CN112624078B - Preparation method of high-purity nano lanthanum phosphate powder - Google Patents

Preparation method of high-purity nano lanthanum phosphate powder Download PDF

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CN112624078B
CN112624078B CN202011550991.2A CN202011550991A CN112624078B CN 112624078 B CN112624078 B CN 112624078B CN 202011550991 A CN202011550991 A CN 202011550991A CN 112624078 B CN112624078 B CN 112624078B
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刘卫
杨泱
崔小震
肖勇
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YIYANG HONGYUAN RARE EARTH CO LTD
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    • C—CHEMISTRY; METALLURGY
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract

The preparation method of the high-purity nano lanthanum phosphate powder comprises the following steps: (1) Adding lanthanum oxide, lanthanum hydroxide or lanthanum carbonate into deionized water or deionized water containing a dispersing agent, and heating to obtain lanthanum-containing suspension; (2) preparing a phosphoric acid solution; (3) preparing a strong acid solution; (4) Adding lanthanum-containing suspension and phosphoric acid solution into strong acid solution by adopting a parallel adding mode, or adding lanthanum-containing suspension into phosphoric acid solution added with strong acid solution, filtering, washing and drying after the constant-temperature reaction is completed. The high-purity nanometer lanthanum phosphate prepared by the method has the purity of more than 99.995 percent, good dispersibility and primary particle diameter of 20-100 nm.

Description

Preparation method of high-purity nano lanthanum phosphate powder
Technical Field
The invention relates to a preparation method of high-purity nano lanthanum phosphate powder.
Background
Lanthanum is a rare earth element and has wide application in materials such as steel, alloy, target material, catalysis, optical glass, ceramic, luminescence, hydrogen storage, magnetic material and the like. The lanthanum phosphate has good thermal stability under the high temperature condition, has good compatibility with other oxides, has lower hardness, and can be applied to the fields of ceramics, catalysis, luminescence, and the like. In these fields of application, lanthanum phosphate is required to have high purity, small particle size, uniform distribution and the like.
The existing preparation method of high-purity nanometer lanthanum phosphate powder, as disclosed in China patent application with the application number of 201210312623.3, is a preparation method of lanthanum phosphate nanowire, wherein phosphate is added into solutions of lanthanum nitrate, lanthanum chloride and the like to generate lanthanum phosphate precipitate, and ammonia nitrogen wastewater or high-salt wastewater is generated by the method; because the generated lanthanum phosphate precipitate particles are small, the salt in the product is higher, and the purity of the product is not high; meanwhile, the concentration of the raw materials and the auxiliary materials is low, and the yield is small. The method is characterized in that phosphate is added into solutions of lanthanum nitrate, lanthanum chloride, lanthanum acetate and the like, the pH value of the solutions is regulated, and the solutions are transferred into a high-pressure reaction kettle for high-temperature reaction for 12-24 hours, so that ammonia nitrogen wastewater or high-salt wastewater is generated, the product purity is low, and the production process is harsh. The method for synthesizing the lanthanum phosphate nano rod by solvothermal method disclosed in China patent application with application number 200810029502.1 takes sodium phosphate and lanthanum chloride as raw materials, simultaneously adds n-butanol, and reacts for 6-8 hours at 140-220 ℃, and has the advantages of high production cost, high sodium content of products and more severe production process. Wu Hong published papers on low heat solid phase synthesized lanthanum phosphate and crystallinity thereof, dai Jie published papers on morphology control synthesis and luminous performance research of rare earth lanthanum phosphate fluorescent powder, chen Lin published papers on controllable preparation of monodisperse lanthanum phosphate nano rod, liu Zifeng and other published papers on molten salt method synthesized lanthanum phosphate powder and morphology thereof, and the research on the method has the defects of waste water generation, high impurity content of products, high production cost, complex production process and the like because lanthanum salt and phosphate are taken as raw materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing the preparation method of the high-purity nano lanthanum 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 lanthanum phosphate powder comprises the following steps:
(1) Adding lanthanum oxide, lanthanum hydroxide or lanthanum carbonate into deionized water or deionized water containing a dispersing agent, and heating to obtain lanthanum-containing suspension;
(2) Preparing a phosphoric acid solution;
(3) Preparing a strong acid solution;
(4) Adding lanthanum-containing suspension and phosphoric acid solution into strong acid solution by adopting a parallel adding mode, or adding lanthanum-containing suspension into phosphoric acid solution added with strong acid solution, filtering, washing and drying after the constant-temperature reaction is completed.
Further, in the step (1), the rare earth relative purity of the lanthanum oxide, the lanthanum hydroxide or the lanthanum carbonate is more than or equal to 99.995wt%. The concentration of the lanthanum-containing suspension is 0.5 mol/L-2 mol/L.
Further, in the step (1), the dispersant is CTAB (cetyltrimethylammonium bromide), PEG (polyethylene glycol) or a mixed dispersant of CTAB and PEG.
In the step (1), the addition amount of the dispersing agent is 0.1-0.5% of the mass of lanthanum oxide, lanthanum hydroxide or lanthanum carbonate, and the lanthanum hydroxide or lanthanum carbonate is calculated by rare earth oxide.
Further, in the step (1), the temperature is heated to 60-100 ℃.
Further, in the step (2), the phosphoric acid is excessive by 1% -5% according to the theoretical amount, and the whole reaction equation is as follows: la (La) 2 O 3 +2H 3 PO 4 ＝2LaPO 4 +3H 2 O. The molar concentration of the phosphoric acid solution is 0.5mol/L to 3mol/L.
Further, in the step (3), the strong acid solution is hydrochloric acid, nitric acid or a mixed solution of hydrochloric acid and nitric acid. The molar concentration of the strong acid solution is 0.01mol/L to 0.5mol/L.
Further, in the step (3), lanthanum oxide, lanthanum hydroxide or lanthanum carbonate (calculated by rare earth oxide) with the mass of 0.1-0.5% of CTAB, PEG or a mixed dispersing agent of CTAB and PEG is added into the strong acid solution.
Further, in the step (4), the temperature of the constant temperature reaction is 10 to 100 ℃, preferably 60 to 90 ℃.
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 columnar lanthanum phosphate powder with the purity of more than 99.995 percent and the primary particle diameter of 20-100 nm, and simultaneously, the invention does not bring other impurities and discharge waste water, the whole process is green and circulated, the production process is simple, and the production environment is friendly.
Drawings
FIG. 1 is an X-ray diffraction chart of the high purity nano lanthanum phosphate powder obtained in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the high purity nano lanthanum phosphate powder obtained in example 1 of the present invention;
FIG. 3 is a scanning electron microscope image of the high purity nano lanthanum phosphate powder obtained in example 2 of the present invention;
FIG. 4 is a scanning electron microscope image of the high purity nano lanthanum phosphate powder obtained in example 3 of the present invention.
Detailed Description
The invention is further illustrated by the following examples.
Example 1
The preparation method of the high-purity nano lanthanum phosphate powder comprises the following steps:
(1) 200g of lanthanum oxide with the rare earth relative purity of more than or equal to 99.995 percent is taken and added into 1L of deionized water, and stirred and heated to 60 ℃ to obtain lanthanum-containing suspension;
(2) 144g of 85wt% phosphoric acid is taken and diluted to 1L by deionized water to obtain a phosphoric acid solution;
(3) Diluting nitric acid to 0.5L by deionized water, controlling the concentration of nitric acid to be 0.1mol/L, adding 0.2g CTAB (cetyl trimethyl bromide), and heating to 60 ℃ under stirring to obtain nitric acid solution;
(4) Under the condition of stirring, respectively adding lanthanum-containing suspension and phosphoric acid solution into nitric acid solution by using peristaltic pumps, aging for 1h after adding, filtering and washing, recycling filtrate, and drying the obtained lanthanum phosphate for 6h at 80 ℃ to obtain a lanthanum phosphate product. The composition and the particle size are shown in Table 1, and the XRD pattern and the scanning electron microscope pattern are shown in FIG. 1 and FIG. 2 respectively.
TABLE 1
Detecting items La 2 O 3 /TREO Fe 2 O 3 Na 2 O SiO 2 CaO MgO MnO Primary particle diameter
Detection result 99.995％ 0.00052％ 0.00011％ 0.00026％ 0.00051％ 0.00037％ 0.0001％ 100nm
Example 2
The preparation method of the high-purity nano lanthanum phosphate powder comprises the following steps:
(1) 2000g (TREO is 50%) of lanthanum carbonate with the rare earth relative purity more than or equal to 99.999% is taken and added into 10L deionized water, and the mixture is stirred and heated to 80 ℃;
(2) 722g of 85wt% phosphoric acid is taken, diluted to 10L by deionized water, 0.2L of 10mol/L hydrochloric acid is added into the diluted phosphoric acid solution, and 4g of PEG6000 (polyethylene glycol 6000) is added;
(3) And heating the phosphoric acid solution to 80 ℃, adding the lanthanum-containing suspension into the phosphoric acid solution under the condition of stirring, aging for 2 hours after the addition, filtering and washing, recycling the filtrate, and drying the obtained lanthanum phosphate for 2 hours under the condition of 150 ℃ to obtain a lanthanum phosphate product. The composition and particle size are shown in Table 2, and the scanning electron microscope is shown in FIG. 3.
TABLE 2
Detecting items La 2 O 3 /TREO Fe 2 O 3 Na 2 O SiO 2 CaO MgO MnO Primary particle diameter
Detection result 99.999％ 0.00021％ 0.00008％ 0.00007％ 0.00021％ 0.00014％ 0.0001％ 20nm
Example 3
The preparation method of the high-purity nano lanthanum phosphate powder comprises the following steps:
(1) Adding 3g of PEG10000 (polyethylene glycol 10000) into 5L of deionized water, heating the solution to 70 ℃, and adding 750g of lanthanum hydroxide (TREO is 80%) with the rare earth relative purity more than or equal to 99.998%;
(2) 445g of 85wt% phosphoric acid is taken, diluted to 4L by deionized water, and 0.2L of 10mol/L nitric acid is added into the diluted phosphoric acid solution;
(3) And heating the phosphoric acid solution to 90 ℃, adding the lanthanum-containing suspension into the phosphoric acid solution under the condition of stirring, aging for 3 hours after the addition, filtering and washing, recycling the filtrate, and drying the obtained lanthanum phosphate for 3 hours under the condition of 120 ℃ to obtain a lanthanum phosphate product. The composition and particle size are shown in Table 3, and the scanning electron microscope is shown in FIG. 4.
TABLE 3 Table 3
Detecting items La 2 O 3 /TREO Fe 2 O 3 Na 2 O SiO 2 CaO MgO MnO Primary particle diameter
Detection result 99.998％ 0.00028％ 0.00015％ 0.00014％ 0.00032％ 0.00012％ 0.0001％ 25nm

Claims (7)

1. The preparation method of the high-purity nano lanthanum phosphate powder is characterized by comprising the following steps of:
(1) Adding lanthanum oxide, lanthanum hydroxide or lanthanum carbonate into deionized water or deionized water containing a dispersing agent, and heating to obtain lanthanum-containing suspension;
(2) Preparing a phosphoric acid solution;
(3) Preparing a strong acid solution;
(4) Adding lanthanum-containing suspension and phosphoric acid solution into strong acid solution by adopting a parallel adding mode, or adding the lanthanum-containing suspension into the phosphoric acid solution added with the strong acid solution, filtering, washing and drying after the constant-temperature reaction is completed;
in the step (1), the dispersing agent is CTAB, PEG or a mixed dispersing agent of CTAB and PEG;
in the step (3), the strong acid solution is hydrochloric acid, nitric acid or a mixed solution of hydrochloric acid and nitric acid;
in the step (3), adding CTAB, PEG or a mixed dispersing agent of CTAB and PEG with the mass of 0.1-0.5% of lanthanum oxide, lanthanum hydroxide or lanthanum carbonate in the strong acid solution, wherein the lanthanum hydroxide or lanthanum carbonate is calculated by rare earth oxide.
2. The method for preparing high-purity nano lanthanum phosphate powder according to claim 1, wherein in the step (1), the rare earth relative purity of lanthanum oxide, lanthanum hydroxide or lanthanum carbonate is not less than 99.995%.
3. The method for preparing high-purity nano lanthanum phosphate powder according to claim 1 or 2, wherein in the step (1), the addition amount of the dispersing agent is 0.1% -0.5% by mass of lanthanum oxide, lanthanum hydroxide or lanthanum carbonate, and the lanthanum hydroxide or lanthanum carbonate is calculated by rare earth oxide.
4. The method for preparing high purity nano lanthanum phosphate powder according to claim 1 or 2, wherein in step (1), the temperature is heated to 60 ℃ to 100 ℃.
5. The method for preparing high purity nano lanthanum phosphate powder according to claim 1 or 2, wherein in the step (2), the phosphoric acid is excessive by 1% -5% by theoretical amount, and the whole reaction equation is as follows: la (La) 2 O 3 +2H 3 PO 4 =2LaPO 4 +3H 2 O。
6. The method for preparing high purity nano lanthanum phosphate powder according to claim 1 or 2, wherein in the step (4), the temperature of the constant temperature reaction is 10 ℃ to 100 ℃.
7. The method for preparing high purity nano lanthanum phosphate powder according to claim 1 or 2, wherein in step (4), the drying temperature is controlled to 80 ℃ to 150 ℃.
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