CN103011231A - Method for preparing multihole sheet large-grain praseodymium oxide - Google Patents
Method for preparing multihole sheet large-grain praseodymium oxide Download PDFInfo
- Publication number
- CN103011231A CN103011231A CN2012103829262A CN201210382926A CN103011231A CN 103011231 A CN103011231 A CN 103011231A CN 2012103829262 A CN2012103829262 A CN 2012103829262A CN 201210382926 A CN201210382926 A CN 201210382926A CN 103011231 A CN103011231 A CN 103011231A
- Authority
- CN
- China
- Prior art keywords
- praseodymium
- ammonia
- bicarbonate
- hours
- grain
- 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.)
- Granted
Links
Images
Abstract
The invention relates to a method for preparing multihole sheet large-grain praseodymium oxide, which belongs to the field of a material preparation process. The method comprises the following steps of: preparing an ammonium bicarbonate solution by using ammonium bicarbonate, ammonia and deionized water; adding a praseodymium nitrate solution to the ammonium bicarbonate solution to obtain a mixed solution of the ammonium bicarbonate, the ammonia and praseodymium nitrate; adding hydrogen peroxide to the mixed solution to generate praseodymium carbonate peroxide precipitate; aging for 24-48 hours; filtering and washing the praseodymium carbonate peroxide precipitate; burning at the temperature of 900-1200 DEG C, and preserving the temperature for 4 hours to obtain a multihole sheet large-grain praseodymium oxide product which has central grain diameter D50 of 20-35 micrometers, uniform grain and good flowability.
Description
Technical field
The present invention relates to a kind of method for preparing porous flake macrobead Praseodymium trioxide, belong to a kind of material preparation process.
Background technology
Praseodymium 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 Praseodymium trioxide.CN101633515A provides a kind of large-proportion praseodymium oxide method, and take praseodymium chloride as feed liquid, bicarbonate of ammonia is precipitation agent, precipitation temperature is precipitated greater than 90 ℃, through calcination, obtain large proportion macrobead Praseodymium trioxide product, but Praseodymium trioxide product particle globule size is not reported; 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 different 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
50Preparation method for the porous flake macrobead Praseodymium trioxide of 20-35 μ m.
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 praseodymium nitrate solution of 1.59mol/L, bicarbonate of ammonia and praseodymium nitrate mol ratio are 1: 0.014, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; Add concentration in the mixing solutions and be 30% hydrogen peroxide, praseodymium nitrate and hydrogen peroxide mol ratio are 1: 8.55, react 1.5 hours, ageing 24-48 hour, obtain peroxide praseodymium carbonate precipitation, with washing of precipitate, filtration, calcination temperature is 900-1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50Be 20-35 μ m, the porous flake macrobead Praseodymium trioxide product of uniform particles, good fluidity.
The invention effect
Peroxide praseodymium carbonate precipitation digestion time and calcination temperature are that preparation porous flake macrobead Praseodymium trioxide is crucial among the present invention, among the peroxide praseodymium carbonate preparation method, digestion time was less than 4 hours, peroxide praseodymium carbonate deposit seeds is very thin, sad filter, static ageing obtained macrobead peroxide praseodymium carbonate more than 24 hours, the peroxide praseodymium carbonate is under 900-1200 ℃ at calcination temperature, obtains medium particle diameter D
50Be the Praseodymium trioxide product of 20-35 μ m, control peroxide praseodymium carbonate precipitates digestion time and calcination temperature, can prepare the porous flake macrobead Praseodymium trioxide product of varying particle size, uniform particles, good fluidity, and this technique is convenient to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the XRD figure of porous flake macrobead Praseodymium trioxide of the present invention;
Fig. 2 is the particle size distribution figure of porous flake macrobead Praseodymium trioxide of the present invention;
Fig. 3 is the SEM figure of porous flake macrobead Praseodymium 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 40ml concentration is the praseodymium nitrate solution of 1.59mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; Add 56ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 1.5 hours, ageing 28 hours obtains peroxide praseodymium carbonate precipitation, and with sedimentation and filtration, washing, calcination temperature is 900 ℃, is incubated 4h, obtains medium particle diameter D
50It is the porous flake macrobead Praseodymium trioxide of 24.93 μ m.
Embodiment 2
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 40ml concentration is the praseodymium nitrate solution of 1.59mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; Add 56ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 1.5 hours, ageing 32 hours obtains peroxide praseodymium carbonate precipitation, and with sedimentation and filtration, washing, calcination temperature is 1000 ℃, is incubated 4h, obtains medium particle diameter D
50It is the porous flake macrobead Praseodymium trioxide of 28.34 μ m.
Embodiment 3
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 40ml concentration is the praseodymium nitrate solution of 1.59mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; Add 56ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 1.5 hours, ageing 44 hours obtains peroxide praseodymium carbonate precipitation, and with sedimentation and filtration, washing, calcination temperature is 1100 ℃, is incubated 4h, obtains medium particle diameter D
50It is the porous flake macrobead Praseodymium trioxide of 30.84 μ m.
Embodiment 4
Adding 350g bicarbonate of ammonia, 300ml concentration are 28% ammoniacal liquor and deionized water 520ml in reactor, and adding 40ml concentration is the praseodymium nitrate solution of 1.59mol/L again, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; Add 56ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 1.5 hours, ageing 48 hours obtains peroxide praseodymium carbonate precipitation, and with sedimentation and filtration, washing, calcination temperature is 1200 ℃, is incubated 4h, obtains medium particle diameter D
50It is the porous flake macrobead Praseodymium trioxide of 34.85 μ m.
Claims (1)
1. the method for preparing porous flake macrobead Praseodymium trioxide, it is characterized in that, add respectively bicarbonate of ammonia, concentration in the reactor and be 28% ammoniacal liquor and deionized water, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the praseodymium nitrate solution of 1.59mol/L, bicarbonate of ammonia and praseodymium nitrate mol ratio are 1: 0.014, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; Add concentration in the mixing solutions and be 30% hydrogen peroxide, praseodymium nitrate and hydrogen peroxide mol ratio are 1: 8.55, react 1.5 hours, ageing 24-48 hour, generate peroxide praseodymium carbonate precipitation, with washing of precipitate, filtration, calcination temperature is 900-1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50Be 20-35 μ m, the porous flake macrobead Praseodymium trioxide product of uniform particles, good fluidity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210382926.2A CN103011231B (en) | 2012-09-22 | 2012-09-22 | Method for preparing multihole sheet large-grain praseodymium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210382926.2A CN103011231B (en) | 2012-09-22 | 2012-09-22 | Method for preparing multihole sheet large-grain praseodymium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103011231A true CN103011231A (en) | 2013-04-03 |
| CN103011231B CN103011231B (en) | 2014-12-03 |
Family
ID=47960414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210382926.2A Active CN103011231B (en) | 2012-09-22 | 2012-09-22 | Method for preparing multihole sheet large-grain praseodymium oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103011231B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114082413A (en) * | 2021-11-19 | 2022-02-25 | 中国科学院城市环境研究所 | Praseodymium oxide catalyst and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7504356B1 (en) * | 2006-02-17 | 2009-03-17 | University Of Central Florida Research Foundation, Inc. | Nanoparticles of cerium oxide having superoxide dismutase activity |
| CN102502760A (en) * | 2011-10-28 | 2012-06-20 | 内蒙古科技大学 | Method for preparing large-particle and flaky praseodymium neodymium oxide |
-
2012
- 2012-09-22 CN CN201210382926.2A patent/CN103011231B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7504356B1 (en) * | 2006-02-17 | 2009-03-17 | University Of Central Florida Research Foundation, Inc. | Nanoparticles of cerium oxide having superoxide dismutase activity |
| CN102502760A (en) * | 2011-10-28 | 2012-06-20 | 内蒙古科技大学 | Method for preparing large-particle and flaky praseodymium neodymium oxide |
Non-Patent Citations (4)
| Title |
|---|
| C.A.D.S. QUEIROZ ET AL.: "《Synthesis and thermoanalytical characterization of samarium peroxocarbonate》", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| CARLOS A. DA S. QUEIROZ ET AL.: "《Thermoanalytical characterization of neodymium peroxicarbonate》", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| M.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》 * |
| 沈旭等: "《化学选矿技术》", 31 July 2011, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114082413A (en) * | 2021-11-19 | 2022-02-25 | 中国科学院城市环境研究所 | Praseodymium oxide catalyst and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103011231B (en) | 2014-12-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103539210B (en) | A kind of preparation method of cobalt molybdate crystallite | |
| CN102580721B (en) | Method for preparing TiO2/BiVO4 composite photocatalyst by MH method | |
| KR101738498B1 (en) | Method for preparing nickel-cobalt-manganese hydroxide | |
| CN103253717A (en) | Method for preparing small-size nickel-cobalt lithium manganate precursor | |
| CN103449534B (en) | A kind of take ionic liquid as the method that template prepares magnetic nano-particle | |
| CN102115214B (en) | Method for preparing small-particle-size cobalt carbonate | |
| CN105417570A (en) | Method for preparing spinel-type complex oxide through co-precipitation, homogenization and spray drying | |
| CN104671289B (en) | A kind of Fe2O3Nanometer sheet and preparation method thereof | |
| CN103833086B (en) | A kind of preparation method of sheet ferric oxide | |
| CN105498732A (en) | Magnetic nano-imprinted compound adsorbent as well as preparation method and application thereof | |
| CN102992379B (en) | Method for preparing spherical macro-granular neodymium oxide | |
| CN103011231B (en) | Method for preparing multihole sheet large-grain praseodymium oxide | |
| CN101973538A (en) | Method for preparing iron phosphate | |
| CN102962470A (en) | Method for preparing spherical ultrafine nickel powder at room temperature | |
| CN105271443A (en) | Method for preparing flaky nano CoO or Co3O4 through assistant microwave heating | |
| CN102583493A (en) | Method for preparing large-particle Ce rich rare earth oxide | |
| CN105390691A (en) | Method for preparing spherical nickel cobalt lithium manganate by liquid phase template method | |
| CN101591176A (en) | A kind of synthetic Gd 3Ga 5O 12(GGG) the nanocrystalline method of crystalline ceramics | |
| CN103058724B (en) | Preparation method of large-particle gadolinium oxide | |
| CN102992381B (en) | Method for preparing macrogranular ytterbium oxide | |
| CN103204554A (en) | Method for preparing spherical nickel hydroxide | |
| CN103058256B (en) | Method for preparing large-granule dysprosium oxide | |
| CN103614139B (en) | Reverse co-precipitation is adopted to prepare Gd 2ti 2o 7: the method for Ce nano-luminescent powder body | |
| CN103058255B (en) | Method for preparing large-granule erbium oxide | |
| CN102120618A (en) | Preparation method of high-tap density manganese carbonate |
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 |