阅读说明：本技术 用燃烧法制备质轻多孔的纳米氧化铈 (Method for preparing light porous nano cerium oxide by combustion method ) 是由 钟声亮 李盛凯 宁海金 徐先进 刘汉锋 廖道发 于 2019-12-26 设计创作，主要内容包括：本发明提供了一种制备纳米氧化铈的方法,该方法包括以下步骤：(1)将铈源与络合剂混合,研磨,在研磨的过程中加入一定量的水；(2)将步骤(1)研磨后得到的混合物在一定温度下干燥一段时间；(3)将步骤(2)干燥后的混合物煅烧,得到纳米氧化铈。该方法工艺简单、绿色环保、制备原料成本低、设备要求低、生产效率高、重现性好、易于工业生产,并可以通过控制铈源与络合剂的比例,调控纳米氧化铈的颜色。本发明在无沉淀剂和表面活性剂的情况下获得纳米氧化铈,得到质轻多孔的纳米氧化铈比表面积在49.5～55.5m<Sup>2</Sup>·g<Sup>-1</Sup>,质轻多孔、颜色可调。(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 m 2 ·g ‑1 Light weight, multiple holes and adjustable color.)

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.

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