CN103058255B - Method for preparing large-granule erbium oxide - Google Patents
Method for preparing large-granule erbium oxide Download PDFInfo
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- CN103058255B CN103058255B CN201210386974.9A CN201210386974A CN103058255B CN 103058255 B CN103058255 B CN 103058255B CN 201210386974 A CN201210386974 A CN 201210386974A CN 103058255 B CN103058255 B CN 103058255B
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Abstract
The invention relates to a method for preparing large-granule erbium oxide, belonging to a material preparation technique. The method comprises the following steps: preparing ammonium bicarbonate, ammonia water and deionized water into an ammonium bicarbonate solution; adding an erbium chloride solution into the ammonium bicarbonate solution to obtain a mixed solution of ammonium bicarbonate, ammonia water and erbium chloride; adding oxydol into the mixed solution, standing for aging for 12 hours to start generating an erbium peroxycarbonate precipitate, and aging for 24-48 hours; and filtering the precipitate, washing, and firing at 900-1200 DEG C for 4 hours to obtain the lamina-constituted efflorescent large-granule erbium oxide product with uniform granules and favorable flowability, of which the central granule size D50 is 80-90 mu m.
Description
Technical field
The present invention relates to a kind of method of preparing macrobead Erbium trioxide, belong to a kind of material preparation process.
Background technology
Erbium trioxide is mainly as YIG stone additive and nuclear reactor control material, also for the manufacture of extraordinary fluorescent glass and the ultrared glass of absorption, also as glass colorant.The photoelectric characteristic of Erbium trioxide, makes it have higher using value in photonics, optics and communication science field; Macrobead Erbium trioxide is applied to coated material, and the corrosion resistance that it is good is expected to become good erosion shield; Its high refractive index, high-clarity are used for the devices such as solar cell as reflectance coating; Erbium trioxide coating is for fusion reactor blanket hydrogen resistance coating, erbium oxide hydrogen resistance coating material is applied in thermonuclear reactor experiment conventionally, and its effect is anti-tritium diffusion, taking activation martensitic steel or austenitic steel as matrix, on matrix, taking Fe-Er as intermediate metal, on it, apply Erbium trioxide coating.
Summary of the invention
The object of the present invention is to provide a kind of uniform particles, good fluidity, medium particle diameter D
50for 80-90 μ m, pattern form flower-shaped macrobead Erbium trioxide preparation method by thin slice.
Technical solution: the present invention adds respectively ammoniacal liquor and the deionized water that bicarbonate of ammonia, concentration are 28% in reactor, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the Erbium trichloride solution of 1.71mol/L, bicarbonate of ammonia and Erbium trichloride mol ratio are 1: 0.05, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Be 30% hydrogen peroxide to adding concentration in mixing solutions, Erbium trichloride and hydrogen peroxide mol ratio are 1: 4.8, react 1.5 hours, static ageing starts to produce peroxide carbonic acid erbium precipitation for 12 hours, and ageing 24-48 hour obtains peroxide carbonic acid erbium precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50for 80-90 μ m, even particle distribution, good fluidity, pattern form flower-shaped macrobead Erbium trioxide by thin slice.
Invention effect
In the present invention, peroxide carbonic acid erbium precipitation digestion time and calcination temperature are crucial, digestion time is the key factor that determines peroxide carbonic acid erbium granularity, and static digestion time reaches 12 hours, starts to produce peroxide carbonic acid erbium precipitation, static ageing more than 24 hours, obtains macrobead peroxide carbonic acid erbium; Peroxide carbonic acid erbium calcination temperature selects suitability for industrialized production erbium oxalate or carbonic acid erbium to be decomposed into the temperature range of Erbium trioxide, be convenient to suitability for industrialized production Device-General, calcination temperature is 900-1200 DEG C, according to the market requirement, and can suitability for industrialized production uniform particles, good fluidity, medium particle diameter D
50for 80-90 μ m, pattern form flower-shaped macrobead Erbium trioxide by thin slice.
Brief description of the drawings
Fig. 1 is the XRD figure of macrobead Erbium trioxide of the present invention;
Fig. 2 is the particle size distribution figure of macrobead Erbium trioxide of the present invention;
Fig. 3 is the SEM figure of macrobead Erbium trioxide of the present invention.
Embodiment
Embodiment 1
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300m1 concentration are 28%, then to add 130m1 concentration be the Erbium trichloride solution of 1.71mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Be 30% hydrogen peroxide to adding 110ml concentration in mixing solutions, react 1.5 hours, static ageing starts to produce peroxide carbonic acid erbium precipitation for 12 hours, ageing 28 hours, obtains peroxide carbonic acid erbium precipitation, by sedimentation and filtration, washing, calcination temperature is 900 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead Erbium trioxide of 80.35 μ m.
Embodiment 2
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 130ml concentration be the Erbium trichloride solution of 1.71mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Be 30% hydrogen peroxide to adding 110ml concentration in mixing solutions, react 1.5 hours, static ageing starts to produce peroxide carbonic acid erbium precipitation for 12 hours, ageing 36 hours, obtains peroxide carbonic acid erbium precipitation, by sedimentation and filtration, washing, calcination temperature is 1000 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead Erbium trioxide of 82.13 μ m.
Embodiment 3
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 130ml concentration be the Erbium trichloride solution of 1.71mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Be 30% hydrogen peroxide to adding 110ml concentration in mixing solutions, react 1.5 hours, static ageing starts to produce peroxide carbonic acid erbium precipitation for 12 hours, ageing 44 hours, obtains peroxide carbonic acid erbium precipitation, by sedimentation and filtration, washing, calcination temperature is 1100 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead Erbium trioxide of 87.64 μ m.
Embodiment 4
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 130ml concentration be the Erbium trichloride solution of 1.71mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Be 30% hydrogen peroxide to adding 110ml concentration in mixing solutions, react 1.5 hours, static ageing starts to produce peroxide carbonic acid erbium precipitation for 12 hours, ageing 48 hours, obtains peroxide carbonic acid erbium precipitation, by sedimentation and filtration, washing, calcination temperature is 1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50it is the macrobead Erbium trioxide of 90.46 μ m.
Claims (1)
1. prepare the method for macrobead Erbium trioxide, it is characterized in that, in reactor, add respectively ammoniacal liquor and the deionized water that bicarbonate of ammonia, concentration are 28%, the mol ratio of bicarbonate of ammonia, ammoniacal liquor and deionized water is 1: 1: 6.27, adding concentration is the Erbium trichloride solution of 1.71mol/L, bicarbonate of ammonia and Erbium trichloride mol ratio are 1: 0.05, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and Erbium trichloride; Be 30% hydrogen peroxide to adding concentration in mixing solutions, Erbium trichloride and hydrogen peroxide mol ratio are 1: 4.8, react 1.5 hours, static ageing starts to produce peroxide carbonic acid erbium precipitation for 12 hours, and ageing 24-48 hour obtains peroxide carbonic acid erbium precipitation, by sedimentation and filtration, washing, calcination temperature is 900-1200 DEG C, is incubated 4 hours, obtains medium particle diameter D
50for 80-90 μ m, even particle distribution, good fluidity, pattern form flower-shaped macrobead Erbium trioxide by thin slice.
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| CN103058255B true CN103058255B (en) | 2014-12-03 |
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| CN108264080B (en) * | 2018-04-08 | 2019-11-12 | 常州市卓群纳米新材料有限公司 | A kind of method that reaction ball milling method prepares nano oxidized erbium |
| CN111592028A (en) * | 2020-04-24 | 2020-08-28 | 广西科学院 | Microwave calcination preparation method of rare earth oxide superfine powder |
Citations (3)
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| CN101362605A (en) * | 2008-08-11 | 2009-02-11 | 中国科学院长春应用化学研究所 | Rare-earth nano oxide preparation method |
| 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 |
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Patent Citations (3)
| 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 |
| CN101362605A (en) * | 2008-08-11 | 2009-02-11 | 中国科学院长春应用化学研究所 | Rare-earth nano oxide preparation method |
| 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 (7)
| Title |
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| "Solubility behavior of rare earths with ammonium carbonate and ammonium carbonate plus ammonium hydroxide: Precipitation of their peroxicarbonates";M.E. de Vasconcellos et al.;《Journal of Alloys and Compounds》;20080228;第451卷(第1-2期);第426–428页 * |
| "Synthesis and thermoanalytical characterization of samarium peroxocarbonate";C.A.d.S. Queiroz et al.;《Journal of Alloys and Compounds》;20040714;第374卷(第1-2期);第401-404页 * |
| "Thermoanalytical characterization of neodymium peroxicarbonate";Carlos A. da S. Queiroz et al.;《Journal of Alloys and Compounds》;20021231;第344卷;第32-35页 * |
| C.A.d.S. Queiroz et al.."Synthesis and thermoanalytical characterization of samarium peroxocarbonate".《Journal of Alloys and Compounds》.2004,第374卷(第1-2期),第401-404页. * |
| Carlos A. da S. Queiroz et al.."Thermoanalytical characterization of neodymium peroxicarbonate".《Journal of Alloys and Compounds》.2002,第344卷第32-35页. * |
| 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》.2008,第451卷(第1-2期),第426–428页. * |
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