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Preparation method of hollow cerium dioxide

A ceria, hollow technology, applied in the field of preparation of hollow ceria, can solve the problems of long period, cumbersome process of hollow ceria, etc.

Inactive Publication Date: 2020-06-23
SHENZHEN INST OF ADVANCED TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the above-mentioned problems of cumbersome and long-term preparation of hollow ceria by the existing template method, the present invention provides a low-cost, easy-to-operate template-free preparation method of hollow ceria

Method used

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  • Preparation method of hollow cerium dioxide

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preparation example Construction

[0026] A kind of preparation method of hollow ceria provided by the invention comprises the following steps:

[0027] In step S1, water-soluble trivalent cerium salt and citric acid and / or citrate are dissolved in deionized water to form a mixed solution, and Ce in the mixed solution 3+ The ratio of the amount of the substance to the citrate ion is 1:1-2:1.

[0028] Further, in this step, the water-soluble trivalent cerium salt may be cerium nitrate or cerium chloride.

[0029] Preferably, Ce in the mixed solution 3+ The concentration is 0.3mol / L~0.9mol / L.

[0030] Further, in this step, the citrate may be sodium citrate.

[0031] Preferably, the concentration of citrate ions in the mixed solution is 0.2mol / L-0.5mol / L.

[0032] Citric acid and / or citrate as an organic linker is a polycarboxylic acid organic compound with carboxyl ligands; in addition, citric acid or citrate can be partially deprotonated or completely deprotonated with different pH In effect, there are mul...

Embodiment 1

[0041] First, 0.4130 g of cerium nitrate hexahydrate and 0.1010 g of citric acid monohydrate were dissolved in 2 mL of deionized water to prepare a mixed solution.

[0042] Then, the above mixed solution was placed in a polytetrafluoroethylene-lined autoclave and subjected to ultrasonic treatment for 20 min, and a hydrothermal reaction was performed at 210° C. for 1 h to obtain a hydrothermal product.

[0043] Finally, after the reaction was completed, the hydrothermal product was cooled to room temperature, and after solid-liquid separation, the obtained solid phase was centrifuged and washed three times with ethanol, and vacuum-dried for 2 hours to obtain the product.

[0044] Adopt X-ray diffractometer (Germany Bruker D8 advance, Cu target radiation λ=0.15418nm) to measure the product that present embodiment obtains, its X-ray diffraction test (XRD) result is as follows figure 1 shown. The diffraction peaks of this product are similar to those of fluorite-type CeO 2 The d...

Embodiment 2

[0048] First, 2.4490 g of cerium nitrate hexahydrate and 0.5930 g of citric acid monohydrate were dissolved in 10 mL of deionized water to prepare a mixed solution.

[0049] Then, the above mixed solution was placed in a polytetrafluoroethylene-lined autoclave and subjected to ultrasonic treatment for 20 min, and a hydrothermal reaction was performed at 230° C. for 5 h to obtain a hydrothermal product.

[0050] Finally, after the completion of the hydrothermal reaction, the hydrothermal product is cooled to room temperature, and after solid-liquid separation, the obtained solid phase is centrifuged and washed three times with deionized water, and vacuum-dried for 8 hours to obtain hollow cerium oxide. The outer diameter of the hollow cerium oxide is is 3 μm, and the shell thickness is 100 nm.

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Abstract

The invention discloses a preparation method of hollow cerium dioxide. The preparation method comprises the following steps: S1, dissolving a water-soluble trivalent cerium salt, citric acid and / or citrate in deionized water to prepare a mixed solution, wherein the mass ratio of Ce <3+> to citrate ions in the mixed solution is 1: 1-2: 1; and S2, carrying out a hydrothermal reaction on the mixed solution at 180-230 DEG C for 1-5 hours to obtain hollow cerium dioxide. A template-free method is adopted, and hollow cerium dioxide is synthesized in one step in a high-temperature closed environment.The preparation method is simple and efficient in steps, micron-sized hollow cerium dioxide with uniform distribution is obtained, and the average particle size of hollow cerium dioxide is 4 [mu]m. The defects that in the prior art, a template and a surfactant are required, and complex after-treatments such as high-temperature sintering is needed are overcome, the production period of hollow cerium dioxide is effectively shortened, and the production cost of hollow cerium dioxide is reduced.

Description

technical field [0001] The invention relates to the technical field of oxide preparation, in particular to a method for preparing hollow ceria. Background technique [0002] Ceria in nature (CeO 2 ) exists in typical bastnaesite, monazite and other rare earth ores, and its content is above 45%. As a typical light rare earth oxide, CeO 2 It has been widely used in the fields of automobile exhaust purification catalyst, ultraviolet absorber, luminescent material, polishing agent, radiation-resistant glass, chemical decolorizer of glass and advanced ceramic preparation; CeO 2 It is also used in photocatalysts, gas sensors, fuel cells, anti-corrosion coatings, etc. [0003] CeO 2 It belongs to the cubic crystal system, and the crystal structure is fluorite type. CeO 2 Has a fast Ce 3+ / C 4+ Redox conversion performance: under reducing conditions such as high temperature or rich CO, CeO 2 Loss of lattice oxygen forms oxygen vacancies, part of Ce 4+ Revert to Ce 3+ , wh...

Claims

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Application Information

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IPC IPC(8): C01F17/235C01F17/10
CPCC01P2004/34C01P2004/61C01P2004/62C01F17/00C01F17/10C01F17/235
Inventor 于淑会吴旭东孙蓉
Owner SHENZHEN INST OF ADVANCED TECH
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