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Monodisperse spherical cerium oxide preparing method

A cerium oxide, monodisperse technology, applied in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc., can solve the problems of high hydrothermal temperature, cumbersome process, long preparation period, etc., and achieve uniform particle distribution and good fluidity. Effect

Inactive Publication Date: 2016-01-13
BAOTOU RES INST OF RARE EARTHS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN103641147A uses ammonium bicarbonate as a precipitant and cetyltrimethylammonium bromide as a surfactant to prepare ellipsoidal cerium oxide. The process is cumbersome and the preparation cycle is extremely long
Patent CN104370300 uses hydrothermal method to prepare highly dispersed spherical cerium oxide, which also has the disadvantages of long preparation period and high hydrothermal temperature
At present, in the method of preparing spherical cerium oxide, the use of Ce 4+ The solution is the raw material, adding an appropriate amount of surfactant solution and the preparation period is short and the preparation method with good product dispersibility has not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The method for preparing monodisperse spherical cerium oxide comprises the following steps:

[0015] (1) Add 500ml triethylenetetramine and 500ml deionized water respectively in container, then add 12.2g cetyltrimethylammonium bromide, obtain surfactant solution after stirring;

[0016] (2) Add 1000ml concentration of 0.35mol / L (NH 4 ) 4 Ce(NO 3 ) 6 solution and heated to 90°C, add 52ml of the surfactant solution prepared in step (1) to it, then add ammonia water to the reaction system until the pH is 7, continue to react and age for 1h, and obtain a purple precipitate that is easy to filter, wash the precipitate , filtered, and dried to obtain a loose yellow powder, which was fired at 800°C for 3 hours to obtain a powder with very good fluidity, uniform particle distribution, and a median particle size of D 50 It is 9.8μm monodisperse spherical cerium oxide.

Embodiment 2

[0018] Add 1000ml concentration of 0.52mol / L (NH 4 ) 4 Ce(NO 3 ) 6 Solution is heated to 93 DEG C, and 78ml of the surfactant solution prepared in step (1) of Example 1 is added thereto, then ammonia water is added to the reaction system until the pH is 7, and the reaction aging is continued for 1h to obtain a purple precipitate that is easy to filter. The precipitate was washed, filtered, and dried to obtain a loose yellow powder. The powder was fired at 800°C for 3 hours to obtain a powder with very good fluidity, uniform particle distribution, and a median particle size of D 50 10.5μm monodisperse spherical cerium oxide.

Embodiment 3

[0020] Add 1000ml of Ce(NO 3 ) 4 Solution is heated to 85 DEG C, and 43ml of the surfactant solution prepared in Example 1 step (1) is added thereto, and ammonia water is added to the reaction system until the pH is 7, and the reaction aging is continued for 1h to obtain a purple precipitate that is easy to filter. The precipitate was washed, filtered, and dried to obtain a loose yellow powder. The powder was fired at 800°C for 3 hours to obtain a powder with very good fluidity, uniform particle distribution, and a median particle size of D 50 It is a monodisperse spherical cerium oxide of 12.3 μm.

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Abstract

The present invention discloses a low-cost monodisperse spherical cerium oxide preparing method, which belongs to a material preparation technology. Deionized water, triethylenetetramine and cetyl trimethyl ammonium bromide are used to prepared a surfactant solution, the prepared surfactant solution is added into a Ce4+ solution at 85-93 DEG C, and after the adding ammonia water is used to adjust the pH of the reaction to 7. The reaction is continued for aging for 1 h to obtain easily filtered purple precipitate. The precipitate is filtered, washed, and dried at 80 DEG C to obtain a yellow powder which is loose and good in liquidity. The powder is burnt at 800 DEG C for 3 h to obtain a monodisperse spherical cerium oxide which is very good in liquidity, is uniform in particles, and has a median particle size D50 of 7-15 (mu)m.

Description

technical field [0001] The invention relates to a preparation method of monodisperse spherical cerium oxide, which belongs to a material preparation process. Background technique [0002] Cerium oxide is a cheap but widely used rare earth material. With the development of science and technology, people have higher requirements for the shape and particle size of cerium oxide. In some special polishing fields, cerium oxide microspheres are more and more used. more extensive. At present, there are many methods for preparing cerium oxide microspheres, mainly including mechanochemical method, detonation method, spray pyrolysis method, hydrothermal method, and chemical precipitation method. In the literature "Mechanochemical Reaction Preparation Method of Monodisperse Spherical Ultrafine Cerium Oxide", the wet solid phase mechanochemical reaction method is used to prepare monodisperse spherical cerium oxide powder, which requires a long time for ball milling and the powder partic...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 赵永志张瑞祥郝先库贾红梅王士智刘海旺刘莎莎马显东许宗泽
Owner BAOTOU RES INST OF RARE EARTHS
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