CN115012037B - Preparation method of high-purity magnesium fluoride crystal material - Google Patents
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- CN115012037B CN115012037B CN202210668707.4A CN202210668707A CN115012037B CN 115012037 B CN115012037 B CN 115012037B CN 202210668707 A CN202210668707 A CN 202210668707A CN 115012037 B CN115012037 B CN 115012037B
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- C—CHEMISTRY; METALLURGY
- 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
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/28—Fluorides
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- C—CHEMISTRY; METALLURGY
- 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
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/04—Production of homogeneous polycrystalline material with defined structure from liquids
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- C—CHEMISTRY; METALLURGY
- 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
- 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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- 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
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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 mineral powder, heating with 15-20% ammonium chloride solution to obtain magnesium-calcium ion-containing leaching solution, uniformly mixing the leaching solution with a surfactant, precipitating with ammonia water, treating the obtained filter residue with 5-8% ammonium chloride solution to remove calcium ions, calcining at high temperature, uniformly mixing the obtained powder with a proper amount of water, 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 to coat a film on the surface of an optical device, such as a lens, a filter, etc., so as to achieve the purposes of antireflection, transmittance improvement, etc. 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 has ideal anti-reflection effect, 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 critical index, and therefore, a higher requirement is also put on the purity of the magnesium fluoride material used in the field. The current mainstream industrial preparation method of magnesium fluoride material is magnesium carbonate method, namely, magnesite is used as raw material, impurities in the raw material are removed through a certain pretreatment, and then the raw material reacts with hydrofluoric acid, so that the magnesium fluoride material with high purity is obtained. Although the method has the advantages of low cost and simple process, the magnesium fluoride material meeting the requirements of optical coating performance is difficult to obtain. Whereas the magnesium oxide method, the sol-gel method, etc. either require a high purity raw material or the production process is complicated and can be applied only to laboratory 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 technology, 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 a high temperature to obtain light calcined mineral powder;
s2, adding the light burned mineral powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 15-20%, heating, stirring, reacting, filtering after the reaction is finished, and collecting leaching liquid;
s3, uniformly mixing the leaching solution obtained in the step S2 with a surfactant, then adding an ammonia water solution with the concentration of 3-6mol/L, heating and stirring for reaction, 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 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 and reacting, filtering after the reaction is finished, and washing and drying the obtained filter residues to obtain the high-purity magnesium fluoride crystal material.
Preferably, in S1, the high temperature calcination temperature is 600-800 ℃ and the time is 2-4h.
Preferably, in S2, the temperature of the heating and stirring reaction is 80-90 ℃ and the time is 3-5h.
Preferably, in S2, the ratio of the light burned mineral powder to the ammonium chloride solution is 1g: (30-40) mL.
Preferably, in S3, the ratio of leachate, surfactant and aqueous ammonia solution is 1mL: (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 temperature of the heating and stirring reaction is 40-60 ℃ and the time is 1.5-2.5h.
Preferably, in S4, the ratio of the dried filter residue to the ammonium chloride solution is 1g: (20-30) mL, and stirring at normal temperature for 2-4h.
Preferably, in S4, the high temperature calcination is carried out at a temperature of 400-450 ℃ for 0.5-1h.
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 temperature of the heating and stirring reaction is 80-90 ℃ and the time is 4-5h.
The beneficial effects of the invention are as follows:
the invention takes low-grade magnesite powder as raw material, light burned mineral powder is obtained through high-temperature calcination to form oxides containing magnesium and impurities such as silicon, calcium, iron, aluminum and the like, then the oxides are mixed with high-concentration ammonium chloride solution and heated for decomposition reaction, magnesium oxide and calcium oxide are dissolved out to obtain leaching solution containing magnesium ions and calcium ions, so that the impurities such as silicon, iron, aluminum and the like are primarily removed, then under the assistance of a surfactant, magnesium ions and calcium ions are further separated and precipitated under proper conditions by ammonia water to form uniform precipitated phase, calcium ions and other impurities are fully dissolved out from the precipitated phase by low-concentration ammonium chloride solution, residual surfactant is removed through high-temperature calcination of the precipitated phase, and MgO with high purity is obtained at the same time, and the MgO with high purity is reacted 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 scheme of the invention is described in detail through specific embodiments.
In the following examples and comparative examples, the chemical composition of the magnesite powder used 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 mineral powder;
s2, adding the light burned mineral powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 15%, wherein the ratio of the light burned mineral powder to the ammonium chloride solution is 1g:40mL, heating and stirring at 80 ℃ for reaction for 5h, filtering after the reaction is finished, and collecting leaching liquid;
s3, uniformly mixing the leaching solution obtained in the step S2 with sodium dodecyl sulfate, and then adding an ammonia water solution with the concentration of 3mol/L, wherein the ratio of the leaching solution to the sodium dodecyl sulfate to the ammonia water solution is 1mL:0.05g:1mL, heating and stirring at 40 ℃ for 2.5h, filtering after the reaction, 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 1g:30mL, stirring at normal temperature for reaction for 2h, filtering after the reaction is finished, collecting filter residues, drying, and calcining at 400 ℃ for 1h to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, and then adding hydrofluoric acid, heating and stirring at 80 ℃ for reaction 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 residues 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 mineral powder;
s2, adding the light burned mineral powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 20%, wherein the ratio of the light burned mineral powder to the ammonium chloride solution is 1g:30mL, heating and stirring at 90 ℃ for reaction for 3h, filtering after the reaction is finished, and collecting leaching liquid;
s3, uniformly mixing the leaching solution obtained in the step S2 with sodium dodecyl sulfate, and then adding an ammonia water solution with the concentration of 6mol/L, wherein the ratio of the leaching solution to the sodium dodecyl sulfate to the ammonia water solution is 1mL:0.01g:0.5mL, heating and stirring at 60 ℃ to react 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 1g: stirring 20mL at normal temperature for reaction for 4h, filtering after the reaction is finished, collecting filter residues, drying, and calcining at a 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, and then adding hydrofluoric acid, heating and stirring at 90 ℃ for reaction 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 residues 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 mineral powder;
s2, adding the light burned mineral powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 18%, wherein the ratio of the light burned mineral powder to the ammonium chloride solution is 1g:35mL, heating and stirring at 85 ℃ for reaction for 4 hours, filtering after the reaction is finished, and collecting leaching liquid;
s3, uniformly mixing the leaching solution obtained in the step S2 with sodium dodecyl sulfate, and then adding an ammonia water solution with the concentration of 5mol/L, wherein the ratio of the leaching solution to the sodium dodecyl sulfate to the ammonia water solution is 1mL:0.04g:0.8mL, heating and stirring at 50 ℃ for 2h, filtering after the reaction, 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 1g:25mL, stirring at normal temperature for reaction for 3h, filtering after the reaction is finished, collecting filter residues, drying, and calcining at 420 ℃ for 40min to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, and then adding hydrofluoric acid, heating and stirring at 85 ℃ for reaction 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 residues 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 mineral powder;
s2, adding the light burned mineral powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 18%, wherein the ratio of the light burned mineral powder to the ammonium chloride solution is 1g:35mL, heating and stirring at 85 ℃ for reaction for 4 hours, filtering after the reaction is finished, and collecting leaching liquid;
s3, adding 5mol/L ammonia water solution into the leaching solution obtained in the step S2, wherein the ratio of the leaching solution to the ammonia water solution is 1mL:0.8mL, heating and stirring at 50 ℃ for 2h, filtering after the reaction, 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 1g:25mL, stirring at normal temperature for reaction for 3h, filtering after the reaction is finished, collecting filter residues, drying, and calcining at 420 ℃ for 40min to obtain powder;
s5, uniformly mixing the powder obtained in the step S4 with a proper amount of water, and then adding hydrofluoric acid, heating and stirring at 85 ℃ for reaction 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 residues to obtain the high-purity magnesium fluoride crystal material.
The magnesium fluoride crystal materials prepared in examples 1-3 and comparative example 1 were subjected to the following standard: the detection results of purity and impurity detection of GB/T31860-2015 magnesium fluoride for coating show that the magnesium fluoride crystal materials prepared in examples 1-3 can meet the technical requirements that the magnesium fluoride content is more than or equal to 99.90% and the Ca content is less than or equal to 0.015%, and the magnesium fluoride crystal material has low impurity content and high purity and can meet the performance requirements of the magnesium fluoride material for coating; the magnesium fluoride crystal material prepared in comparative example 1 has a Ca content of 0.018% and a Ca content exceeding the standard, and cannot meet the performance requirements of the coating material.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The preparation method of the high-purity magnesium fluoride crystal material is characterized by comprising the following steps of:
s1, calcining magnesite powder at a high temperature to obtain light calcined mineral powder;
s2, adding the light burned mineral powder obtained in the step S1 into an ammonium chloride solution with the mass concentration of 15-20%, heating, stirring, reacting, filtering after the reaction is finished, and collecting leaching liquid;
s3, uniformly mixing the leaching solution obtained in the step S2 with a surfactant, then adding an ammonia water solution with the concentration of 3-6mol/L, heating and stirring for reaction, 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 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 and reacting, filtering after the reaction is finished, and washing and drying the obtained filter residues to obtain the high-purity magnesium fluoride crystal material.
2. The method for preparing a high purity magnesium fluoride crystal material according to claim 1, wherein in S1, the high temperature calcination temperature is 600 to 800 ℃ for 2 to 4 hours.
3. The method for preparing a high purity magnesium fluoride crystal material according to claim 1, wherein in S2, the temperature of the heating and stirring reaction is 80-90 ℃ for 3-5 hours.
4. The method for preparing high-purity magnesium fluoride crystal material according to claim 1, wherein in S2, the ratio of light burned ore powder to ammonium chloride solution is 1g: (30-40) mL.
5. The method for producing a high purity magnesium fluoride crystal material according to claim 1, wherein in S3, the ratio of the leaching solution, the surfactant and the aqueous ammonia solution is 1mL: (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 in S3, the temperature of the heating and stirring reaction is 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 1g: (20-30) mL, and stirring at normal temperature for 2-4h.
8. The method for preparing a high purity magnesium fluoride crystal material according to claim 1, wherein in S4, the high temperature calcination temperature is 400 to 450 ℃ for 0.5 to 1 hour.
9. The method for preparing a high purity magnesium fluoride crystal material according to claim 1, wherein in S5, the mass ratio of powder, water and hydrofluoric acid is 1: (0.3-0.5): (2-3).
10. The method for producing a high purity magnesium fluoride crystal material according to claim 1, wherein in S5, the temperature of the heating and stirring reaction is 80 to 90 ℃ for 4 to 5 hours.
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Citations (3)
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015154196A1 (en) * | 2014-04-10 | 2015-10-15 | Karnalyte Resources Inc. | Process for producing high grade hydromagnesite and magnesium oxide |
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Patent Citations (3)
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 辽宁某低品位菱镁矿浮选除杂试验研究;董庆国;白阳;吴清峰;黄浩;常俊基;;非金属矿(03) * |
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