CN102992379A - Method for preparing spherical macro-granular neodymium oxide - Google Patents
Method for preparing spherical macro-granular neodymium oxide Download PDFInfo
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- CN102992379A CN102992379A CN2012103835070A CN201210383507A CN102992379A CN 102992379 A CN102992379 A CN 102992379A CN 2012103835070 A CN2012103835070 A CN 2012103835070A CN 201210383507 A CN201210383507 A CN 201210383507A CN 102992379 A CN102992379 A CN 102992379A
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Abstract
The invention relates to a method for preparing spherical macro-granular neodymium oxide, belonging to material preparation processes. The method comprises the following steps: preparing an ammonium bicarbonate solution by using ammonium bicarbonate, ammonia water and deionized water, adding a neodymium nitrate solution into the ammonium bicarbonate solution to obtain a mixed solution consisting of the ammonium bicarbonate, the ammonia water and the neodymium nitrate, adding hydrogen peroxide into the mixed solution to generate neodymium carbonate peroxide precipitates, ageing for 24-48 hours, filtering and washing the precipitates, scorching at the temperature of 900-1200 DEG C, and preserving heat for 4 hours to obtain spherical macro-granular neodymium oxide products, which have the medium particle diameter D50 being 40-50 microns, are uniform in particle and good in flowability and are formed by porous lamellas in appearance.
Description
Technical field
The present invention relates to a kind of method for preparing spherical macrobead Neodymium trioxide, belong to a kind of material preparation process.
Background technology
Neodymium trioxide is very extensive in the application in the fields such as magneticsubstance, glass, pottery, catalysis, electronics.Along with the development of science and technology, have great application prospect for packing material, spray material, special magnetic material, neutron-absorbing material aspect macrobead Neodymium trioxide.The volume particle size Neodymium trioxide Study on Preparation that document horse jade-like stone is shown, rare earth, 2011,32 (5): 56-59, provide a kind of with the standby macrobead Neodymium trioxide of oxalate precipitation legal system, medium particle diameter is 50-150 μ m; Chinese patent CN102531024A and CN102502760A provide two kinds to prepare macrobead Praseodymium trioxide neodymium method, take the praseodymium chloride neodymium as feed liquid, bicarbonate of ammonia is precipitation agent, two kinds of precipitation temperatures, and obtaining pattern is the Praseodymium trioxide neodymium product of 25-45 μ m for spherical and sheet, medium particle diameter.
Summary of the invention
The object of the present invention is to provide a kind of uniform particles, good fluidity, medium particle diameter D
50Be that 40 μ m-50 μ m, pattern are the preparation method of the spherical macrobead Neodymium trioxide of porous flake composition.
Technical solution: it is 28% ammoniacal liquor and deionized water that the present invention adds respectively bicarbonate of ammonia, concentration in the reactor, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the neodymium nitrate solution of 1.06mol/L, bicarbonate of ammonia and neodymium nitrate mol ratio are 1: 0.0172, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add concentration in the mixing solutions and be 30% hydrogen peroxide, neodymium nitrate and hydrogen peroxide mol ratio are 1: 6.38, react 2.5 hours, ageing 24-48 hour, obtain peroxide neodymium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 900-1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50Be 40-50 μ m, uniform particles, good fluidity, pattern are the spherical macrobead Neodymium trioxide that porous flake forms.
The invention effect
Peroxide neodymium carbonate precipitation digestion time and calcination temperature are that the spherical macrobead Neodymium trioxide of preparation is crucial among the present invention, among the peroxide neodymium carbonate preparation method, digestion time is the key factor that determines peroxide neodymium carbonate granularity, digestion time was less than 4 hours, and peroxide neodymium carbonate deposit seeds is very thin, sad filter, static ageing is more than 24 hours, obtain macrobead peroxide neodymium carbonate, the peroxide neodymium carbonate is under 900-1200 ℃ at calcination temperature, obtains medium particle diameter D
50Be the Neodymium trioxide product of 40-50 μ m, control peroxide neodymium carbonate precipitation digestion time and calcination temperature can prepare varying particle size, uniform particles, good fluidity, pattern and be spherical macrobead Neodymium trioxide product, and this technique is convenient to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the XRD figure of the spherical macrobead Neodymium trioxide of the present invention;
Fig. 2 is the particle size distribution figure of the spherical macrobead Neodymium trioxide of the present invention;
Fig. 3 is the SEM figure of the spherical macrobead Neodymium trioxide of the present invention.
Embodiment
Embodiment 1
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 72ml concentration is the neodymium nitrate solution of 1.06mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 50ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2.5 hours, ageing 28 hours obtains the peroxide neodymium carbonate and precipitates, and with sedimentation and filtration, washing, calcination temperature is 900 ℃, is incubated 4 hours, obtains medium particle diameter D
50It is the spherical macrobead Neodymium trioxide of 50.29 μ m.
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 72ml concentration is the neodymium nitrate solution of 1.06mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 50ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2.5 hours, ageing 36 hours obtains the peroxide neodymium carbonate and precipitates, and with sedimentation and filtration, washing, calcination temperature is 1000 ℃, is incubated 4 hours, obtains medium particle diameter D
50It is the spherical macrobead Neodymium trioxide of 43.66 μ m.
Embodiment 3
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 72ml concentration is the neodymium nitrate solution of 1.06mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 50ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2.5 hours, ageing 40 hours obtains the peroxide neodymium carbonate and precipitates, and with sedimentation and filtration, washing, calcination temperature is 1100 ℃, is incubated 4 hours, obtains medium particle diameter D
50It is the spherical macrobead Neodymium trioxide of 43.77 μ m.
Embodiment 4
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 72ml concentration is the neodymium nitrate solution of 1.06mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 50ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2.5 hours, ageing 48 hours obtains the peroxide neodymium carbonate and precipitates, and with sedimentation and filtration, washing, calcination temperature is 1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50It is the spherical macrobead Neodymium trioxide of 43.86 μ m.
Claims (1)
1. the method for preparing spherical macrobead Neodymium trioxide, it is characterized in that, it is 28% ammoniacal liquor and deionized water that the present invention adds respectively bicarbonate of ammonia, concentration in the reactor, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the neodymium nitrate solution of 1.06mol/L, bicarbonate of ammonia and neodymium nitrate mol ratio are 1: 0.0172, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add concentration in the mixing solutions and be 30% hydrogen peroxide, neodymium nitrate and hydrogen peroxide mol ratio are 1: 6.38, react 2.5 hours, ageing 24-48 hour, obtain peroxide neodymium carbonate precipitation, with sedimentation and filtration, washing, calcination temperature is 900-1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50Be 40-50 μ m, uniform particles, good fluidity, pattern are the spherical macrobead Neodymium trioxide that porous flake forms.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110510653A (en) * | 2019-09-27 | 2019-11-29 | 内蒙古包钢和发稀土有限公司 | The preparation method of neodymia |
| CN112194168A (en) * | 2020-10-26 | 2021-01-08 | 常州市卓群纳米新材料有限公司 | Preparation method of rare earth neodymium oxide |
| CN114671450A (en) * | 2022-03-29 | 2022-06-28 | 包头稀土研究院 | Preparation method of samarium oxide spherical particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008279552A (en) * | 2007-05-11 | 2008-11-20 | Agc Seimi Chemical Co Ltd | Method of recovering rare earth element |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2008279552A (en) * | 2007-05-11 | 2008-11-20 | Agc Seimi Chemical Co Ltd | Method of recovering rare earth element |
Non-Patent Citations (4)
| Title |
|---|
| CARLOS A. DA S. QUEIROZ ET AL.: "Thermoanalytical characterization of neodymium peroxicarbonate", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 344, 7 October 2002 (2002-10-07), pages 32 - 35 * |
| MARI E. DE VASCONCELLOS ET AL.: "Solubility behavior of rare earths with ammonium carbonate and ammonium carbonate plus ammonium hydroxide:Precipitation of their peroxicarbonates", 《JOURNAL OF ALLOYS AND COMPOUNDS》, vol. 451, 18 April 2007 (2007-04-18), pages 426 - 428 * |
| 冷忠义等: "用碳酸氢铵作沉淀剂制取碳酸钕和氧化钕", 《稀土》, vol. 21, no. 6, 31 December 2000 (2000-12-31), pages 26 - 29 * |
| 沈旭等: "《化学选矿技术》", 31 July 2011, article "沉淀条件", pages: 113 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110510653A (en) * | 2019-09-27 | 2019-11-29 | 内蒙古包钢和发稀土有限公司 | The preparation method of neodymia |
| CN110510653B (en) * | 2019-09-27 | 2021-11-09 | 内蒙古包钢和发稀土有限公司 | Preparation method of neodymium oxide |
| CN112194168A (en) * | 2020-10-26 | 2021-01-08 | 常州市卓群纳米新材料有限公司 | Preparation method of rare earth neodymium oxide |
| CN112194168B (en) * | 2020-10-26 | 2023-06-20 | 常州市卓群纳米新材料有限公司 | Preparation method of rare earth neodymium oxide |
| CN114671450A (en) * | 2022-03-29 | 2022-06-28 | 包头稀土研究院 | Preparation method of samarium oxide spherical particles |
| CN114671450B (en) * | 2022-03-29 | 2024-04-12 | 包头稀土研究院 | Preparation method of samarium oxide spherical particles |
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