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Preparation method of high specific surface area nano-cerium oxide

A technology of nano-cerium oxide and high specific surface area, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of difficult post-processing, unsuitable for industrial production, etc., and achieve the effect of low cost

Inactive Publication Date: 2006-06-14
INNER MONGOLIA UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0006] Chinese Journal of Rare Earth. 1996, 14(4): 372~375 reported the use of hydrogen peroxide-ammonia precipitation method to prepare cerium oxide ultrafine powder. Controlling appropriate conditions can produce a particle size range of 5~13nm, roasting at 250°C The specific surface area is 118m 2 / g CeO 2 Ultrafine powder, but this method is difficult to post-processing, not suitable for industrial production
[0007] The Journal of Nanjing University. 1999, 35(4): 486-490 reported the preparation of CeO by sol-gel method using citric acid as a ligand. 2 Ultrafine particles, calcined at 320°C for 2 hours, the specific surface area is 57m 2 / g, the average particle size is 10nm; Nanjing University Journal. 2000, 36 (1): 10-103 reported the preparation of CeO by freezing dehydration 2 Ultrafine particles, calcined at 200°C for 5 hours, the specific surface area is 89m 2 / g, the average particle size is 7nm, and CeO is prepared by urea hydrolysis 2 Ultrafine particles, calcined at 400°C for 2 hours, the specific surface area is 127m 2 / g, the average particle size is greater than 500nm, but these methods are not suitable for industrial production

Method used

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  • Preparation method of high specific surface area nano-cerium oxide

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Experimental program
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Effect test

Embodiment 1

[0028] 5.2kg cerium carbonate (CeO 2 ≥45%) with 2.91LHNO 3 Dissolve, and add 12.69L deionized water to make solution A, add 46.8g polyethylene glycol, and then add 1.65kg ammonium citrate to make solution C. Take 26.6L1.5mol / L of NH 4 HCO 3 into solution D. Then, under the condition of stirring, add solution C dropwise to solution D. During the dropping process, the pH value of solution D decreases continuously. After solution C is dropped, add ammonia solution dropwise until the pH value of the reaction system is 6.5. ±0.5; At this time, a white precipitate is formed, stir the precipitate for 0.5 hours, filter the precipitate, and wash with deionized water for 3 to 4 times, then dry the precipitate in static air at 80°C for 12 hours, and then roast at 450°C hours, the heating rate is 200°C / hour, the product is cerium oxide, and the specific surface area is 122.6m 2 / g (measured by BET method), the particle size is 20-70nm.

Embodiment 2

[0030] 2.1kg Ce(NO 3 ) 3 ·6H 2 O and 4.83L of deionized water were made into solution A, in which 24.9g of polyethylene glycol was added, and then 0.207kg of ammonium chloride was added into solution C. Take 12.1L1.2mol / L of NaHCO 3 into solution D. Then, under the condition of stirring, the solution D is added dropwise to the solution C. During the dropping process, the pH value of the solution C increases continuously. After the solution D is dropped, the ammonia solution is added dropwise until the pH value of the reaction system is 6.5±0.5; At this time, a white precipitate is formed, and then stir the precipitate for 0.5 hours, filter the precipitate, and wash it with deionized water for 3 to 4 times, then dry the precipitate in static air at 100°C for 12 hours, and then bake it at 480°C 2 hours, the heating rate is 150°C / hour, the product is cerium oxide, and the specific surface area is 110.8m 2 / g (measured by BET method), and its particle size is 40-70nm.

Embodiment 3

[0032] 1.2kg cerium oxide (CeO 2 ≥99%) with 1.49LHNO 3 Dissolve, and add 4.51L deionized water to make solution A, add 48g polyethylene glycol, and then add 0.891g ammonium tartrate to make solution C. Take 10.5L of 2.0mol / L NaOH to make solution D. Then, under the condition of stirring, the solution D is added dropwise to the solution C. During the dropping process, the pH value of the solution C increases continuously. After the solution D is dropped, the ammonia solution is added dropwise until the pH value of the reaction system is 6.5±0.5; At this time, a white precipitate is formed, and then stir the precipitate for 0.3 hours, filter the precipitate, and wash it with deionized water for 3 to 4 times, then dry the precipitate in static air at 120°C for 6 hours, and then bake it at 420°C 2 hours, the heating rate is 200°C / hour, the product is cerium oxide, and the specific surface area is 145.2m 2 / g (measured by BET method), its particle size is 20-50nm (see attached ...

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Abstract

The preparation method of nano cerium oxide with high specific surface area includes the following steps: firstly, preparing salt solution A containing cerium ions, adding surfactant F and additive T in said solution to form solution C; using one or more than two kinds of precipitants and making them in water to form solution D; mixing solution C and solution D to make chemical reaction, reaction time is 10-200min, regulating end point pH value of reaction suspension to 5-10 to produce precipitate, stirring said precipitate for 10-100min, filtering, washing and drying said precipitate, igniting said precipitate for 2-10hr at 400-1000deg.C its heating speed is 50-500deg.C for every hour, so that the nano cerium oxide whose specific surface area is greater than 100sq.m / g.

Description

1. Technical field: [0001] The invention relates to a method for preparing nano cerium oxide with high specific surface area, which belongs to the preparation of rare earth compounds [0002] technology field. 2. Background technology: [0003] In recent years, with the continuous development of science and technology, countries all over the world are actively carrying out research on new materials. The research on materials is developing towards the limit state. Rare earth powder materials require high uniformity, filling, dispersibility and reaction operation. properties, etc., and the rare earth oxides with large specific surface area have attracted more and more attention due to their special properties, especially cerium oxide with large specific surface area has become a research hotspot in recent years, and cerium oxide with large specific surface area is mainly used in catalytic materials, etc. , and these catalytic materials are mainly used in energy environment su...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 李梅柳召刚胡艳宏王秀江史振学
Owner INNER MONGOLIA UNIV OF SCI & TECH
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