CN103011231B - Method for preparing multihole sheet large-grain praseodymium oxide - Google Patents
Method for preparing multihole sheet large-grain praseodymium oxide Download PDFInfo
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- CN103011231B CN103011231B CN201210382926.2A CN201210382926A CN103011231B CN 103011231 B CN103011231 B CN 103011231B CN 201210382926 A CN201210382926 A CN 201210382926A CN 103011231 B CN103011231 B CN 103011231B
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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 of 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 scientific and technological development, for packing material, spray material, special magnetic material, neutron-absorbing material aspect macrobead Praseodymium trioxide, have great application prospect.CN101633515A provides a kind of large-proportion praseodymium oxide method, take praseodymium chloride as feed liquid, and bicarbonate of ammonia is precipitation agent, precipitation temperature is greater than 90 ℃, is precipitated, 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 praseodymium chloride neodymium as feed liquid, bicarbonate of ammonia is precipitation agent, two kinds of different precipitation temperatures, and it is spherical obtaining pattern and sheet, medium particle diameter are the Praseodymium trioxide neodymium product of 25-45 μ m.
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: 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 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; To adding concentration in mixing solutions, be 30% hydrogen peroxide, praseodymium nitrate and hydrogen peroxide mol ratio are 1: 8.55, react 1.5 hours, ageing 24-48 hour, obtains peroxide praseodymium carbonate precipitation, by washing of precipitate, filtration, calcination temperature is 900-1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50for 20-35 μ m, the porous flake macrobead Praseodymium trioxide product of uniform particles, good fluidity.
Invention effect
In the present invention, peroxide praseodymium carbonate precipitation digestion time and calcination temperature are to prepare porous flake macrobead Praseodymium trioxide key, in peroxide praseodymium carbonate preparation method, digestion time is less than 4 hours, peroxide praseodymium carbonate deposit seeds is very thin, sad filter, static ageing more than 24 hours, obtains macrobead peroxide praseodymium carbonate, peroxide praseodymium carbonate is at 900-1200 ℃ at calcination temperature, obtains medium particle diameter D
50for the Praseodymium trioxide product of 20-35 μ m, control peroxide praseodymium carbonate precipitation digestion time and calcination temperature, can prepare the porous flake macrobead Praseodymium trioxide product of varying particle size, uniform particles, good fluidity, this technique is convenient to realize suitability for industrialized production.
Accompanying drawing explanation
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
In reactor, add ammoniacal liquor and deionized water 520ml that 350g bicarbonate of ammonia, 300ml concentration are 28%, then to add 40ml concentration be the praseodymium nitrate solution of 1.59mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; To adding 56ml concentration in mixing solutions, be 30% hydrogen peroxide, react 1.5 hours, ageing 28 hours, obtains peroxide praseodymium carbonate precipitation, and by sedimentation and filtration, washing, calcination temperature is 900 ℃, and insulation 4h, obtains medium particle diameter D
50it is the porous flake macrobead Praseodymium trioxide of 24.93 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 40ml concentration be the praseodymium nitrate solution of 1.59mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; To adding 56ml concentration in mixing solutions, be 30% hydrogen peroxide, react 1.5 hours, ageing 32 hours, obtains peroxide praseodymium carbonate precipitation, and by sedimentation and filtration, washing, calcination temperature is 1000 ℃, and insulation 4h, obtains medium particle diameter D
50it is the porous flake macrobead Praseodymium trioxide of 28.34 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 40ml concentration be the praseodymium nitrate solution of 1.59mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; To adding 56ml concentration in mixing solutions, be 30% hydrogen peroxide, react 1.5 hours, ageing 44 hours, obtains peroxide praseodymium carbonate precipitation, and by sedimentation and filtration, washing, calcination temperature is 1100 ℃, and insulation 4h, obtains medium particle diameter D
50it is the porous flake macrobead Praseodymium trioxide of 30.84 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 40ml concentration be the praseodymium nitrate solution of 1.59mol/L, obtain the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and praseodymium nitrate; To adding 56ml concentration in mixing solutions, be 30% hydrogen peroxide, react 1.5 hours, ageing 48 hours, obtains peroxide praseodymium carbonate precipitation, and by sedimentation and filtration, washing, calcination temperature is 1200 ℃, and insulation 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, 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 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; To adding concentration in mixing solutions, be 30% hydrogen peroxide, praseodymium nitrate and hydrogen peroxide mol ratio are 1: 8.55, react 1.5 hours, ageing 24-48 hour, generates peroxide praseodymium carbonate precipitation, by washing of precipitate, filtration, calcination temperature is 900-1200 ℃, is incubated 4 hours, obtains medium particle diameter D
50for 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 |
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| CN201210382926.2A CN103011231B (en) | 2012-09-22 | 2012-09-22 | Method for preparing multihole sheet large-grain praseodymium oxide |
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| CN103011231A CN103011231A (en) | 2013-04-03 |
| CN103011231B true CN103011231B (en) | 2014-12-03 |
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| 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 |
| CN115957235A (en) * | 2022-12-20 | 2023-04-14 | 山东省海洋科学研究院(青岛国家海洋科学研究中心) | Praseodymium oxide particle, preparation method and application thereof, and bacteriostatic agent |
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| US7504356B1 (en) * | 2006-02-17 | 2009-03-17 | University Of Central Florida Research Foundation, Inc. | Nanoparticles of cerium oxide having superoxide dismutase activity |
| CN102502760B (en) * | 2011-10-28 | 2014-12-03 | 内蒙古科技大学 | Method for preparing large-particle and flaky praseodymium neodymium oxide |
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