Process for preparing rare-earth nano oxide by ball grinding and solid-phase chemical reaction

A solid-phase chemical reaction, nano-rare earth technology, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc. The effect of increasing the surface area

Inactive Publication Date: 2002-12-25
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] From the contents of the above two Chinese patent applications, it can be seen that they both prepare precursors or precursors through liquid-phase chemical reactions, and the thermal decomposition of precursors or precursors is completed at high temperatures, so not only a large amount of solvents are required, but also numerous processes , and lead to increased energy consumption and cost

Method used

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  • Process for preparing rare-earth nano oxide by ball grinding and solid-phase chemical reaction
  • Process for preparing rare-earth nano oxide by ball grinding and solid-phase chemical reaction

Examples

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Embodiment 1

[0029] In this embodiment, the rare earth inorganic salt is cerium nitrate, and the ligand is sodium oxalate. The process flow is as follows: figure 1 As shown, there are the following steps in sequence:

[0030] (1) Ingredients

[0031] The molar ratio of cerium nitrate and sodium oxalate is 1: 4;

[0032] (2) Mixing

[0033] Mix cerium nitrate and sodium oxalate until uniform;

[0034] (3) Preparation of precursors by ball milling solid-phase chemical reaction

[0035] Place the mixture of cerium nitrate and sodium oxalate in a star-shaped ball mill and add lubricant ethanol for ball milling. The amount of ethanol added is limited to keep the dispersed state of the ball mill. The speed of the ball mill is controlled at 230 rpm. The ball mill is at room temperature, Carried out under normal pressure, cerium nitrate and sodium oxalate can be completely chemically reacted to form the precursor cerium oxalate in 20 minutes;

[0036] (4) Precursor removal

[0037] Cerium ox...

Embodiment 2

[0043] In this embodiment, the rare earth inorganic salt is cerium ammonium nitrate, and the ligand is oxalic acid. The process flow is as follows: figure 1 As shown, there are the following steps in sequence:

[0044] (1) Ingredients

[0045] The molar ratio of ceric ammonium nitrate and oxalic acid is 1: 4;

[0046] (2) Mixing

[0047] Mix ammonium cerium nitrate and oxalic acid until uniform;

[0048] (3) Preparation of precursors by ball milling solid-phase chemical reaction

[0049] The mixture of ammonium cerium nitrate and oxalic acid is placed in a star-shaped ball mill and the lubricant ethanol is added for ball milling. The amount of ethanol added is limited to keep the dispersed state of the ball mill, the speed of the ball mill is controlled at 270 rpm, and the ball mill is at room temperature, Carried out under normal pressure, cerium ammonium nitrate and oxalic acid can be completely chemically reacted to form the precursor cerium oxalate in 15 minutes;

[0...

Embodiment 3

[0057] In this embodiment, the rare earth inorganic salt is cerium chloride, and the ligand is sodium bicarbonate, and the process flow is as follows figure 1 As shown, there are the following steps in sequence:

[0058] (1) Ingredients

[0059] The mol ratio of cerium chloride and sodium bicarbonate is 1: 8;

[0060] (2) Mixing

[0061] Mix cerium chloride and sodium bicarbonate until uniform;

[0062] (3) Preparation of precursors by ball milling solid-phase chemical reaction

[0063] The mixture of cerium chloride and sodium bicarbonate is placed in a star-shaped ball mill and added lubricant ethanol for ball milling. The amount of ethanol added is limited to keep the dispersed state of the ball mill. The speed of the ball mill is controlled at 250 rpm. Carried out at room temperature and normal pressure, the chemical reaction between cerium chloride and sodium bicarbonate can completely occur in 25 minutes to form the precursor cerium bicarbonate;

[0064] (4) Precurs...

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Abstract

A nano rare-earth oxide is prepared from the inorganic salt of rare-earth element (Ce, La, Pr, Nd, or Tb) and ligand (oxalic acid, sodium oxalate, dicarbonate, 8-hydroxyquinoline, complexon, etc) through proportioning, mixing, and ball grinding while solid-phase chemical reaction to obtain precursor, removing impurities, drying, and medium-temp thermal decomposition. Its advantages are simple process, low cost, saving energy, high purity (more than 99%) and narrow size distribution (10-30 nm).

Description

1. Technical field [0001] The invention relates to a preparation method of nano-rare earth oxide by ball milling solid-phase chemical reaction. 2. Background technology [0002] The Chinese patent application number 91110578.6 discloses a preparation method of cerium oxide. The method uses cerium-containing mixed rare earths as raw materials. The process steps are as follows: (1) the Ce in the mixed rare earths is 3+ All oxidized to Ce 4+ , and then dissolved with sulfuric acid to obtain a mixed rare earth sulfuric acid feed solution; (2) adding sodium sulfate to the mixed rare earth sulfuric acid feed solution, the reaction generates less cerium RE 3+ (3) in the filtrate that filters double salt precipitation gained, add ferrous sulfate reaction and generate cerium sulfate sodium double salt precipitation; (4) precipitation after filtration is converted into cerium hydroxide with caustic soda reaction; (5) will Dissolve cerium hydroxide with hydrochloric acid to form ceri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00C04B35/50
Inventor 庄稼朱达川涂铭旌迟燕华
Owner SICHUAN UNIV
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