CN116102049A - Preparation method of high-purity nano neodymium oxide - Google Patents
Preparation method of high-purity nano neodymium oxide Download PDFInfo
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- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 title claims abstract description 186
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 20
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 20
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 18
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 18
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 150000001206 Neodymium Chemical class 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000011068 loading method Methods 0.000 claims abstract description 3
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 claims description 14
- 239000002245 particle Substances 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 5
- 239000005357 flat glass Substances 0.000 abstract description 3
- 239000011858 nanopowder Substances 0.000 description 17
- 229910017493 Nd 2 O 3 Inorganic materials 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 238000007873 sieving Methods 0.000 description 14
- 239000002105 nanoparticle Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 229940113125 polyethylene glycol 3000 Drugs 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 229940113116 polyethylene glycol 1000 Drugs 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 229910052779 Neodymium Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- -1 neodymium ions Chemical class 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 229910000583 Nd alloy Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 1
- RKLPWYXSIBFAJB-UHFFFAOYSA-N [Nd].[Pr] Chemical compound [Nd].[Pr] RKLPWYXSIBFAJB-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 229910001172 neodymium magnet Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000006353 oxyethylene group Chemical group 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention belongs to the technical field of preparation of window glass doped materials, and particularly relates to a preparation method of high-purity nano neodymium oxide, which comprises the following steps: (1) preparing neodymium salt solution with the concentration of 0.25-0.35 mol/L; (2) Slowly pouring polyethylene glycol 2000 accounting for 4% -6% of the theoretical mass of a final neodymium oxide product into a neodymium salt solution, and fully dispersing to obtain a mixed solution; (3) Dripping 0.5-0.7mol/L ammonium bicarbonate solution into the mixed solution in the step (2) at the speed of 2-10L/min, stirring for 0.3-0.7h in a reaction kettle after dripping, aging for 8-13h, filtering, washing with water, loading the filtered product into a pot, and calcining for 3-5h at 800-950 ℃ to obtain the high-purity nano neodymium oxide, wherein the ammonium bicarbonate dosage is 3-4.5 times of the molar mass of neodymium salt. The nano neodymium oxide particles prepared by the method have high purity, uniform particle size and good dispersibility.
Description
Technical Field
The invention belongs to the technical field of preparation of window glass doped materials, and particularly relates to a preparation method of high-purity nano neodymium oxide.
Background
Neodymium oxide is one of rare earth oxides with wider application, and is mainly used for producing high-performance neodymium-iron-boron permanent magnet materials in the current market, and praseodymium-neodymium alloy is the main material of a permanent magnet motor; neodymium oxide is also often incorporated into yttrium aluminum garnet for laser emitters; in addition, the absorption spectrum line of neodymium ions is special, and the neodymium ions show different colors under different illumination, so that the reduction of yellow light in the spectrum can improve the glare reduction effect, neodymium oxide is also often added into glass, and the requirements on the particle fineness, uniformity and purity of neodymium oxide are quite strict because the transmittance of the glass is achieved and certain yellow light is absorbed. The purity of the neodymium oxide prepared at present is mostly 3N and 4N, and the manufacturing cost is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of high-purity nano neodymium oxide, which has the characteristics of low preparation cost, uniform particles and good dispersibility.
In order to achieve the purpose of the invention, the technical scheme adopted is as follows: the preparation process of high purity nanometer neodymium oxide includes the following steps:
(1) Preparing neodymium salt solution with the concentration of 0.25-0.35 mol/L;
(2) Slowly pouring polyethylene glycol 2000 accounting for 4% -6% of the theoretical mass of a final neodymium oxide product into a neodymium salt solution, and fully dispersing to obtain a mixed solution;
(3) Dripping 0.5-0.7mol/L ammonium bicarbonate solution into the mixed solution in the step (2) at the speed of 2-10L/min, stirring for 0.3-0.7h in a reaction kettle after dripping, aging for 8-14h, filtering, washing with water, loading the filtered product into a pot, and calcining at 800-950 ℃ for 3-5h to obtain the high-purity nano neodymium oxide, wherein the purity can reach 5N generally, and the ammonium bicarbonate dosage is 3-4.5 times of the molar mass of neodymium salt.
The neodymium salt in step (1) is preferably neodymium chloride.
The concentration of the neodymium salt solution in the step (1) is preferably 0.3mol/L.
The polyethylene glycol 2000 is preferably used in step (2) in an amount of 5% of the theoretical mass of the final neodymium oxide product.
The concentration of the precipitant in step (3) is preferably 0.6mol/L.
The aging time in step (3) is preferably 10 to 12 hours.
The calcination temperature in step (3) is preferably 850 to 950 ℃.
The calcination time in step (3) is preferably 4 to 4.5 hours.
Compared with the prior art, the nano neodymium oxide particles prepared by the method have high purity, uniform particle size and good dispersibility, and are a good window glass doping material.
Drawings
FIG. 1 is an SEM image of neodymium oxide obtained in example 1.
FIG. 2 is an SEM image of neodymium oxide obtained by adjusting the concentration of neodymium chloride to 0.2mol/L in comparative example 1;
FIG. 3 is an SEM image of neodymium oxide obtained at 700g of polyethylene glycol 2000 in comparative example 2;
FIG. 4 is an SEM image of neodymium oxide obtained in comparative example 3;
FIG. 5 is an SEM image of neodymium oxide obtained in comparative example 5;
FIG. 6 is an SEM image of neodymium oxide obtained in comparative example 6 with ammonium bicarbonate concentrations of 0.4mol/L, respectively.
Detailed Description
The invention is further described in detail below in connection with the examples:
example 1:
preparation of 10kg of Neodymium oxide
(1) Taking 297L of 0.3mol/L neodymium chloride solution;
(2) Dissolving 500g of polyethylene glycol 2000 in 10L of pure water, slowly pouring into a neodymium chloride solution, and stirring for 30min to obtain a mixed solution;
(3) Dissolving 18.77kg of ammonium bicarbonate in 396L of pure water, namely, 0.6mol/L of ammonium bicarbonate solution, dripping the ammonium bicarbonate solution into the mixed solution in the step (2) at the speed of 4L/min, and closing stirring after 60min of dripping;
(4) Aging for 12h, and washing with pure water at 70 ℃ or above for 6h after aging;
(5) Washing with water, drying, filling into a bowl, and calcining at 950 ℃ for 4 hours;
sieving with 60 mesh sieve to obtain light blue neodymium oxide product with yield of 94%, BET of 25.25m 2 Per g, D10:0.107 μm, D50:0.276 μm, D90:0.806 μm (see Table 1 for details), the packing with inert gas ensures that the finished neodymium oxide product is not contaminated by air oxidation.
Table 1:
comparative example 1
Preparation of 10kg of Neodymium oxide
In comparison with the method for preparing nano neodymium oxide in example 1, the concentration of neodymium chloride in the step (1) was adjusted to 0.2mol/L, 0.4mol/L and 0.6mol/L, and the other conditions were the same as in example 1. Namely, when the molar concentration is 0.2mol/L, 0.4mol/L and 0.6mol/L, neodymium oxide nano-particles with uniform particles and uniform morphology cannot be obtained. Wherein the yield of the nano powder prepared by neodymium chloride with the molar concentration of 0.2mol/L is 94% after sieving by a 60-mesh sieve, and D10:0.15 μm, D50:0.338 μm, D90:1.079 μm, BET 20.15 μm 2 /g,Nd 2 O 3 REO 99.999%; the yield of the nano powder prepared by neodymium chloride with the molar concentration of 0.4mol/L is 92% after sieving by a 60-mesh sieve, and D10:0.187 μm, D50:0.391 μm, D90:0.998 μm, BET 21.67 μm 2 /g，Nd 2 O 3 REO 99.999%; the yield of the nano powder prepared from 0.6mol/L neodymium chloride is 92% after sieving by a 60-mesh sieve, D10:0.211 μm, D50:0.402 μm, D90:1.203 μm, BET 18.85m 2 /g,Nd 2 O 3 /REO:99.999％。
It is explained that the concentration of neodymium chloride precursor prepared by the neodymium oxide nano powder prepared in the invention is optimal to be 0.3mol/L.
Comparative example 2
Preparation of 10kg of Neodymium oxide
In comparison with the preparation method of nano neodymium oxide in example 1, 300g and 700g of polyethylene glycol 2000 in the step (2) are respectively dissolved in 10L of pure water, and then slowly poured into neodymium chloride solution and stirred for 30min, and other conditions are the same as in example 1. The obtained neodymium oxide nano powder particles have uneven dispersibility and certain cohesiveness or a small amount of flakes. Wherein, the polyethylene glycol 2000 takes 300g of the obtained experimental result, and the yield is 95% after sieving by a 60-mesh sieve, D10:0.29 μm, D50:0.791 μm, D90:1.704 μm, BET 14.62m 2 /g,Nd 2 O 3 REO 99.999%; wherein, the polyethylene glycol 2000 takes 700g of the obtained experimental result, and the yield is 93% after sieving by a 60-mesh sieve, D10:0.161 μm, D50:0.264 μm, D90:0.87 μm, BET 26.15m 2 /g,Nd 2 O 3 /REO:99.999％；
The amount of surfactant used in the neodymium oxide nano-powder prepared in the present invention was 500g.
Comparative example 3
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of nano neodymium oxide in the embodiment 1, the preparation method comprises the steps of adjusting the polyethylene glycol 2000 in the step (2), dissolving in 10L of pure water, slowly pouring the solution into the prepared ammonium bicarbonate solution, uniformly mixing, dripping the solution into the neodymium chloride solution at the speed of 4L/min, and closing stirring after 60min of dripping, wherein other conditions are the same as the embodiment 1. As a result, the obtained neodymium oxide nano powder particles have poor dispersibility, nonuniform particles and large-area adhesion. The obtained neodymium oxide nano powder D10:0.187 μm, D50:0.396 μm, D90:1.315 μm, BET 21.33m 2 /g,Nd 2 O 3 /REO:99.999％。
The surfactant used in the neodymium oxide nano-powder prepared in the present invention should be added to the neodymium salt solution.
Comparative example 4
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of nano neodymium oxide in the embodiment 1, the surfactant in the step (2) is respectively polyethylene glycol 1000, polyethylene glycol 3000 and polyethylene glycol 20000, and other conditions are the same as those in the embodiment 1, when the polyethylene glycol 1000, the polyethylene glycol 3000 and the polyethylene glycol 20000 are respectively dissolved in 10L of pure water, the solution of neodymium chloride is poured into and stirred, and when the solution enters a washing stage, the washing speed of the polyethylene glycol 1000 is faster, the obtained particles are larger, and the dispersion effect is weaker than that of the polyethylene glycol 2000, the polyethylene glycol 3000 and the polyethylene glycol 20000; polyethylene glycol 2000, polyethylene glycol 3000 water washing effect is optimal; polyethylene glycol 20000 has a thicker hydrated oxyethylene layer, can greatly reduce van der Waals force among particles, has good dispersion effect, but has lower efficiency in the water washing process, and polyethylene glycol 3000 and polyethylene glycol 20000 have high manufacturing cost relative to polyethylene glycol 2000, so the polyethylene glycol 2000 is selected to be beneficial to production, and has low cost.
Comparative example 5
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of nano neodymium oxide in the embodiment 1, in the adjustment step (3), the prepared neodymium chloride solution is dripped into the ammonium bicarbonate solution at the speed of 4L/min under other conditionsThe same as in example 1. The obtained neodymium oxide nano particles have uneven dispersivity and have an area of adhesion or a small amount of flakes. The obtained neodymium oxide nano powder D10:0.245 μm, D50:0.621 μm, D90:1.709 μm, BET 18.15m 2 /g,Nd 2 O 3 /REO:99.999％。
Comparative example 6
Preparation of 10kg of Neodymium oxide
In comparison with the preparation method of nano neodymium oxide in example 1, the precipitant ammonium bicarbonate in the step (3) is regulated into sodium carbonate or sodium hydroxide solution in equimolar quantity, and other conditions are the same as in example 1. As a result, the content of sodium ions in the obtained neodymium oxide nano powder is too high, and sodium ions in the powder cannot be completely removed. Wherein the yield of the nano neodymium oxide powder particles obtained after the precipitant is changed into sodium carbonate is 91% after 60-mesh sieving, D10:0.224 μm, D50:0.481 μm, D90:1.362 μm, BET 14.23m 2 /g; wherein the yield of the nano neodymium oxide powder particles obtained after the precipitant is changed into sodium hydroxide is 92% after 60-mesh sieving, D10:0.209 μm, D50:0.425 μm, D90:1.117 μm, BET 16.33m 2 /g, na in the product 2 O mass content 0.11%.
The invention shows that the purity of the neodymium oxide nano powder prepared by the invention can be improved by ammonium bicarbonate precipitation.
Comparative example 7
Preparation of 10kg of Neodymium oxide
In comparison with the preparation method of nano neodymium oxide in example 1, the adjustment of pure water amounts of 1188L, 594L and 297L in the step (3), that is, ammonium bicarbonate concentrations of 0.2mol/L, 0.4mol/L and 0.8mol/L, respectively, are otherwise the same as in example 1, and neodymium oxide nano particles with good dispersibility are not obtained when pure water amounts of 1188L, 594L and 297L are used. Wherein, the yield of the nano neodymium oxide obtained by sieving the nano neodymium oxide with 60 meshes under the ammonium bicarbonate concentration of 0.2mol/L is 91%, D10:0.145 μm, D50:0.32 μm, D90:0.861 μm, BET 17.6m 2 /g,Nd 2 O 3 REO 99.999%; wherein, the yield of the nano neodymium oxide obtained by sieving the nano neodymium oxide with 60 meshes under the ammonium bicarbonate concentration of 0.4mol/L is 93 percent, D10:0.161 μm, D50:0.374 μm, D90：0.876μm，BET:19.29m 2 /g,Nd 2 O 3 REO 99.999%; wherein, the yield of the nano neodymium oxide obtained by sieving the nano neodymium oxide with 60 meshes under the ammonium bicarbonate concentration of 0.8mol/L is 93 percent, D10:0.155 μm, D50:0.392 μm, D90:0.926 μm, BET 18.52m 2 /g,Nd 2 O 3 /REO:99.999％。
Comparative example 8
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of the nano neodymium oxide in the embodiment 1, the aging time in the step (4) is respectively 2h, 6h and 24h, other conditions are the same as those in the embodiment 1, when the aging time is 2h and 6h, the washing speed is slower, the impurity content of the obtained neodymium oxide nano powder is too high, the washing speed is faster when the obtained neodymium oxide nano powder is aged for 24h, the obtained neodymium oxide nano ball particles grow larger, and the high-purity neodymium oxide nano particles cannot be obtained.
The aging time of the neodymium oxide nano powder particles prepared in the invention is about 12 hours.
Example 2
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of nano neodymium oxide in the example 1, the calcination temperature in the step (5) is adjusted to 800 ℃, 850 ℃ and 900 ℃, and as a result, the yield of the nano neodymium oxide burnt for 4 hours at 800 ℃ in the obtained neodymium oxide nano particles is 95% after sieving by a 60-mesh sieve, and D10:0.177 μm, D50:0.369 μm, D90:0.941 μm, BET 23.68m 2 /g,Nd 2 O 3 REO 99.999%; wherein, the yield of the nano neodymium oxide burnt for 4 hours at 850 ℃ is 95% after being sieved by a 60-mesh sieve, and D10:0.16 μm, D50:0.343 μm, D90:0.859 μm, BET 21.95m 2 /g,Nd 2 O 3 REO 99.999%; wherein, the yield of the nano neodymium oxide burnt for 4 hours at 900 ℃ is 93 percent after being sieved by a 60-mesh sieve, D10:0.141 μm, D50:0.388 μm, D90:0.904 μm, BET 22.6m 2 /g,Nd 2 O 3 /REO:99.999％。
Comparative example 9
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of nano neodymium oxide in the example 1, the calcination temperature of 100 in the step (5) is adjustedAs a result, the obtained neodymium oxide nano particles have no uniformity, the yield of the nano neodymium oxide burnt for 4 hours at 1000 ℃ is 91% after being sieved by a 60-mesh sieve, and D10:0.195 μm, D50:0.421 μm, D90:1.408 μm, BET 16.12 μm 2 /g,Nd 2 O 3 /REO:99.999％。
Comparative example 10
Preparation of 10kg of Neodymium oxide
Compared with the preparation method of the nano neodymium oxide in the embodiment 1, the firing time in the step (5) is respectively adjusted to be 2h and 6h, and the obtained neodymium oxide nano particles are unevenly dispersed and seriously agglomerated. Wherein, the yield of the neodymium oxide nano powder obtained by calcining at 950 ℃ for 2 hours is 93% after sieving by a 60-mesh sieve, and D10:0.192 μm, D50:0.417 μm, D90:0.106 μm, BET 21.66m 2 /g,Nd 2 O 3 REO 99.999%; wherein, the yield of the neodymium oxide nano powder obtained by calcining at 950 ℃ for 6 hours is 91% after sieving by a 60-mesh sieve, and D10:0.269 μm, D50:0.784 μm, D90:1.863 μm, BET 12.11m 2 /g,Nd 2 O 3 /REO:99.999％。
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme and the concept of the present invention, and should be covered by the scope of the present invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
Claims (7)
1. A preparation method of high-purity nano neodymium oxide is characterized in that: the method comprises the following steps:
(1) Preparing neodymium salt solution with the concentration of 0.25-0.35 mol/L;
(2) Slowly pouring polyethylene glycol 2000 accounting for 4% -6% of the theoretical mass of a final neodymium oxide product into a neodymium salt solution, and fully dispersing to obtain a mixed solution;
(3) Dripping 0.5-0.7mol/L ammonium bicarbonate solution into the mixed solution in the step (2) at the speed of 2-10L/min, stirring for 0.3-0.7h in a reaction kettle after dripping, aging for 8-13h, filtering, washing with water, loading the filtered product into a pot, and calcining for 3-5h at 800-950 ℃ to obtain the high-purity nano neodymium oxide, wherein the ammonium bicarbonate dosage is 3-4.5 times of the molar mass of neodymium salt.
2. The method for preparing high-purity nano neodymium oxide according to claim 1, wherein the method comprises the following steps: the neodymium salt in the step (1) is neodymium chloride.
3. The method for preparing high-purity nano neodymium oxide according to claim 1, wherein the method comprises the following steps: the concentration of the neodymium salt solution in the step (1) is 0.3mol/L.
4. The method for preparing high-purity nano neodymium oxide according to claim 1, wherein the method comprises the following steps: the polyethylene glycol 2000 dosage in the step (2) is 5% of the theoretical mass of the final neodymium oxide product.
5. The method for preparing high-purity nano neodymium oxide according to claim 1, wherein the method comprises the following steps: the concentration of the precipitant in the step (3) is 0.6mol/L.
6. The method for preparing high-purity nano neodymium oxide according to claim 1, wherein the method comprises the following steps: the aging time in the step (3) is 10-12h.
7. The method for preparing high-purity nano neodymium oxide according to claim 1, wherein the method comprises the following steps: the calcination temperature in the step (3) is 850-950 ℃ and the calcination time is 4-4.5h.
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