CN115012037A - Preparation method of high-purity magnesium fluoride crystal material - Google Patents
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- CN115012037A CN115012037A CN202210668707.4A CN202210668707A CN115012037A CN 115012037 A CN115012037 A CN 115012037A CN 202210668707 A CN202210668707 A CN 202210668707A CN 115012037 A CN115012037 A CN 115012037A
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
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- C01F5/28—Fluorides
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- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The invention discloses a preparation method of a high-purity magnesium fluoride crystal material, which comprises the steps of calcining magnesite powder at high temperature to obtain light-burned ore powder, heating the light-burned ore powder by using an ammonium chloride solution with the mass concentration of 15-20% to obtain a leachate containing magnesium and calcium ions, uniformly mixing the leachate with a surfactant, precipitating the leachate with ammonia water, treating obtained filter residue by using an ammonium chloride solution with the mass concentration of 5-8% to remove the calcium ions, uniformly mixing the obtained powder with proper amount of water after high-temperature calcination, and adding hydrofluoric acid to react to obtain the high-purity magnesium fluoride crystal material. The preparation process is simple, and the prepared magnesium fluoride crystal material has high purity and can meet the performance requirement of the material for optical coating.
Description
Technical Field
The invention relates to the technical field of optical materials, in particular to a preparation method of a high-purity magnesium fluoride crystal material.
Background
The optical coating is a coating on the surface of an optical device, such as a lens, an optical filter, and the like, so as to achieve the purposes of antireflection, transmittance improvement, and the like. The magnesium fluoride crystal has good optical performance, mechanical performance and chemical stability, is an important optical coating material, and the magnesium fluoride film formed on the surface of an optical device not only has an ideal antireflection effect, but also has good wear resistance and stable physicochemical performance, and can play a role in improving the wear resistance and chemical stability of the optical device. In order to meet the use standard in the field of optical coating, the purity of the coating material is a crucial index, and therefore higher requirements are also put on the purity of the magnesium fluoride material used in the field. At present, the mainstream factory preparation method of the magnesium fluoride material is a magnesium carbonate method, namely, magnesite is used as a raw material, impurities in the raw material are removed through certain pretreatment, and then the raw material reacts with hydrofluoric acid, so that the high-purity magnesium fluoride material is obtained. Although the method has the advantages of low cost and simple process, the magnesium fluoride material meeting the requirement of optical coating performance is difficult to obtain. The magnesium oxide method, the sol-gel method and the like either require high-purity raw materials or have complicated production processes and can only be applied to laboratories or small-scale production. Therefore, the development of the preparation method of the magnesium fluoride crystal material with simple process and high product purity has very important practical significance.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a high-purity magnesium fluoride crystal material.
The invention provides a preparation method of a high-purity magnesium fluoride crystal material, which comprises the following steps:
s1, calcining magnesite powder at high temperature to obtain light-burned ore powder;
s2, adding the light-burned ore powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 15-20%, heating, stirring and reacting, filtering after the reaction is finished, and collecting leachate;
s3, uniformly mixing the leachate obtained in the step S2 with a surfactant, adding an ammonia water solution with the concentration of 3-6mol/L, heating, stirring, reacting, filtering after the reaction is finished, collecting filter residues, and drying;
s4, adding the dried filter residue obtained in the step S3 into an ammonium chloride solution with the mass concentration of 5-8%, stirring at normal temperature for reaction, filtering after the reaction is finished, collecting the filter residue, drying, and calcining at high temperature to obtain powder;
and S5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, adding hydrofluoric acid, heating, stirring, reacting, filtering after the reaction is finished, and washing and drying the obtained filter residue to obtain the high-purity magnesium fluoride crystal material.
Preferably, in S1, the temperature of the high-temperature calcination is 600-800 ℃, and the time is 2-4 h.
Preferably, in S2, the reaction is carried out at 80-90 deg.C for 3-5 h.
Preferably, in S2, the ratio of the light burned ore powder to the ammonium chloride solution is 1 g: (30-40) mL.
Preferably, in S3, the ratio of the leaching solution, the surfactant and the aqueous ammonia solution is 1 mL: (0.01-0.05) g: (0.5-1) mL; the surfactant is sodium dodecyl sulfate, sodium dodecyl benzene sulfonate or a combination thereof.
Preferably, in S3, the heating and stirring reaction temperature is 40-60 ℃ and the time is 1.5-2.5 h.
Preferably, in S4, the ratio of the dried filter residue to the ammonium chloride solution is 1 g: (20-30) mL, and the reaction time is 2-4h under stirring at normal temperature.
Preferably, in S4, the temperature of the high-temperature calcination is 400-450 ℃, and the time is 0.5-1 h.
Preferably, in S5, the mass ratio of the powder, water and hydrofluoric acid is 1: (0.3-0.5): (2-3).
Preferably, in S5, the reaction is carried out at 80-90 deg.C for 4-5 h.
The invention has the following beneficial effects:
the method comprises the steps of taking low-grade magnesite powder as a raw material, firstly calcining at high temperature to obtain light calcined ore powder, forming oxides containing magnesium, silicon, calcium, iron, aluminum and other impurities, then mixing and heating the oxides with a high-concentration ammonium chloride solution to perform decomposition reaction, dissolving out magnesium oxide and calcium oxide to obtain leachate containing magnesium ions and calcium ions, preliminarily removing the silicon, iron, aluminum and other impurities, further separating and precipitating the magnesium ions and the calcium ions with ammonia water under proper conditions with the aid of a surfactant to form a uniform precipitated phase, sufficiently dissolving out the calcium ions and other impurities from the precipitated phase with the low-concentration ammonium chloride solution, calcining the precipitated phase at high temperature to remove the residual surfactant, simultaneously forming high-purity MgO, and reacting the MgO with hydrofluoric acid to obtain the high-purity magnesium fluoride crystal material. The preparation process is simple, and the prepared magnesium fluoride crystal material has high purity and can meet the performance requirement of the material for optical coating.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
In the following examples and comparative examples, the chemical composition of magnesite powder is shown in table 1:
TABLE 1 chemical composition of magnesite powder
| Chemical composition | MgO | SiO 2 | CaO | Fe 2 O 3 | Al 2 O 3 |
| Content (wt%) | 46.85 | 1.97 | 0.86 | 0.47 | 0.34 |
Example 1
A preparation method of a high-purity magnesium fluoride crystal material comprises the following steps:
s1, calcining magnesite powder at a high temperature of 600 ℃ for 4 hours to obtain light burned ore powder;
s2, adding the light burned ore powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 15%, wherein the proportion of the light burned ore powder to the ammonium chloride solution is 1 g: 40mL, heating and stirring at 80 ℃ for reaction for 5 hours, filtering after the reaction is finished, and collecting leachate;
s3, uniformly mixing the leachate obtained in the step S2 with sodium dodecyl sulfate, and then adding an ammonia water solution with the concentration of 3mol/L, wherein the proportion of the leachate, the sodium dodecyl sulfate and the ammonia water solution is 1 mL: 0.05 g: 1mL, heating and stirring at 40 ℃ for reaction for 2.5h, filtering after the reaction is finished, collecting filter residues, and drying;
s4, adding the dried filter residue obtained in the step S3 into an ammonium chloride solution with the mass concentration of 5%, wherein the ratio of the dried filter residue to the ammonium chloride solution is 1 g: stirring and reacting for 2 hours at normal temperature, filtering after the reaction is finished, collecting filter residues, drying, and calcining for 1 hour at high temperature of 400 ℃ to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, adding hydrofluoric acid, heating and stirring at 80 ℃, and reacting for 5 hours, wherein the mass ratio of the powder to the water to the hydrofluoric acid is 1: 0.3: and 2, filtering after the reaction is finished, and washing and drying the obtained filter residue to obtain the high-purity magnesium fluoride crystal material.
Example 2
A preparation method of a high-purity magnesium fluoride crystal material comprises the following steps:
s1, calcining magnesite powder at a high temperature of 800 ℃ for 2 hours to obtain light burned ore powder;
s2, adding the light burned ore powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 20%, wherein the ratio of the light burned ore powder to the ammonium chloride solution is 1 g: 30mL, heating and stirring at 90 ℃ for reaction for 3 hours, filtering after the reaction is finished, and collecting leachate;
s3, uniformly mixing the leachate obtained in the step S2 with sodium dodecyl sulfate, and then adding an ammonia water solution with the concentration of 6mol/L, wherein the proportion of the leachate, the sodium dodecyl sulfate and the ammonia water solution is 1 mL: 0.01 g: 0.5mL, heating and stirring at 60 ℃ for reaction for 1.5h, filtering after the reaction is finished, collecting filter residues, and drying;
s4, adding the dried filter residue obtained in the step S3 into an ammonium chloride solution with the mass concentration of 8%, wherein the ratio of the dried filter residue to the ammonium chloride solution is 1 g: 20mL, stirring at normal temperature for reaction for 4h, filtering after the reaction is finished, collecting filter residues, drying, and calcining at the high temperature of 450 ℃ for 0.5h to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, adding hydrofluoric acid, heating and stirring at 90 ℃, and reacting for 4 hours, wherein the mass ratio of the powder to the water to the hydrofluoric acid is 1: 0.5: and 3, filtering after the reaction is finished, and washing and drying the obtained filter residue to obtain the high-purity magnesium fluoride crystal material.
Example 3
A preparation method of a high-purity magnesium fluoride crystal material comprises the following steps:
s1, calcining magnesite powder at a high temperature of 700 ℃ for 3 hours to obtain light burned ore powder;
s2, adding the light burned ore powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 18%, wherein the ratio of the light burned ore powder to the ammonium chloride solution is 1 g: 35mL, heating and stirring at 85 ℃ for reaction for 4 hours, filtering after the reaction is finished, and collecting leachate;
s3, uniformly mixing the leachate obtained in the step S2 with sodium dodecyl sulfate, and then adding an ammonia water solution with the concentration of 5mol/L, wherein the proportion of the leachate to the sodium dodecyl sulfate to the ammonia water solution is 1 mL: 0.04 g: 0.8mL, heating and stirring at 50 ℃ for reaction for 2 hours, filtering after the reaction is finished, collecting filter residues, and drying;
s4, adding the dried filter residue obtained in the step S3 into an ammonium chloride solution with the mass concentration of 6%, wherein the ratio of the dried filter residue to the ammonium chloride solution is 1 g: stirring at normal temperature for reaction for 3 hours in an amount of 25mL, filtering after the reaction is finished, collecting filter residues, drying, and calcining at the high temperature of 420 ℃ for 40min to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, adding hydrofluoric acid, heating and stirring at 85 ℃, and reacting for 4.5 hours, wherein the mass ratio of the powder to the water to the hydrofluoric acid is 1: 0.4: and 2.5, filtering after the reaction is finished, and washing and drying the obtained filter residue to obtain the high-purity magnesium fluoride crystal material.
Comparative example 1
A preparation method of a high-purity magnesium fluoride crystal material comprises the following steps:
s1, calcining magnesite powder at a high temperature of 700 ℃ for 3 hours to obtain light burned ore powder;
s2, adding the light burned ore powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 18%, wherein the ratio of the light burned ore powder to the ammonium chloride solution is 1 g: 35mL, heating and stirring at 85 ℃ for reaction for 4 hours, filtering after the reaction is finished, and collecting leachate;
s3, adding an ammonia water solution with the concentration of 5mol/L into the leachate obtained in the step S2, wherein the proportion of the leachate to the ammonia water solution is 1 mL: 0.8mL, heating and stirring at 50 ℃ for reaction for 2 hours, filtering after the reaction is finished, collecting filter residues, and drying;
s4, adding the dried filter residue obtained in the step S3 into an ammonium chloride solution with the mass concentration of 6%, wherein the ratio of the dried filter residue to the ammonium chloride solution is 1 g: stirring at normal temperature for reaction for 3 hours in an amount of 25mL, filtering after the reaction is finished, collecting filter residues, drying, and calcining at the high temperature of 420 ℃ for 40min to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, adding hydrofluoric acid, heating and stirring at 85 ℃, and reacting for 4.5 hours, wherein the mass ratio of the powder to the water to the hydrofluoric acid is 1: 0.4: and 2.5, filtering after the reaction is finished, and washing and drying the obtained filter residue to obtain the high-purity magnesium fluoride crystal material.
The magnesium fluoride crystal materials prepared in examples 1 to 3 and comparative example 1 were prepared according to the following standards: the purity and impurity detection of GB/T31860-2015 magnesium fluoride for coating shows that the magnesium fluoride crystal material prepared in the embodiment 1-3 can meet the technical requirements that the content of magnesium fluoride is more than or equal to 99.90 percent and the content of Ca is less than or equal to 0.015 percent, has low impurity content and high purity, and can meet the performance requirements of the magnesium fluoride material for coating; and the content of Ca in the magnesium fluoride crystal material prepared in the comparative example 1 is 0.018%, and the content of Ca exceeds the standard, so that the requirement of the use performance of the coating material cannot be met.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (10)
1. A preparation method of a high-purity magnesium fluoride crystal material is characterized by comprising the following steps:
s1, calcining magnesite powder at high temperature to obtain light-burned ore powder;
s2, adding the light-burned ore powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 15-20%, heating, stirring and reacting, filtering after the reaction is finished, and collecting leachate;
s3, uniformly mixing the leachate obtained in the step S2 with a surfactant, adding an ammonia water solution with the concentration of 3-6mol/L, heating, stirring, reacting, filtering after the reaction is finished, collecting filter residues, and drying;
s4, adding the dried filter residue obtained in the step S3 into an ammonium chloride solution with the mass concentration of 5-8%, stirring at normal temperature for reaction, filtering after the reaction is finished, collecting the filter residue, drying, and calcining at high temperature to obtain powder;
and S5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, adding hydrofluoric acid, heating, stirring, reacting, filtering after the reaction is finished, and washing and drying the obtained filter residue to obtain the high-purity magnesium fluoride crystal material.
2. The method for preparing a high-purity magnesium fluoride crystalline material as claimed in claim 1, wherein the high-temperature calcination in S1 is carried out at a temperature of 600-800 ℃ for a period of 2-4 h.
3. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein the heating and stirring reaction in S2 is carried out at a temperature of 80-90 ℃ for 3-5 hours.
4. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein in S2, the ratio of the light burned ore powder to the ammonium chloride solution is 1 g: (30-40) mL.
5. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein in S3, the ratio of the leaching solution, the surfactant and the ammonia water solution is 1 mL: (0.01-0.05) g: (0.5-1) mL; the surfactant is sodium dodecyl sulfate, sodium dodecyl benzene sulfonate or a combination thereof.
6. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein the heating and stirring reaction in S3 is carried out at a temperature of 40-60 ℃ for 1.5-2.5 hours.
7. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein in S4, the ratio of the dried filter residue to the ammonium chloride solution is 1 g: (20-30) mL, and the reaction time is 2-4h under stirring at normal temperature.
8. The method for preparing a high-purity magnesium fluoride crystalline material as claimed in claim 1, wherein the temperature of the high-temperature calcination in S4 is 400-450 ℃ and the time is 0.5-1 h.
9. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein in S5, the mass ratio of the powder, water and hydrofluoric acid is 1: (0.3-0.5): (2-3).
10. The method for preparing a high-purity magnesium fluoride crystal material according to claim 1, wherein the heating and stirring reaction in S5 is carried out at 80-90 ℃ for 4-5 hours.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219800A (en) * | 2007-01-08 | 2008-07-16 | 杜高翔 | Method for producing nano-magnesium hydroxide by using low-level magnesite |
| CN101759206A (en) * | 2009-12-29 | 2010-06-30 | 孙力厚 | Process for preparing magnesia with high purity |
| CN106348322A (en) * | 2016-10-11 | 2017-01-25 | 张旭 | Method for preparing high-purity magnesium fluoride by using magnesite |
| US20170081204A1 (en) * | 2014-04-10 | 2017-03-23 | Karnalyte Resources Inc. | Process for producing high grade hydromagnesite and magnesium oxide |
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- 2022-06-14 CN CN202210668707.4A patent/CN115012037B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101219800A (en) * | 2007-01-08 | 2008-07-16 | 杜高翔 | Method for producing nano-magnesium hydroxide by using low-level magnesite |
| CN101759206A (en) * | 2009-12-29 | 2010-06-30 | 孙力厚 | Process for preparing magnesia with high purity |
| US20170081204A1 (en) * | 2014-04-10 | 2017-03-23 | Karnalyte Resources Inc. | Process for producing high grade hydromagnesite and magnesium oxide |
| CN106348322A (en) * | 2016-10-11 | 2017-01-25 | 张旭 | Method for preparing high-purity magnesium fluoride by using magnesite |
Non-Patent Citations (1)
| Title |
|---|
| 董庆国;白阳;吴清峰;黄浩;常俊基;: "辽宁某低品位菱镁矿浮选除杂试验研究", 非金属矿, no. 03 * |
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