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Method for preparing mesoporous cerium oxide powder by using sol-gel method

A cerium oxide and mesoporous technology, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems affecting popularization and application, long reaction time, etc., and achieve the effect of low cost, simple and easy to control process

Inactive Publication Date: 2015-04-29
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But its synthetic process needs crystallization 5 days under pH value 11 environment, and reaction time is longer, has influenced the further popularization and application of this method (J.H. Zhang, Y.Q. Yang, J.M. Shen, J.A. Wang. Mesostrcutured CeO 2 and Pd / CeO 2 nanophases: Templated synthesis, crystalline structure and catalysis properties. Journal of Molecular Catalysis A: Chemical, 2005, 237 (1-2): 182-190)

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  • Method for preparing mesoporous cerium oxide powder by using sol-gel method
  • Method for preparing mesoporous cerium oxide powder by using sol-gel method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Step 1: Prepare Ingredients

[0032] 3.91g of analytically pure Ce(NO 3 ) 3 ·6H 2 O was dissolved in deionized water to obtain Ce(NO 3 ) 3 Solution; 0.98g analytical pure citric acid is dissolved in deionized water to obtain a concentration of citric acid solution of 0.17mol / l; ethanol, acetic acid, butanediol are formulated into 17.14g mixed solution in a 35:2.5:1 molar ratio;

[0033] Step 2: Preparation

[0034] Mix the solution with Ce(NO 3 ) 3 Mix and stir the solution evenly, then add citric acid solution, stir in a water bath at 65°C for 4 hours to mix evenly, and then place it in a drying oven at 55°C for 4.5 hours to obtain a gel; place the obtained gel in a muffle furnace, First heat to 180°C for 30min, then heat to 400°C at a heating rate of 10°C / min and hold for 1.5h, then cool to room temperature with the furnace; 1.50g of light yellow mesoporous cerium oxide powder is obtained.

[0035] The whole preparation process takes about 11 hours, which gre...

Embodiment 2

[0038] Step 1: Prepare Ingredients

[0039] 7.45g of analytically pure Ce(NO 3 ) 3 ·6H 2 O was dissolved in deionized water to obtain Ce(NO 3 ) 3 Solution; 1.70g analytical pure citric acid is dissolved in deionized water to obtain a concentration of citric acid solution of 0.221mol / l; ethanol, acetic acid, butanediol are formulated into 32.48g mixed solution in a mol ratio of 42:3:1;

[0040] Step 2: Preparation

[0041] Mix the solution with Ce(NO 3 ) 3 Mix and stir the solution evenly, then add citric acid solution, stir in a water bath at 70°C for 3 hours to mix evenly, and then place it in a drying oven at 60°C for 4 hours to obtain a gel; put the obtained gel in a muffle furnace, first Heat to 200°C for 20min, then heat to 415°C at a heating rate of 10°C / min for 1h, and cool to room temperature with the furnace; 2.90g of light yellow mesoporous cerium oxide powder is obtained.

[0042] The whole preparation process takes about 9 hours, which greatly shortens the...

Embodiment 3

[0044] Step 1: Prepare Ingredients

[0045] 15.62g of analytically pure Ce(NO 3 ) 3 ·6H 2 O was dissolved in deionized water to obtain Ce(NO 3 ) 3 Solution; 2.58g analytical pure citric acid is dissolved in deionized water to obtain a concentration of citric acid solution of 0.25mol / l; ethanol, acetic acid, butanediol are formulated into 69.68g mixed solution in a 50:5:1 molar ratio;

[0046] Step 2: Preparation

[0047] Mix the solution with Ce(NO 3 ) 3 Mix and stir the solution evenly, then add citric acid solution, stir in a water bath at 80°C for 2 hours to mix evenly, and then place it in a drying oven at 70°C for 2.5 hours to obtain a gel; place the obtained gel in a muffle furnace, First heat to 210°C for 15 minutes, then heat to 450°C at a heating rate of 10°C / min and hold for 0.5h, then cool to room temperature with the furnace; 6.15g of light yellow mesoporous cerium oxide powder is obtained. The whole preparation process takes about 6 hours, which greatl...

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Abstract

The invention belongs to the technical field of crystal powder materials, and in particular relates to a method for preparing mesoporous cerium oxide powder by using a sol-gel method. According to the method provided by the invention, a mixture liquid consisting of ethanol, acetic acid, butanediol and citric acid is adopted as a template agent, and a novel synthesis route is provided for synthesis of the mesoporous cerium oxide powder. The template agent is a chemical reagent which is easy to obtain and low in cost; 2.30 Yuan is spent in preparing 1g of the mesoporous cerium oxide powder. The method provided by the invention has the following advantages: the preparation period is short, and the shortest reaction period is 6 hours; the process is controllable, i.e., only a calcining step needs to be accomplished under a high temperature condition, and the highest required temperature is 450 DEG C; the efficiency is high, i.e., 0.40g of the mesoporous cerium oxide powder can be produced from 1g of Ce(NO3)3.6H2O. The prepared mesoporous cerium oxide powder is small in grain, the average particle size is 5.00 mu m, the pore passage is small and uniform, 90% of the apertures are within 3.0-5.0nm.

Description

technical field [0001] The invention belongs to the technical field of preparation of crystal powder materials, and in particular relates to a method for preparing mesoporous cerium oxide powder by a sol-gel method. Background technique [0002] Due to the unique 4f electrons of rare earth elements, their compounds have special optical, electrical and magnetic properties. Among them, cerium oxide with a fluorite structure and its solid solution have strong oxygen storage and oxygen release capabilities and high-temperature ion conductivity. They have great potential in the fields of catalysis, energy, electronics, magnetism, superconductivity, and optical energy. Huge potential for development. Especially micro-nano cerium oxide powder, with Ce 4+ / C 3+ Two oxidation states (Ce 3+ ? Ce 4+ +e). Under oxygen-poor or reducing conditions, a part of Ce on the surface of cerium oxide 4+ is reduced to Ce 3+ , and generate oxygen vacancies to form a series of CeO with oxygen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 左敏刘世权李嘉王艳赵德刚耿浩然
Owner UNIV OF JINAN