A post-treatment method for improving the purity of K / NaMgF3 particles

Abstract

The present invention provides a post-treatment method for improving the purity of K / NaMgF3 particles, particularly relating to the field of chemistry. The method comprises the following specific steps: (1) placing K / NaMgF3 particles in an aqueous solution and stirring and dissolving them thoroughly; (2) adding a fluoride salt and a buffer to the solution treated in step (1) and stirring thoroughly; (3) adding a magnesium salt and a chloride salt to the solution treated in step (2) and stirring thoroughly; and (4) pouring out the residual solution treated in step (3) and drying the residual solid in step (4). The K / NaMgF3 of the present invention remains unchanged and does not introduce new impurities. The method can remove MgF2 impurities while neither destroying the structure of K / NaMgF3 nor introducing new impurities. The steps are closely related, and no intermediate rinsing or treatment is required. The process is simple, and while ensuring efficient impurity removal, energy conservation and environmental protection are also taken into account. The method is applicable to various K / NaMgF3 preparation methods, does not use toxic and hazardous substances, and has low waste liquid treatment costs.

Description

Technical Field

[0001] The present invention relates to the field of chemistry, and in particular provides a post-treatment method for improving the purity of K / NaMgF3 particles. Background Art

[0002] As a member of the perovskite family, K / NaMgF3 exhibits excellent optical uniformity, high transmittance, high thermal stability, and excellent cross-luminescence properties under high-energy irradiation. It holds significant application prospects in photocatalytic materials, window materials, scintillating materials, and tunable laser materials. In particular, K / NaMgF3 can effectively photocatalytically degrade stubborn substances such as phenol, chlorophenol, methyl orange, rhodamine B, and water-soluble dyes, thus possessing significant implications for environmental governance and remediation, as well as air purification and wastewater treatment.

[0003] Currently, the main processes for synthesizing K / NaMgF3 include high-temperature solid-phase methods, microemulsion methods, molten salt methods, hydrothermal and solvothermal synthesis methods, direct precipitation methods, and ethylene glycol reflux methods. However, these methods all share a common drawback: the final product contains MgF2 as an impurity. Therefore, it is crucial to find a method to remove MgF2 without destroying the K / NaMgF3 and introducing foreign matter. However, existing technologies do not yet offer a solution to this problem. Summary of the Invention

[0004] The purpose of the present invention is to provide a post-treatment method to improve the purity of K / NaMgF3 particles. K / NaMgF3 is not dissolved by chloride salts, but chloride salts can dissolve MgF2 and react with OH at the same time. - Other precipitates form, so fluoride, buffers, chloride salts, and magnesium salts are added to the solution to prevent this process.

[0005] In order to achieve the above object, the present invention provides the following technical solutions:

[0006] A post-treatment method for improving the purity of K / NaMgF3 particles, the specific steps of the method are as follows:

[0007] (1) Place K / NaMgF3 particles into aqueous solution and stir thoroughly;

[0008] (2) adding fluoride salt and buffer to the solution treated in step (1) and stirring thoroughly;

[0009] (3) adding magnesium salt and chloride salt to the solution treated in step (2) and stirring thoroughly;

[0010] (4) Pour out the residual solution after treatment in step (3) and dry the residual solid in step (4).

[0011] Furthermore, the composition and mass percentage of the aqueous solution in step (1) are as follows: dispersant: 10-20%, the rest is H2O; the aqueous solution treatment temperature is 40-60°C, and the reaction time is 3-6h.

[0012] Furthermore, the fluoride salt in step (2) is one or more of NaF, KF, and NH4F, and the buffer is one or more of boric acid, acetic acid, and hydrochloric acid. The mass percentages of the fluoride salt and the buffer in the solution of step (2) are as follows: 10-20% fluoride salt, 0.1-1% buffer, temperature, 50-70°C, and reaction time 5-8h.

[0013] Furthermore, the magnesium salt in step (3) is one or more of MgCl2, Mg(NO3)2, Mg(CO3)2, MgHCO3, and MgSO4, and the chloride salt is one or more of NaCl, KCl, CaCl2, and NH4Cl. The mass percentages of the magnesium salt and the chloride salt in the solution of step (3) are as follows: 2-5% magnesium salt, 20-50% chloride salt, the solution temperature is 60-80°C, and the reaction time is 10-12h.

[0014] Furthermore, the dispersant in step (1) is one or more of sodium dodecylbenzene sulfonate, sodium dodecylbenzene sulfate, polyvinyl pyrrolidone, polyvinyl alcohol, and polyvinyl ether.

[0015] Beneficial effects of the present invention:

[0016] (1) The present invention can efficiently remove MgF2 impurities without destroying K / NaMgF3 particles and without introducing additional impurities.

[0017] (2) The present invention adopts an environmentally friendly post-treatment solution, which is low in cost and easy to treat the waste liquid.

[0018] (3) The equipment used in the present invention is simple, easy to operate, and suitable for industrial production.

[0019] (4) The present invention first treats K / NaMgF3 particles with an aqueous solution to uniformly distribute them therein, then adds a fluoride salt and a buffer to the solution to positively charge the surface of the MgF2 particles, and finally adds a magnesium salt and a chloride salt to dissolve the MgF2, while leaving the K / NaMgF3 unchanged and without introducing new impurities. This method can remove MgF2 impurities while neither destroying the structure of K / NaMgF3 nor introducing new impurities. The various steps are closely related, requiring no intermediate rinsing or treatment, resulting in a simple process. While ensuring efficient impurity removal, it also takes into account energy conservation and environmental protection requirements. The method is applicable to various K / NaMgF3 preparation methods, does not use toxic or hazardous substances, and has low waste liquid treatment costs. DETAILED DESCRIPTION

[0020] The present invention will be further described below with reference to the examples, but is not limited thereto.

[0021] Example 1

[0022] (1) Place K / NaMgF3 particles in an aqueous solution and stir thoroughly. The aqueous solution composition and its mass percentage are as follows: 10% sodium dodecylbenzenesulfonate, the remainder is H2O; the aqueous solution temperature is 40°C, and the reaction time is 3 hours.

[0023] (2) Add fluoride salt and buffer to the solution treated in step (1) and stir thoroughly. The composition and mass percentage of fluoride salt and buffer in the solution of step (2) are as follows: 1% NaF, 0.1% acetic acid, solution temperature 50°C, reaction time 5h.

[0024] (3) Add magnesium salt and chloride salt to the solution treated in step (2) and stir thoroughly. The mass percentage of magnesium salt and chloride salt in the solution of step (3) is as follows: 2% MgCl2, 30% NaCl, MgCl2 / NaCl mass ratio is 15, solution temperature is 60°C, and reaction time is 10 hours.

[0025] (4) Pour out the residual solution after treatment in step (3) and dry the residual solid in step (4).

[0026] Example 2

[0027] (1) Place K / NaMgF3 particles in an aqueous solution and stir thoroughly. The aqueous solution composition and its mass percentage are as follows: 15% sodium dodecylbenzene sulfate, the remainder is H2O; the aqueous solution temperature is 50°C, and the reaction time is 4 hours.

[0028] (2) Add fluoride salt and buffer to the solution treated in step (1) and stir thoroughly. The composition and mass percentage of fluoride salt and buffer in the solution of step (2) are as follows: 2% KF, 0.1% boric acid, solution temperature 50°C, reaction time 5h.

[0029] (3) Add magnesium salt and chloride salt to the solution treated in step (2) and stir thoroughly. The mass percentage of magnesium salt and chloride salt in the solution of step (3) is as follows: 2% Mg(NO3)2, 25% KCl, Mg(NO3)2 / KCl mass ratio is 12.5, solution temperature is 65°C, and reaction time is 10 hours.

[0030] (4) Pour out the residual solution after treatment in step (3) and dry the residual solid in step (4).

[0031] Example 3

[0032] (1) Place K / NaMgF3 particles in an aqueous solution and stir thoroughly. The aqueous solution composition and its mass percentage are as follows: 16% polyvinylpyrrolidone, the remainder is H2O; the aqueous solution temperature is 45°C, and the reaction time is 4.5 hours.

[0033] (2) Add fluoride salt and buffer to the solution treated in step (1) and stir thoroughly. The composition and mass percentage of fluoride salt and buffer in the solution of step (2) are as follows: 5% NH4F, 0.5% acetic acid, solution temperature 65°C, reaction time 7h.

[0034] (3) Add magnesium salt and chloride salt to the solution treated in step (2) and stir thoroughly. The mass percentage of magnesium salt and chloride salt in the solution of step (3) is as follows: 2% MgSO2, 50% NH4Cl, MgSO2 / NH4Cl mass ratio is 25, solution temperature is 78°C, and reaction time is 10.5h.

[0035] (4) Pour out the residual solution after treatment in step (3) and dry the residual solid in step (4).

[0036] Example 4

[0037] (1) Place K / NaMgF3 particles in an aqueous solution and stir thoroughly. The aqueous solution composition and its mass percentage are as follows: 10% polyvinyl alcohol, 5% polyvinyl ether, and the remainder is H2O; the aqueous solution temperature is 45°C, and the reaction time is 4.5 hours.

[0038] (2) Add fluoride salt and buffer to the solution treated in step (1) and stir thoroughly. The composition and mass percentage of fluoride salt and buffer in the solution of step (2) are as follows: 8% NaF, 0.5% hydrochloric acid, solution temperature 70°C, reaction time 8h.

[0039] (3) Add magnesium salt and chloride salt to the solution treated in step (2) and stir thoroughly. The mass percentage of magnesium salt and chloride salt in the solution of step (3) is as follows: 3% MgCl2, 30% NaCl, MgCl2 / NaCl mass ratio is 10, solution temperature is 80°C, and reaction time is 12 hours.

[0040] (4) Pour out the residual solution after treatment in step (3) and dry the residual solid in step (4).

[0041] The purity of the K / NaMgF3 particles obtained in Examples 1-4 above is 100%.

[0042] Matters not covered by the present invention are known technologies.

[0043] The above embodiments are intended only to illustrate the technical concepts and features of the present invention. Their purpose is to enable those skilled in the art to understand the contents of the present invention and implement them accordingly. They are not intended to limit the scope of protection of the present invention. Any equivalent changes or modifications made in accordance with the spirit of the present invention are intended to be covered by the scope of protection of the present invention.

Claims

1. A post-treatment method for improving the purity of K / NaMgF3 particles, characterized by: The specific steps of this method are as follows: (1) Place K / NaMgF3 particles into aqueous solution and stir thoroughly; (2) adding fluoride salt and buffer to the solution treated in step (1) and stirring thoroughly; (3) adding magnesium salt and chloride salt to the solution treated in step (2) and stirring thoroughly; (4) pouring out the residual solution after the treatment in step (3) and drying the residual solid in step (4); the composition and mass percentage of the aqueous solution in step (1) are as follows: dispersant: 10-20%, and the rest is H2O; the aqueous solution treatment temperature is 40-60°C, and the reaction time is 3-6h; the dispersant in step (1) is one or more of sodium dodecylbenzene sulfonate, sodium dodecylbenzene sulfate, polyvinyl pyrrolidone, polyvinyl alcohol, and polyvinyl ether; the fluoride salt in step (2) is one or more of NaF, KF, and NH4F, and the buffer is one or more of boric acid, acetic acid, and hydrochloric acid. The mass percentage of fluoride salt and buffer in the solution of step (2) is as follows: 1-10% fluoride salt, 0.1-1% buffer, temperature, 50-70°C, and reaction time 5-8h.

2. A post-treatment method for improving the purity of K / NaMgF3 particles according to claim 1, characterized in that: The magnesium salt in step (3) is one or more of MgCl2, Mg(NO3)2, MgCO3, Mg(HCO3)2, and MgSO4, and the chloride salt is one or more of NaCl, KCl, CaCl2, and NH4Cl. The mass percentages of the magnesium salt and the chloride salt in the solution of step (3) are as follows: 2-5% magnesium salt, 20-50% chloride salt, the solution temperature is 60-80°C, and the reaction time is 10-12h.