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Preparation method of high-purity nano cerium phosphate powder

A technology of cerium phosphate and powder, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of harsh production process, complex production process, high production cost, etc., and achieve the effect of friendly production environment and simple production process

Active Publication Date: 2021-03-26
YIYANG HONGYUAN RARE EARTH
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Problems solved by technology

The Chinese patent application with the application number CN200910076998.2 discloses a fluorescent nanomaterial with a core-shell structure and its preparation method. In this method, phosphate is added to soluble cerium salts such as cerium nitrate, cerium chloride, and cerium sulfate. React at 180°C-230°C for 3h-72h. After the reaction is completed, filter, wash, and dry. This method produces ammonia nitrogen wastewater or high-salt wastewater. The product has low purity and the production process is harsh.
The Chinese patent application with the application number CN201010287623.3 discloses a method for hydrothermally synthesizing cerium phosphate micro-nanospheres. The method uses Ce 3+ With polyphosphoric acid as raw material, cerium phosphate micro-nanospheres are obtained through hydrothermal reaction. This method has high production cost, high acid content in wastewater, and harsh production process.
The Chinese patent application with the application number CN200910109858.0 discloses a method for preparing cerium phosphate nanowires. The method uses soluble cerium salt and phosphate as raw materials, adjusts the pH value through precipitation reaction, and obtains cerium phosphate precipitation. This method produces High cost, high acid content in wastewater, high alkali metal ions in the product
Papers published by Yang Lige et al. "Hydrothermal synthesis and fluorescence properties of cerium phosphate nanomaterials in different crystal forms", papers published by Bi Huifang "Hydrothermal synthesis of cerium phosphate micro-nanospheres", papers published by Zhang Xinqi et al. Synthesis and Characterization of Cerium Phosphate One-Dimensional Nanomaterials" and other researches. Their raw materials are cerium salt and phosphate as raw materials, which will have disadvantages such as waste water, high impurity content in the product, high production cost, and complicated production process.
[0004] For the synthesis of cerium phosphate, the main methods are precipitation method, hydrothermal method, etc. For the precipitation method, the soluble cerium salt is first reacted with phosphate, and the pH value is adjusted to obtain cerium phosphate precipitation, which will generate waste water and the product purity is not high. shortcoming

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Embodiment 1

[0022] A preparation method of high-purity nano cerium phosphate powder, comprising the following steps:

[0023] (1) Take 172g of cerium carbonate with a relative purity of rare earth of 99.995% (the total amount of rare earth is 50%), add it to 1L of deionized water and stir to obtain a cerium-containing suspension;

[0024] (2) Prepare 1L of solution with phosphoric acid concentration of 0.5mol / L, nitric acid concentration of 0.05mol / L, and hydrogen peroxide concentration of 0.0025mol / L;

[0025] (3) At a constant temperature of 25°C, add cerium suspension to the phosphoric acid solution, raise the temperature to 80°C under stirring, and keep the temperature for 30 minutes to obtain a cerium phosphate precipitate, filter and wash the cerium phosphate precipitate, and recycle the filtrate to obtain the cerium phosphate Dry at 80°C for 6 hours to obtain cerium phosphate product.

[0026] The composition and the particle diameter of the cerium phosphate product gained in the ...

Embodiment 2

[0030] A preparation method of high-purity nano cerium phosphate powder, comprising the following steps:

[0031] (1) Take 2000 g of cerium hydroxide with a relative rare earth purity of 99.999% (30% of the total amount of rare earth), add it to 10L deionized water and stir to obtain a cerium-containing suspension;

[0032] (2) Prepare 5L of solution of phosphoric acid concentration 0.72mol / L, nitric acid concentration 0.01mol / L, ascorbic acid concentration 0.003mol / L;

[0033] (3) At a constant temperature of 80°C, add the cerium-containing suspension to the phosphoric acid solution under stirring conditions, age for 2 hours after the addition, filter and wash, and recycle the filtrate, and dry the obtained cerium phosphate at 150°C for 1 hour to obtain Cerium phosphate products.

[0034] The composition and particle size of the cerium phosphate product obtained in this embodiment are shown in Table 2.

[0035] Table 2

[0036] Test items La 2 o 3 / TREO

Embodiment 3

[0038] A preparation method of high-purity nano cerium phosphate powder, comprising the following steps:

[0039] (1) Take 3000 g of basic cerium carbonate with a relative rare earth purity of 99.998% (60% of the total amount of rare earth), add it to 10L deionized water and stir to obtain a cerium-containing suspension;

[0040] (2) prepare phosphoric acid concentration 1.5mol / L, nitric acid concentration 0.1mol / L, solution 7.1L of ascorbic acid concentration 0.022mol / L;

[0041] (3) At a constant temperature of 90°C, add the cerium-containing suspension to the phosphoric acid solution under stirring conditions, age for 1 hour after the addition, filter and wash, and recycle the filtrate, and dry the obtained cerium phosphate at 100°C for 3 hours to obtain Cerium phosphate products.

[0042] The composition and particle size of the cerium phosphate product obtained in this embodiment are shown in Table 3.

[0043] table 3

[0044] Test items La 2 o 3 / TREO ...

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Abstract

The invention relates to a preparation method of high-purity nano cerium phosphate powder, which comprises the following steps: (1) taking cerium carbonate, basic cerium carbonate or cerium hydroxide,adding into deionized water or deionized water containing a dispersing agent, and stirring to obtain a cerium-containing suspension, (2) preparing a phosphoric acid solution, adding nitric acid or hydrochloric acid into the phosphoric acid solution, and adding hydrogen peroxide or ascorbic acid to obtain a phosphoric acid solution containing hydrogen peroxide or ascorbic acid, and (3) adding thecerium-containing suspension into a phosphoric acid solution containing hydrogen peroxide or ascorbic acid for reaction, and after the reaction is finished, filtering, washing and drying precipitatesto obtain cerium phosphate powder. The purity of the high-purity nano cerium phosphate prepared by the method is greater than 99.995%, the dispersity is good, and the primary particle size of the high-purity nano cerium phosphate is spherical-like powder of 100nm-500nm.

Description

technical field [0001] The invention relates to a preparation method of high-purity nanometer cerium phosphate powder. Background technique [0002] Cerium is a rare earth element widely used in grinding and polishing, catalysts, and fuel electronics. Cerium phosphate exists in the monazite structure in nature. Due to its unique excellent properties, cerium phosphate is widely used in semiconductor materials, ceramics, lubricant materials, luminescent materials and other fields. However, in these application fields, cerium phosphate is required to have high purity and particle size. small and evenly distributed. [0003] The existing preparation method of high-purity nano-cerium phosphate powder, such as the preparation method of a low-temperature phosphorus-containing cerium-copper composite denitration catalyst disclosed in the Chinese patent application with the application number CN201611049447.3, uses cerous nitrate, coke Phosphoric acid and urea are used as raw mater...

Claims

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Application Information

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IPC IPC(8): C01B25/37B82Y30/00B82Y40/00
CPCC01B25/37B82Y30/00B82Y40/00C01P2006/80C01P2004/62C01P2004/64C01P2004/03C01P2002/72Y02E60/10
Inventor 刘卫杨泱肖勇崔小震
Owner YIYANG HONGYUAN RARE EARTH
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