerium salt solution into a mixed solution of ethylene glycol and water, fully stirring, adding a surfactant, and uniformly stirring and mixing;
(3) adjusting the pH value of the solution obtained in the step (2) to 8-10 by using ammonia water;
(4) adding the solution obtained in the step (3) into a hydrothermal kettle for hydrothermal reaction for 6-10h to generate a precipitate;
(5) filtering, drying and roasting to obtain a product;
wherein, the cerium-containing compound in the step (1) is cerium oxide or cerium carbonate, and the concentration of the cerium salt solution is 0.5-1.5 mol/L; the acid solution in the step (1) is one of hydrochloric acid, nitric acid and sulfuric acid, and the concentration of the acid solution is 0.6-2.0 mol/L;
the volume mixing ratio of the ethylene glycol and the water in the step (2) is 10 (1-3);
the surfactant in the step (2) is one of cetyl trimethyl ammonium bromide and cetyl trimethyl ammonium chloride;
the final concentration of each component in the system in the step (2) is as follows: surfactant (b): 0.05-0.2mol/L, cerium salt: 0.1-0.5 mol/L;
the ammonia-containing mass concentration of the ammonia water in the step (3) is 20-28%;
the temperature of the hydrothermal reaction in the step (4) is 100-140 ℃;
in the step (5), the drying temperature is 120-160 ℃, the drying time is 4-8h, the roasting temperature is 450 ℃, and the roasting time is 4 h.
2. The method for preparing micron-sized cerium oxide powder according to claim 1, comprising the steps of: adding cerium oxide into 0.6mol/L hydrochloric acid to prepare a cerium chloride salt solution with the concentration of 0.5 mol/L; adding a cerium salt solution into a mixed solution of ethylene glycol and water, wherein the volume mixing ratio of the ethylene glycol to the water is 10:1, fully stirring, adding a surfactant CTAB, and uniformly stirring and mixing, wherein the concentration of the surfactant in a final system is 0.05mol/L, and the concentration of the cerium salt is 0.1 mol/L; adjusting the pH value of the solution to 9 by using ammonia water with the mass concentration of 28%; adding the solution into a hydrothermal kettle, carrying out hydrothermal reaction for 8 hours at 120 ℃, generating precipitates in the system, then filtering, and drying for 8 hours at 140 ℃; finally roasting for 4 hours at 450 ℃ to obtain cerium oxide powder.
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| CN109772290A (en) * | 2019-02-28 | 2019-05-21 | 江苏国盛新材料有限公司 | A kind of preparation method of cerium zirconium sosoloid |
| CN114604888B (en) * | 2020-12-09 | 2023-06-20 | 中国科学院大连化学物理研究所 | Method for preparing rod-like, cube-like and polyhedral cerium oxide |
| CN113830809B (en) * | 2021-10-27 | 2022-05-24 | 中国科学院青海盐湖研究所 | Preparation method of superfine alumina powder and product thereof |
| CN116409810A (en) * | 2023-05-24 | 2023-07-11 | 内蒙古中科镧铈稀材科技有限公司 | Preparation technology of large-particle cerium oxide |
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Effective date of registration: 20211102 Address after: 225400 group Zhouchen 90, Guangling Town, Taixing City, Taizhou City, Jiangsu Province Patentee after: JIANGSU CHINALCO NEW MATERIAL Co.,Ltd. Patentee after: GRIREM ADVANCED MATERIALS Co.,Ltd. Address before: 225400 Zhouchen group 90, Guangling Town, Taixing City, Taizhou City, Jiangsu Province (Jiangsu Guosheng New Material Co., Ltd.) Patentee before: JIANGSU CHINALCO NEW MATERIAL Co.,Ltd. |