CN110817927A - Method for preparing light porous nano cerium oxide by combustion method - Google Patents
Method for preparing light porous nano cerium oxide by combustion method Download PDFInfo
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- CN110817927A CN110817927A CN201911362849.2A CN201911362849A CN110817927A CN 110817927 A CN110817927 A CN 110817927A CN 201911362849 A CN201911362849 A CN 201911362849A CN 110817927 A CN110817927 A CN 110817927A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C01—INORGANIC CHEMISTRY
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- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The invention provides a method for preparing nano cerium oxide, which comprises the following steps: (1) mixing a cerium source and a complexing agent, grinding, and adding a certain amount of water in the grinding process; (2) drying the mixture obtained after grinding in the step (1) at a certain temperature for a period of time; (3) and (3) calcining the dried mixture obtained in the step (2) to obtain the nano cerium oxide. The method has the advantages of simple process, environmental protection, low cost of raw materials, low equipment requirement, high production efficiency, good reproducibility and easy industrial production, and can regulate and control the color of the nano cerium oxide by controlling the proportion of the cerium source and the complexing agent. The method obtains the nano cerium oxide under the condition of no precipitator and surfactant, and the obtained light porous nano cerium oxide has the specific surface area of 49.5-55.5 m2·g‑1Light weight, multiple holes and adjustable color.
Description
Technical Field
The invention relates to a preparation method of a rare earth material, in particular to a preparation method of nano cerium oxide.
Background
Cerium oxide is a cheap and widely-used material, and is one of the most important elements in rare earth elements. The polishing material is mainly applied to polishing materials, electronic ceramics, fuel cell raw materials, hydrogen storage materials, gasoline catalysts, automobile exhaust purification, catalyst carriers and the like.
The existing methods for synthesizing cerium oxide include: precipitation, microemulsion, solvothermal, sol-gel, microwave-assisted heating, etc. The precipitation method has more influence factors on products in the reaction process, such as: the conditions of reaction temperature, concentration, roasting time, solution pH value and the like are difficult to control in the industrial production process; the methods such as the microemulsion method, the solvothermal method and the like have the defects of high raw material cost, high-temperature calcination of the obtained precursor, complex process, environmental pollution, easy agglomeration of the obtained product and the like, so that the method is limited in industrial production application.
Chinese patent application with publication number CN101182027A discloses a method for preparing nano cerium dioxide by an autocatalytic combustion method, which comprises the steps of taking cerium nitrate as a cerium source, taking a polyhydroxy organic matter as a combustion agent, preparing a solution according to the molar ratio of the polyhydroxy organic matter to cerous nitrate being 0.5: 1-3: 1, dropwise adding ammonia water to adjust the pH value of the solution to be 3-10, placing the complex sol in a forced air drying box, evaporating the solvent at the temperature of more than 150 ℃, and then carrying out autocatalytic combustion for 12 hours to obtain the nano cerium dioxide.
Chinese patent application publication No. CN1887718A discloses a method for preparing nano ceria by combustion, which comprises preparing an aqueous solution of malic acid by using cerium nitrate and malic acid as a cerium source and a complexing agent, respectively, adding cerium nitrate, stirring to dissolve, adjusting pH with ammonia water, stirring at room temperature, evaporating the solvent, drying, and heating for self-propagating combustion to obtain nano ceria.
As can be seen from the above several preparation methods, the existing methods for preparing high-quality cerium oxide have the disadvantages of complex reaction process, long reaction time, high cost, difficult treatment of waste gas and waste material, difficult application in mass production, etc.
Therefore, it is necessary to provide a synthesis method of nano cerium oxide with cheap raw materials, simple process, low energy consumption and high yield.
Disclosure of Invention
The invention aims to provide a method for preparing nano cerium oxide, which has the advantages of simple process, greenness, good reproducibility, high yield and the like, and the prepared nano cerium oxide is light and porous and has adjustable color.
The invention provides a method for preparing nano cerium oxide, which comprises the following steps:
(1) mixing a cerium source and a complexing agent, grinding, and adding a certain amount of water in the grinding process;
(2) drying the mixture obtained after grinding in the step (1) at a certain temperature for a period of time;
(3) and (3) calcining the dried mixture obtained in the step (2) to obtain the nano cerium oxide.
Further, the cerium source in the step (1) is one or a mixture of more than two of cerous nitrate hexahydrate, cerous acetate, cerous carbonate and cerous ammonium nitrate.
Further, the complexing agent in the step (1) is one or a mixture of more than two of glycerol, citric acid, ascorbic acid, urea and glucose.
Further, the mass ratio of the cerium source, the complexing agent and the water in the step (1) is 1:0.1: 0.6-1: 0.8: 1.
Further, the temperature in the step (2) is 30-70 ℃, and the time is 1-4 hours.
Further, the calcining temperature in the step (3) is 150-300 ℃, and the calcining time is 0.5-2 h.
The invention has the beneficial effects that: the method for preparing the nano cerium oxide by adopting the combustion method has the advantages of simple process, environmental protection, low cost of preparation raw materials, low equipment requirement, high production efficiency, good reproducibility, high yield and easy industrial productionThe method has the advantages that the nano cerium oxide is obtained under the condition of no precipitator or surfactant, and the specific surface area of the prepared nano cerium oxide is 49.5-55.5 m2·g-1Light weight, multiple holes and adjustable color.
Drawings
FIG. 1 is an XRD pattern and a product photograph of nano cerium oxide prepared in example 1.
FIG. 2 is an SEM photograph of nano-cerium oxide prepared in example 1.
FIG. 3 is an SEM photograph of nano-cerium oxide prepared in example 2.
FIG. 4 is an SEM photograph of nano-cerium oxide prepared in example 3.
FIG. 5 is an SEM photograph of nano-cerium oxide prepared in example 4.
FIG. 6 is an SEM photograph of nano-cerium oxide prepared in example 5.
Detailed Description
Example 1
Weighing 4.34g of cerous nitrate hexahydrate and 0.4g of citric acid at normal temperature, pouring into a mortar for grinding, and adding 2g of deionized water in the grinding process; uniformly grinding, pouring into a crucible, and drying in a forced air drying oven at 50 ℃ for 2 h; then the mixture is put into a muffle furnace to be calcined for 1.5h at 180 ℃ to obtain the light yellow porous nano cerium oxide.
Example 2
Weighing 2.8g of cerous nitrate hexahydrate and 0.2g of glycerol at normal temperature, pouring the weighed materials into a mortar for grinding, and adding 1.5g of deionized water in the grinding process; uniformly grinding, pouring into a crucible, and drying in a forced air drying oven at 40 ℃ for 2 h; then the mixture is put into a muffle furnace to be calcined for 0.5h at 180 ℃ to obtain the light yellow porous nano cerium oxide.
Example 3
At normal temperature, 6.6g of cerium acetate and 0.7g of glycerol are weighed and poured into a mortar for grinding, and 4g of deionized water is added in the grinding process; uniformly grinding, pouring into a crucible, and drying in a forced air drying oven at 50 ℃ for 2 h; then the mixture is put into a muffle furnace to be calcined for 2 hours at the temperature of 200 ℃ to obtain the light yellow porous nano cerium oxide.
Example 4
Weighing 8.22g of cerium acetate and 3.3g of glucose at normal temperature, pouring into a mortar for grinding, and adding 5g of deionized water in the grinding process; uniformly grinding, pouring into a crucible, and drying in a forced air drying oven at 50 ℃ for 3 h; then putting the mixture into a muffle furnace to calcine for 2 hours at the temperature of 200 ℃ to obtain the white light porous nano cerium oxide.
Example 5
Weighing 3.65g of cerium carbonate and 1.3g of urea at normal temperature, pouring into a mortar for grinding, and adding 2.5g of deionized water in the grinding process; uniformly grinding, pouring into a crucible, and drying in a forced air drying oven at 40 ℃ for 2 h; then putting the mixture into a muffle furnace to calcine for 1h at the temperature of 200 ℃ to obtain the white light porous nano cerium oxide.
The amounts of the products of examples 1 to 5 were 1.5, 1.0, 3.1, 4.0 and 1.3g, respectively, and the specific surface areas of the products were 54, 49, 53, 51.5 and 55.5m, respectively2·g-1The valence of cerium in cerium oxide is + 4.
Therefore, the method of the invention does not need ammonia water for adjustment, greatly shortens the reaction time, and can adjust and control the color of the cerium oxide by changing the amount of the complexing agent or the complexing agent.
Claims (7)
1. A method for preparing nano cerium oxide, comprising the steps of:
(1) mixing a cerium source and a complexing agent, grinding, and adding a certain amount of water in the grinding process;
(2) drying the mixture obtained after grinding in the step (1) at a certain temperature for a period of time;
(3) and (3) calcining the dried mixture obtained in the step (2) to obtain the nano cerium oxide.
2. The method of claim 1, wherein: the cerium source in the step (1) is one or a mixture of more than two of cerous nitrate hexahydrate, cerous acetate, cerous carbonate and cerous ammonium nitrate.
3. The method of claim 1, wherein: the complexing agent in the step (1) is one or a mixture of more than two of glycerol, citric acid, ascorbic acid, urea and glucose.
4. The method of claim 1, wherein: the mass ratio of the cerium source, the complexing agent and the water in the step (1) is 1:0.1: 0.6-1: 0.8: 1.
5. The method of claim 1, wherein: the temperature in the step (2) is 30-70 ℃, and the time is 1-4 h.
6. The method of claim 1, wherein: and (4) calcining at the temperature of 150-300 ℃ for 0.5-2 h.
7. Nano-cerium oxide obtainable by a process according to any one of claims 1 to 6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111370740A (en) * | 2020-03-11 | 2020-07-03 | 武汉工程大学 | Preparation method and application of gadolinium oxide doped cerium oxide nano composite material |
| CN112811457A (en) * | 2021-03-03 | 2021-05-18 | 甘肃农业大学 | Preparation method of loose porous nano cerium oxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887718A (en) * | 2006-08-01 | 2007-01-03 | 华东师范大学 | Combustion process of preparing nanometer CeO2 |
| CN101182027A (en) * | 2007-11-09 | 2008-05-21 | 浙江大学 | Method for preparing nano cerium dioxide by autocatalytic burning process |
| CN101475792A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation of coating type cerium oxide / silicon oxide compound abrasive |
| CN105085259A (en) * | 2015-08-25 | 2015-11-25 | 江西师范大学 | Preparation method of pentaerythritol unsaturated fatty acid ester |
-
2019
- 2019-12-26 CN CN201911362849.2A patent/CN110817927A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1887718A (en) * | 2006-08-01 | 2007-01-03 | 华东师范大学 | Combustion process of preparing nanometer CeO2 |
| CN101182027A (en) * | 2007-11-09 | 2008-05-21 | 浙江大学 | Method for preparing nano cerium dioxide by autocatalytic burning process |
| CN101475792A (en) * | 2009-01-20 | 2009-07-08 | 江苏工业学院 | Preparation of coating type cerium oxide / silicon oxide compound abrasive |
| CN105085259A (en) * | 2015-08-25 | 2015-11-25 | 江西师范大学 | Preparation method of pentaerythritol unsaturated fatty acid ester |
Non-Patent Citations (2)
| Title |
|---|
| ASHUTOSH SHARMA等: ""Synthesis of Nanocrystalline Cerium Oxide by both Solid and Liquid Processing Routes"", 《INTERNATIONAL CONFERENCE ON NANOTECHNOLOGY AND BIOSENSORS》 * |
| 李秀萍等: ""燃烧法快速合成轻质纳米氧化铈及其脱色性能"", 《中国粉体技术》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111370740A (en) * | 2020-03-11 | 2020-07-03 | 武汉工程大学 | Preparation method and application of gadolinium oxide doped cerium oxide nano composite material |
| CN111370740B (en) * | 2020-03-11 | 2021-08-13 | 武汉工程大学 | Preparation method and application of gadolinium oxide doped cerium oxide nano composite material |
| CN112811457A (en) * | 2021-03-03 | 2021-05-18 | 甘肃农业大学 | Preparation method of loose porous nano cerium oxide |
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Application publication date: 20200221 |