CN102992379B - Method for preparing spherical macro-granular neodymium oxide - Google Patents
Method for preparing spherical macro-granular neodymium oxide Download PDFInfo
- Publication number
- CN102992379B CN102992379B CN201210383507.0A CN201210383507A CN102992379B CN 102992379 B CN102992379 B CN 102992379B CN 201210383507 A CN201210383507 A CN 201210383507A CN 102992379 B CN102992379 B CN 102992379B
- Authority
- CN
- China
- Prior art keywords
- neodymium
- hours
- granular
- concentration
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
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 preparing spherical macro-granular neodymium oxide, belong to a kind of material preparation process.
Background technology
The application of Neodymium trioxide in fields such as magneticsubstance, glass, pottery, catalysis, electronics widely.Along with the development of science and technology, have great application prospect for packing material, spray material, special magnetic material, neutron-absorbing material aspect macro-granular neodymium oxide.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 one oxalate precipitation process to prepare macro-granular neodymium oxide, medium particle diameter is 50-150 μm; Chinese patent CN102531024A and CN102502760A provides two kinds and prepares macrobead praseodymium neodymium oxide method, with praseodymium chloride neodymium for feed liquid, bicarbonate of ammonia is precipitation agent, two kinds of precipitation temperatures, and to obtain pattern be spherical and sheet, medium particle diameter is the praseodymium neodymium oxide product of 25-45 μm.
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 40 μm-50 μm, pattern is the preparation method of spherical macro-granular neodymium oxide of porous flake composition.
Technical solution: the present invention adds bicarbonate of ammonia respectively in reactor, concentration is 28% ammoniacal liquor and deionized water, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, add the neodymium nitrate solution that concentration is 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; In mixing solutions, add the hydrogen peroxide that concentration is 30%, neodymium nitrate and hydrogen peroxide mol ratio are 1: 6.38, react 2.5 hours, ageing 24-48 hour, obtains neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50for 40-50 μm, uniform particles, good fluidity, pattern are the spherical macro-granular neodymium oxide of porous flake composition.
Invention effect
In the present invention, neodymium carbonate peroxide precipitation digestion time and calcination temperature are that preparation spherical macro-granular neodymium oxide is crucial, in neodymium carbonate peroxide preparation method, digestion time is the key factor determining neodymium carbonate peroxide granularity, digestion time is less than 4 hours, and neodymium carbonate peroxide deposit seeds is very thin, sad filter, static ageing more than 24 hours, obtain macrobead neodymium carbonate peroxide, neodymium carbonate peroxide, at calcination temperature is 900-1200 DEG C, obtains medium particle diameter D
50for the Neodymium trioxide product of 40-50 μm, control neodymium carbonate peroxide precipitation digestion time and calcination temperature, can prepare varying particle size, uniform particles, good fluidity, pattern be spherical macro-granular neodymium oxide product, this technique is convenient to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the XRD figure of spherical macro-granular neodymium oxide of the present invention;
Fig. 2 is the particle size distribution figure of spherical macro-granular neodymium oxide of the present invention;
Fig. 3 is the SEM figure of spherical macro-granular neodymium oxide of the present invention.
Embodiment
Embodiment 1
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the neodymium nitrate solution that 72ml concentration is 1.06mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add the hydrogen peroxide that 50ml concentration is 30%, react 2.5 hours, ageing 28 hours, obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 900 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 50.29 μm.
Embodiment 2
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the neodymium nitrate solution that 72ml concentration is 1.06mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add the hydrogen peroxide that 50ml concentration is 30%, react 2.5 hours, ageing 36 hours, obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 1000 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 43.66 μm.
Embodiment 3
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the neodymium nitrate solution that 72ml concentration is 1.06mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add the hydrogen peroxide that 50ml concentration is 30%, react 2.5 hours, ageing 40 hours, obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 43.77 μm.
Embodiment 4
Add 350g bicarbonate of ammonia in the reactor, 300ml concentration be 28% ammoniacal liquor and deionized water 520ml, then add the neodymium nitrate solution that 72ml concentration is 1.06mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add the hydrogen peroxide that 50ml concentration is 30%, react 2.5 hours, ageing 48 hours, obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 43.86 μm.
Claims (3)
1. prepare the method for spherical macro-granular neodymium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the neodymium nitrate solution that 72 ml concentration are 1.06 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add the hydrogen peroxide that 50ml concentration is 30%, react 2.5 hours, ageing 28 hours, obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 900 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 50.29 μm.
2. prepare the method for spherical macro-granular neodymium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the neodymium nitrate solution that 72 ml concentration are 1.06 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add 50 ml concentration is the hydrogen peroxide of 30%, reacts 2.5 hours, ageing 36 hours, and obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 1000 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 43.66 μm.
3. prepare the method for spherical macro-granular neodymium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the neodymium nitrate solution that 72 ml concentration are 1.06 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add 50 ml concentration is the hydrogen peroxide of 30%, reacts 2.5 hours, ageing 40 hours, and obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 43.77 μm.
4. prepare the method for spherical macro-granular neodymium oxide, it is characterized in that, add 350 g bicarbonate of ammonia in the reactor, 300 ml concentration be 28% ammoniacal liquor and deionized water 520 ml, add the neodymium nitrate solution that 72 ml concentration are 1.06 mol/L again, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; In mixing solutions, add 50 ml concentration is the hydrogen peroxide of 30%, reacts 2.5 hours, ageing 48 hours, and obtain neodymium carbonate peroxide precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the spherical macro-granular neodymium oxide of 43.86 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210383507.0A CN102992379B (en) | 2012-09-22 | 2012-09-22 | Method for preparing spherical macro-granular neodymium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210383507.0A CN102992379B (en) | 2012-09-22 | 2012-09-22 | Method for preparing spherical macro-granular neodymium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102992379A CN102992379A (en) | 2013-03-27 |
| CN102992379B true CN102992379B (en) | 2014-12-17 |
Family
ID=47921585
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210383507.0A Active CN102992379B (en) | 2012-09-22 | 2012-09-22 | Method for preparing spherical macro-granular neodymium oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102992379B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN114671450B (en) * | 2022-03-29 | 2024-04-12 | 包头稀土研究院 | Preparation method of samarium oxide spherical particles |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4969313B2 (en) * | 2007-05-11 | 2012-07-04 | Ａｇｃセイミケミカル株式会社 | Recovery method of rare earth elements |
-
2012
- 2012-09-22 CN CN201210383507.0A patent/CN102992379B/en active Active
Non-Patent Citations (4)
| Title |
|---|
| Solubility behavior of rare earths with ammonium carbonate and ammonium carbonate plus ammonium hydroxide:Precipitation of their peroxicarbonates;Mari E. de Vasconcellos et al.;《Journal of Alloys and Compounds》;20070418;第451卷;第426-428页 * |
| Thermoanalytical characterization of neodymium peroxicarbonate;Carlos A. da S. Queiroz et al.;《Journal of Alloys and Compounds》;20021007;第344卷;第32-35页 * |
| 沈旭等.沉淀条件.《化学选矿技术》.冶金工业出版社,2011,(第1版),第113页. * |
| 用碳酸氢铵作沉淀剂制取碳酸钕和氧化钕;冷忠义等;《稀土》;20001231;第21卷(第6期);第26-29页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102992379A (en) | 2013-03-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102581294B (en) | Method for preparing nano-metallic copper powder | |
| CN103407969B (en) | A kind of three-dimensional ordered macroporous-gas-phase permeation-precipitation method of mesopore metal oxide or composite oxides and products obtained therefrom | |
| CN101306828A (en) | Device and process for preparing rare-earth compound uniform micro powder | |
| CN102992379B (en) | Method for preparing spherical macro-granular neodymium oxide | |
| CN102580721A (en) | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method | |
| CN102699348A (en) | Method of preparing micron-sized spherical high-purity nickel powder | |
| CN102502760B (en) | Method for preparing large-particle and flaky praseodymium neodymium oxide | |
| CN104419378A (en) | Fluorine doping method of cerium-based rare earth polishing powder | |
| CN104671289A (en) | Fe2O3 nanosheet and preparation method thereof | |
| CN102115214A (en) | Method for preparing small-particle-size cobalt carbonate | |
| CN106082297B (en) | A kind of preparation method of 20~60 microns of gadolinium oxides of medium particle diameter | |
| CN102557098A (en) | Method for preparing superfine high-purity barium carbonate powder | |
| CN103086416B (en) | Preparation method of large-particle samarium oxide | |
| CN102583493A (en) | Method for preparing large-particle Ce rich rare earth oxide | |
| CN103011231B (en) | Method for preparing multihole sheet large-grain praseodymium oxide | |
| CN103058724B (en) | Preparation method of large-particle gadolinium oxide | |
| CN102502835B (en) | Method for preparing silver molybdate nano square crystal | |
| CN102992381B (en) | Method for preparing macrogranular ytterbium oxide | |
| CN103614139B (en) | Reverse co-precipitation is adopted to prepare Gd 2ti 2o 7: the method for Ce nano-luminescent powder body | |
| CN100532277C (en) | Process for preparing nano NiO by ammonia water single phase precipitation | |
| CN104889415A (en) | Preparation method of nano nickel powder | |
| CN102992380B (en) | Method for preparing macrogranular europium oxide | |
| CN103058256B (en) | Method for preparing large-granule dysprosium oxide | |
| CN102910637B (en) | Preparation method for rare earth silicate nano-powder | |
| CN104261455B (en) | A kind of preparation method of high purity stannic acid lanthanum nano-powder |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |