Production method of nano rare earth oxide powder

Abstract

The invention discloses a production method of nano rare earth oxide powder, comprising: preparing a rare earth salt solution, adding an ammonium hydrogen carbonate solution into the rare earth salt solution for precipitation reaction, and performing crystal form conversion on slurry obtained by the precipitation reaction at 90 to 130 DEG C under the condition of 0.2 to 0.6 MPa, and calcining obtained crystal to obtain the nano rare earth oxide powder. The production method has the advantages of low process conditions, low equipment dependence and low cost, and is suitable for industrialization.

Description

technical field

[0001] The invention relates to a production method of rare earth materials, in particular to a production method of nanometer rare earth oxide powder. Background technique

[0002] At present, the preparation of nano rare earth oxide powder mainly includes precipitation method and hydrothermal method. The temperature of the hydrothermal reaction method is generally 150-300°C, the pressure is 5-15Mpa, and the reaction time is 2-7 days. Due to the harsh conditions and high equipment requirements, it is not suitable for industrialization. However, the existing precipitation method often uses more organic dispersant and organic surfactant to improve particle fineness and dispersibility.

[0003] The application number is 201611055990.4 which discloses a preparation method of nano rare earth oxide powder, the steps include:

[0004] 1) mixing the rare earth salt and the precipitating agent with the betaine surfactant respectively to obtain solution A and soluti...

Examples

Embodiment 1

[0053] Dilute the 2.0 mol / L cerium chloride solution with deionized water to prepare a rare earth feed solution with a concentration of 1.2 mol / L, heat the cerium chloride solution to a constant temperature of 60°C, and at the same time, stir the stirrer at a speed of 400 rpm , the pre-prepared 3mol / L ammonium bicarbonate solution (according to the mass ratio of rare earth salt solution and ammonium bicarbonate 1:1.5) is continuously and rapidly added to the cerium chloride solution under stirring, and after the addition of the precipitant solution, continue Stir for 30 minutes until all the generated carbon dioxide gas overflows. At this time, the amorphous precipitate after the normal pressure precipitation reaction is obtained; stop stirring, adjust the temperature and pressure of the reaction kettle, so that the temperature of the precipitation slurry reaches 110 °C and the pressure is 0.2 MPa, and the temperature is maintained for 30 minutes ; Wash the precipitated slurry ...

Embodiment 2

[0055] Dilute the 1.8 mol / L neodymium nitrate solution with deionized water to prepare a rare earth feed solution with a concentration of 1.0 mol / L, heat the neodymium nitrate solution to a constant temperature of 50°C, and simultaneously stir the stirrer at a speed of 350 rpm. Pre-prepared 2mol / L ammonium bicarbonate solution (according to the mass ratio of rare earth salt solution and ammonium bicarbonate 1:1.5) was continuously and rapidly added to the neodymium nitrate solution under stirring, and continued to stir for 20 minutes to All the generated carbon dioxide gas overflows, and the amorphous precipitate after the normal pressure precipitation reaction is obtained at this time; stop stirring, adjust the temperature and pressure of the reactor, make the temperature of the precipitation slurry reach 120 ° C, the pressure is 0.3 MPa, and keep the heat and pressure for 50 minutes; Wash the slurry with deionized water at room temperature until the filtrate does not become t...

Embodiment 3

[0057] Dilute the 1.7 mol / L lanthanum cerium chloride solution with deionized water to prepare a rare earth feed solution with a concentration of 1.1 mol / L, heat the lanthanum cerium chloride solution to a constant temperature of 60°C, and at the same time, the stirrer rotates rapidly at 400rpm Stirring, the pre-prepared 1.5mol / L ammonium bicarbonate solution (according to the mass ratio of rare earth salt solution and ammonium bicarbonate 1:1.5) is continuously and rapidly added to the lanthanum cerium chloride solution under stirring, and the precipitant solution is added After the completion, continue to stir for 30 minutes until all the generated carbon dioxide gas overflows. At this time, the amorphous precipitate after the normal pressure precipitation reaction is obtained; stop stirring, adjust the temperature and pressure of the reactor, so that the temperature of the precipitated slurry reaches 95 °C and the pressure is close to 0.2 MPa. Hold the pressure for 40 minute...

technical field

[0001] The invention relates to a production method of rare earth materials, in particular to a production method of nanometer rare earth oxide powder. Background technique

[0002] At present, the preparation of nano rare earth oxide powder mainly includes precipitation method and hydrothermal method. The temperature of the hydrothermal reaction method is generally 150-300°C, the pressure is 5-15Mpa, and the reaction time is 2-7 days. Due to the harsh conditions and high equipment requirements, it is not suitable for industrialization. However, the existing precipitation method often uses more organic dispersant and organic surfactant to improve particle fineness and dispersibility.

[0003] The application number is 201611055990.4 which discloses a preparation method of nano rare earth oxide powder, the steps include:

[0004] 1) mixing the rare earth salt and the precipitating agent with the betaine surfactant respectively to obtain solution A and soluti...

Examples

Embodiment 1

[0053] Dilute the 2.0 mol / L cerium chloride solution with deionized water to prepare a rare earth feed solution with a concentration of 1.2 mol / L, heat the cerium chloride solution to a constant temperature of 60°C, and at the same time, stir the stirrer at a speed of 400 rpm , the pre-prepared 3mol / L ammonium bicarbonate solution (according to the mass ratio of rare earth salt solution and ammonium bicarbonate 1:1.5) is continuously and rapidly added to the cerium chloride solution under stirring, and after the addition of the precipitant solution, continue Stir for 30 minutes until all the generated carbon dioxide gas overflows. At this time, the amorphous precipitate after the normal pressure precipitation reaction is obtained; stop stirring, adjust the temperature and pressure of the reaction kettle, so that the temperature of the precipitation slurry reaches 110 °C and the pressure is 0.2 MPa, and the temperature is maintained for 30 minutes ; Wash the precipitated slurry ...

Embodiment 2

[0055] Dilute the 1.8 mol / L neodymium nitrate solution with deionized water to prepare a rare earth feed solution with a concentration of 1.0 mol / L, heat the neodymium nitrate solution to a constant temperature of 50°C, and simultaneously stir the stirrer at a speed of 350 rpm. Pre-prepared 2mol / L ammonium bicarbonate solution (according to the mass ratio of rare earth salt solution and ammonium bicarbonate 1:1.5) was continuously and rapidly added to the neodymium nitrate solution under stirring, and continued to stir for 20 minutes to All the generated carbon dioxide gas overflows, and the amorphous precipitate after the normal pressure precipitation reaction is obtained at this time; stop stirring, adjust the temperature and pressure of the reactor, make the temperature of the precipitation slurry reach 120 ° C, the pressure is 0.3 MPa, and keep the heat and pressure for 50 minutes; Wash the slurry with deionized water at room temperature until the filtrate does not become t...

Embodiment 3

[0057] Dilute the 1.7 mol / L lanthanum cerium chloride solution with deionized water to prepare a rare earth feed solution with a concentration of 1.1 mol / L, heat the lanthanum cerium chloride solution to a constant temperature of 60°C, and at the same time, the stirrer rotates rapidly at 400rpm Stirring, the pre-prepared 1.5mol / L ammonium bicarbonate solution (according to the mass ratio of rare earth salt solution and ammonium bicarbonate 1:1.5) is continuously and rapidly added to the lanthanum cerium chloride solution under stirring, and the precipitant solution is added After the completion, continue to stir for 30 minutes until all the generated carbon dioxide gas overflows. At this time, the amorphous precipitate after the normal pressure precipitation reaction is obtained; stop stirring, adjust the temperature and pressure of the reactor, so that the temperature of the precipitated slurry reaches 95 °C and the pressure is close to 0.2 MPa. Hold the pressure for 40 minute...

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