CN112723331B - Preparation method of high-purity nano neodymium phosphate powder - Google Patents
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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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| JP2003238153A (en) * | 2002-02-15 | 2003-08-27 | Dainichiseika Color & Chem Mfg Co Ltd | Fine neodymium oxide and its producing method |
| JP2007063108A (en) * | 2005-08-26 | 2007-03-15 | Daiichi Kigensokagaku Kogyo Co Ltd | Neodymium oxide sol and its production method |
| EP2093192A1 (en) * | 2008-02-25 | 2009-08-26 | Koninklijke Philips Electronics N.V. | Preparation of nanoparticles from metal salts |
| 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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| DE2414513C3 (en) * | 1974-03-26 | 1978-11-09 | Max-Planck-Gesellschaft Zur Foerderung Der Wissenschaften E.V., 3400 Goettingen | Process for the production of neodymium pentaphosphates |
| CN100532254C (en) * | 2007-05-22 | 2009-08-26 | 同济大学 | Method of greenly preparing rare-earth potassium orthophosphate nano/micro crystal |
| CN102951624A (en) * | 2012-08-29 | 2013-03-06 | 深圳大学 | Preparation method of neodymium phosphate nanowire |
| CN105129834B (en) * | 2015-09-29 | 2017-08-01 | 四川省乐山锐丰冶金有限公司 | A kind of nanometer level RE oxide raw powder's production technology |
| CN106315536A (en) * | 2016-11-24 | 2017-01-11 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for preparing rare-earth phosphorate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2003238153A (en) * | 2002-02-15 | 2003-08-27 | Dainichiseika Color & Chem Mfg Co Ltd | Fine neodymium oxide and its producing method |
| JP2007063108A (en) * | 2005-08-26 | 2007-03-15 | Daiichi Kigensokagaku Kogyo Co Ltd | Neodymium oxide sol and its production method |
| EP2093192A1 (en) * | 2008-02-25 | 2009-08-26 | Koninklijke Philips Electronics N.V. | Preparation of nanoparticles from metal salts |
| 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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