CN112723331B - Preparation method of high-purity nano neodymium phosphate powder - Google Patents
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- CN112723331B CN112723331B CN202011546992.XA CN202011546992A CN112723331B CN 112723331 B CN112723331 B CN 112723331B CN 202011546992 A CN202011546992 A CN 202011546992A CN 112723331 B CN112723331 B CN 112723331B
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- DZNFWGVDYGAMJB-UHFFFAOYSA-K neodymium(3+);phosphate Chemical compound [Nd+3].[O-]P([O-])([O-])=O DZNFWGVDYGAMJB-UHFFFAOYSA-K 0.000 title claims abstract description 45
- 239000000843 powder Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 44
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 23
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 22
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000000725 suspension Substances 0.000 claims abstract description 18
- UTWHRPIUNFLOBE-UHFFFAOYSA-H neodymium(3+);tricarbonate Chemical compound [Nd+3].[Nd+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O UTWHRPIUNFLOBE-UHFFFAOYSA-H 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- RCYIWFITYHZCIW-UHFFFAOYSA-N 4-methoxybut-1-yne Chemical compound COCCC#C RCYIWFITYHZCIW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 9
- 150000002910 rare earth metals Chemical class 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- 238000007792 addition Methods 0.000 claims description 5
- YQJSENALOOETOP-UHFFFAOYSA-K neodymium(3+) carbonate hydroxide Chemical compound [OH-].C([O-])([O-])=O.[Nd+3] YQJSENALOOETOP-UHFFFAOYSA-K 0.000 claims description 4
- 239000008118 PEG 6000 Substances 0.000 claims description 3
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 claims description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical group OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000011164 primary particle Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 description 2
- ZUNWSJIYNQRJAE-UHFFFAOYSA-K neodymium(3+) phosphate dihydrate Chemical compound O.O.P(=O)([O-])([O-])[O-].[Nd+3] ZUNWSJIYNQRJAE-UHFFFAOYSA-K 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001206 Neodymium Chemical class 0.000 description 1
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical group [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- ASJWVKODUIDSCN-UHFFFAOYSA-K dihydrogen phosphate neodymium(3+) Chemical compound P(=O)(O)(O)[O-].[Nd+3].P(=O)(O)(O)[O-].P(=O)(O)(O)[O-] ASJWVKODUIDSCN-UHFFFAOYSA-K 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000087 laser glass Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The preparation method of the high-purity nano neodymium phosphate powder comprises the following steps: (1) Adding neodymium carbonate, basic neodymium carbonate, neodymium oxide or neodymium hydroxide into deionized water or deionized water containing a dispersing agent, and stirring to obtain a neodymium-containing suspension; (2) Preparing a phosphoric acid solution, adding a strong acid solution into the phosphoric acid solution, and adding a dispersing agent; (3) And (3) adding a neodymium-containing suspension into the phosphoric acid solution obtained in the step (2) under the stirring condition, and filtering, washing and drying the precipitate after the constant-temperature reaction is completed to obtain neodymium phosphate powder. The high-purity nano neodymium phosphate prepared by the method has the purity of more than 99.995 percent, good dispersibility and the primary particle size of 100-500 nm.
Description
Technical Field
The invention relates to a preparation method of high-purity nano neodymium phosphate powder.
Background
Neodymium is a rare earth element, and has wide application in the fields of magnetic materials, luminescent materials, grinding materials, laser glass materials, catalytic materials and the like. Neodymium phosphate exists in the natural world in a monazite structure, and has unique excellent performance, so that the neodymium phosphate has wide application in the fields of ceramics, luminescence, catalysis and the like, but in the application fields, the properties of high purity, small particle size, uniform distribution and the like of the neodymium phosphate are required.
The existing preparation method of high-purity nano neodymium phosphate powder, as disclosed in Chinese patent application No. CN202010691796.5, is a method for preparing neodymium phosphate dihydrate rod-shaped nanocrystalline, wherein neodymium oxide, deionized water, glacial acetic acid and sodium dihydrogen phosphate solution are used as raw materials, and the neodymium phosphate dihydrate rod-shaped nanocrystalline is obtained by performing constant-temperature reaction for 12 hours through a hydrothermal method, so that the product purity is 98.5% -99.5%. The precipitate is obtained through hydrothermal reaction, and the precipitate is filtered, washed and dried to obtain neodymium phosphate solid. Chinese patent application CN202010413847.8 discloses a process for preparing optical grade neodymium metaphosphate by preparing aqueous solution of monoammonium phosphate and removing water insoluble matter; passing through an ion exchange device to remove nonferrous metals and impurity ions; and combining neodymium oxide and optical grade ammonium dihydrogen phosphate to perform solid-solid two-stage clean calcination reaction at medium-high temperature to obtain optical grade neodymium metaphosphate. The method produces ammonia nitrogen wastewater or high-salt wastewater, and has low product purity and complex production process. According to the preparation method of the high-purity optical glass additive neodymium metaphosphate disclosed in the Chinese patent application with the application number of CN201910395445.7, neodymium oxide, sulfuric acid and phosphoric acid are used as raw materials, neodymium dihydrogen phosphate crystals are roasted to obtain polymeric neodymium metaphosphate, the production cost of the method is high, waste water contains high sulfate radicals, and the production process is complex. The method disclosed in the Chinese patent application No. CN201310133041.3 is to prepare neodymium phosphate precipitate by precipitation reaction with soluble neodymium chloride salt, phosphate, alcohol, butadiene and carbon hexa-oil as raw materials. Mo Guo et al, published paper "solid synthesis of Neodymium phosphate nanocrystalline", which uses Neodymium phosphate and ammonium phosphate as raw materials and PEG 400 as a dispersant solid phase method to synthesize nano neodymium phosphate crystals, which can generate a large amount of oxynitride during calcination and has serious pollution.
For the synthesis of neodymium phosphate, the main methods at present are a precipitation method, a hydrothermal method and a solid phase method, and for the precipitation method, firstly, soluble neodymium salt is used for reacting with phosphate, and pH value is adjusted to precipitate neodymium phosphate, wherein the defects of waste water, low product purity and the like are generated. The hydrothermal method has the advantages of harsh reaction conditions, low yield and high energy consumption, and simultaneously produces a large amount of acid-salt-containing wastewater.
Disclosure of Invention
The invention aims to solve the technical problem of providing the preparation method of the high-purity nano neodymium phosphate powder, which has the advantages of simple production process, simple and convenient operation, no pollution and environmental friendliness.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of the high-purity nano neodymium phosphate powder comprises the following steps:
(1) Adding neodymium carbonate, basic neodymium carbonate, neodymium oxide or neodymium hydroxide into deionized water or deionized water containing a dispersing agent, and stirring to obtain a neodymium-containing suspension;
(2) Preparing a phosphoric acid solution, adding a strong acid solution into the phosphoric acid solution, and adding a dispersing agent;
(3) And (3) adding a neodymium-containing suspension into the phosphoric acid solution obtained in the step (2) under the stirring condition, and filtering, washing and drying the precipitate after the constant-temperature reaction is completed to obtain neodymium phosphate powder.
Further, in the step (1), the rare earth relative purity of the neodymium carbonate, the basic neodymium carbonate, the neodymium oxide or the neodymium hydroxide is more than or equal to 99.995wt%. The concentration of the suspension liquid containing neodymium is 0.5 mol/L-2 mol/L.
Further, in step (1), the neodymium-containing suspension is heated to 0 ℃ to 100 ℃, preferably 20 ℃ to 90 ℃.
Further, in the step (2), the molar concentration of the phosphoric acid solution is 0.5mol/L to 3mol/L, and the concentration of the strong acid solution is controlled to be 0.01mol/L to 0.5mol/L.
Further, in the step (2), the strong acid solution is hydrochloric acid, nitric acid or a mixed solution of hydrochloric acid and nitric acid.
In the step (2), the addition amount of the dispersing agent is 0.1-1% of the mass of neodymium carbonate, neodymium carbonate hydroxide, neodymium oxide or neodymium hydroxide calculated by oxide.
Further, in the step (2), the dispersing agent is PEG6000 or CTAB.
Further, in the step (4), the temperature of the constant temperature reaction is 0℃to 100℃and preferably 20℃to 90 ℃.
In the step (2), the adding amount of the suspension containing neodymium is 90% -98% of the molar amount of phosphoric acid calculated by neodymium carbonate, neodymium carbonate hydroxide, neodymium oxide or neodymium hydroxide, and the whole reaction equation is as follows: nd 2 O 3 +2H 3 PO 4 =2Nd PO 4 +3H 2 O。
Further, in the step (4), after the reaction is completed, the filtrate can be recycled and used for preparing phosphoric acid or preparing strong acid solution, so that no wastewater is generated in the whole process.
Further, in the step (4), the drying temperature is controlled to be 80-150 ℃.
The invention can obtain spherical neodymium phosphate powder with purity of more than 99.995% and primary particle diameter of 100-500 nm, and simultaneously, the invention does not bring other impurities and discharge waste water, and the whole process is green and circular, the production process is simple, and the production environment is friendly.
Drawings
FIG. 1 is an X-ray diffraction chart of a high purity nano neodymium phosphate powder obtained in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the high-purity nano neodymium phosphate powder obtained in example 1 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and examples.
Example 1
The preparation method of the high-purity nano neodymium phosphate powder comprises the following steps:
(1) 230g of neodymium carbonate with the rare earth relative purity of 99.995 percent (50 percent of the total rare earth) is taken and added into 0.5L of deionized water, and the suspension containing neodymium is obtained after stirring;
(2) 1L of solution with the concentration of phosphoric acid of 0.73mol/L and the concentration of nitric acid of 0.05mol/L is prepared, and 0.2g PEG6000 is added;
(3) Adding neodymium-containing suspension into phosphoric acid solution at constant temperature of 25 ℃, heating to 80 ℃ under stirring, keeping the temperature for 30min to obtain neodymium phosphate precipitate, filtering, washing, recycling filtrate, and drying the obtained neodymium phosphate at 105 ℃ for 2h to obtain a neodymium phosphate product.
The composition and particle size of the neodymium phosphate product obtained in this example are shown in table 1, and the xrd pattern and scanning electron microscope pattern are shown in fig. 1 and fig. 2, respectively.
TABLE 1
Example 2
The preparation method of the high-purity nano neodymium phosphate powder comprises the following steps:
(1) 1170g of neodymium oxide with the relative purity of 99.999% is taken and added into 10L of deionized water, and the suspension containing neodymium is obtained after stirring;
(2) 5L of solution with the phosphoric acid concentration of 1.42mol/L and the hydrochloric acid concentration of 0.01mol/L, CTAB and the mass of 5g is prepared;
(3) Adding the neodymium-containing suspension into the phosphoric acid solution at a constant temperature of 80 ℃ under the stirring condition, aging for 2 hours after the addition, filtering and washing, recycling the filtrate, and drying the obtained neodymium phosphate for 1 hour at 150 ℃ to obtain a neodymium phosphate product.
The composition and particle size of the neodymium phosphate product obtained in this example are shown in Table 2.
TABLE 2
Example 3
The preparation method of the high-purity nano neodymium phosphate powder comprises the following steps:
(1) 5000g (59% of total rare earth) of basic neodymium carbonate with the rare earth relative purity of 99.998% is taken and added into 10L deionized water, and the suspension containing neodymium is obtained after stirring;
(2) Preparing 12L of solution with the phosphoric acid concentration of 1.5mol/L and the nitric acid concentration of 0.1mol/L, CTAB and the mass of 15 g;
(3) Adding the neodymium-containing suspension into the phosphoric acid solution at the constant temperature of 90 ℃ under the stirring condition, aging for 1h after the addition, filtering and washing, recycling the filtrate, and drying the obtained neodymium phosphate for 3h at the temperature of 100 ℃ to obtain a neodymium phosphate product.
The composition and particle size of the neodymium phosphate product obtained in the examples are shown in Table 3.
TABLE 3 Table 3
Example 4
The preparation method of the high-purity nano neodymium phosphate powder comprises the following steps:
(1) 3000g of neodymium hydroxide with the rare earth relative purity of 99.998% (80% of the total rare earth) is taken and added into 10L of deionized water, and the suspension containing neodymium is obtained after stirring;
(2) 10L of solution with the phosphoric acid concentration of 1.5mol/L and the hydrochloric acid concentration of 0.05mol/L, CTAB and the mass of 12g is prepared;
(3) And (3) adding the neodymium-containing suspension into the phosphoric acid solution at a constant temperature of 85 ℃ under the stirring condition, aging for 1h after the addition, filtering and washing, recycling the filtrate, and drying the obtained neodymium phosphate for 6h at a temperature of 90 ℃ to obtain a neodymium phosphate product.
The composition and particle size of the neodymium phosphate product obtained in the examples are shown in Table 4.
TABLE 4 Table 4
Claims (4)
1. The preparation method of the high-purity nano neodymium phosphate powder is characterized by comprising the following steps of:
(1) Adding neodymium carbonate, basic neodymium carbonate, neodymium oxide or neodymium hydroxide into deionized water or deionized water containing a dispersing agent, and stirring to obtain a neodymium-containing suspension;
(2) Preparing a phosphoric acid solution, adding a strong acid solution into the phosphoric acid solution, and adding a dispersing agent;
(3) Adding neodymium-containing suspension into the phosphoric acid solution obtained in the step (2) under the stirring condition, and filtering, washing and drying the precipitate after the constant-temperature reaction is completed to obtain neodymium phosphate powder;
in the step (2), the strong acid solution is hydrochloric acid, nitric acid or a mixed solution of hydrochloric acid and nitric acid;
in the step (2), the addition amount of the dispersing agent is 0.1-1% of the mass of neodymium carbonate, neodymium carbonate hydroxide, neodymium oxide or neodymium hydroxide calculated by oxide;
in the step (3), the adding amount of the suspension liquid containing neodymium is 90-98% of the mole amount of phosphoric acid calculated by neodymium carbonate, neodymium carbonate hydroxide, neodymium oxide or neodymium hydroxide according to neodymium oxide;
in the step (2), the dispersing agent is PEG6000 or CTAB.
2. The method for preparing the high-purity nano neodymium phosphate powder according to claim 1, wherein the method comprises the following steps: in the step (1), the rare earth relative purity of the neodymium carbonate, the basic neodymium carbonate, the neodymium oxide or the neodymium hydroxide is more than or equal to 99.995 percent.
3. The method for preparing high-purity nano neodymium phosphate powder according to claim 1 or 2, wherein: in the step (3), the temperature of the constant temperature reaction is 0-100 ℃.
4. The method for preparing high-purity nano neodymium phosphate powder according to claim 1 or 2, wherein: in step (3), the overall reaction equation is as follows: nd 2 O 3 +2H 3 PO 4 =2 NdPO 4 +3H 2 O。
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CN111908439A (en) * | 2020-07-17 | 2020-11-10 | 南昌航空大学 | Method for preparing neodymium phosphate dihydrate rodlike nanocrystal |
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