CN110980752A - Preparation method of alkali metal-based fluorophlogopite sheet - Google Patents
Preparation method of alkali metal-based fluorophlogopite sheet Download PDFInfo
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Abstract
The invention discloses a preparation method of an alkali metal-based fluorophlogopite sheet, which comprises the following steps: (1) inspecting raw materials, grinding and drying; (2) weighing raw materials, stirring and mixing; (3) melting raw materials; (4) preserving heat; (5) cutting off power, and naturally cooling for crystallization; (6) opening the furnace, and taking out the alkali metal-based fluorophlogopite sheet; the sodium fluorophlogopite, the potassium fluorophlogopite and other substances prepared by the method endow fluorophlogopite sheets with various different material characteristics, and can meet the requirements of more industries.
Description
Technical Field
The invention belongs to the technical field of artificial mica sheet synthesis, and particularly relates to a preparation method of an alkali metal-based fluorophlogopite sheet.
Background
The reserves of natural mica in China are small and gradually exhausted, and the gradual replacement of natural mica by artificial mica is a necessary trend; over the years, the research and development and popularization of the artificial mica in China make great progress, and make a contribution to the national economic construction.
The artificial mica crystal is a layered silicate compound which is prepared by high-purity chemical raw materials and high-quality mineral raw materials through high-temperature reaction, melting, cooling, crystallization and growth; the hydroxyl in the natural mica is structurally substituted by fluorine to increase the structural stability and endow the mica with more diversified performances, and the chemical formula is as follows:
XY2.5～5SimO10Fn
wherein: x comprises at least one element of the alkali metal group, alkaline earth metal group or combinations thereof;
y comprises at least one compound of an element or combination thereof, the compound comprising: magnesium, aluminum, lithium, boron, and the like;
m is about 2 to 4, and n is about 1 to 3.
Patent CN104876234B discloses a preparation method of artificially synthesized fluorophlogopite, which comprises the following steps:(1) preparing raw materials: SiO contained in the raw material2、MgO、Al2O3、K2CO3And K2SiF6The molar ratio of (A) to (B) is: SiO 22：MgO：Al2O3：K2CO3：K2SiF6(16-a): 18: 3: (1-a): (2+ a), a is more than or equal to 0.1 and less than or equal to 0.5; (2) building a furnace body, and installing an upper electrode; (3) uniformly mixing the raw materials, and filling the mixture into a furnace body; (4) electrifying to melt the raw materials in the furnace body; (5) cutting off power, and naturally cooling for crystallization; (6) opening the furnace and taking out the artificially synthesized mica. According to the technical scheme, the high-quality artificially synthesized fluorophlogopite is synthesized by optimizing the raw material formula, and the prepared artificially synthesized fluorophlogopite is not mixed with other crystals, meets the requirement of pearlescent package, is clear and transparent, is flexible, is complete in crystallization, is large in wafer and has good electrical insulation performance; but the formula is single, the universality is poor, and the requirements of the market on higher purity and more element functionalization of the artificial mica crystal cannot be met.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of an alkali metal-based fluorophlogopite sheet, which is used for preparing sodium type fluorophlogopite, potassium type fluorophlogopite and other substances, endowing the sodium type fluorophlogopite, the potassium type fluorophlogopite and other substances with various material characteristics, and meeting the requirements of more industries.
A preparation method of an alkali metal-based fluorophlogopite sheet comprises the following steps:
(1) after the raw materials are qualified, grinding the raw materials by a grinding machine and then drying the raw materials for later use;
(2) weighing the raw materials according to the mass ratio, wherein the raw materials comprise the following components: 41-47% of quartz sand, 22-26% of seawater magnesia, 11-14% of alumina, 7-8.5% of magnesium fluoride and 5-14% of alkali metal fluoride, and mixing and uniformly stirring the raw materials;
(3) adding the mixed raw material part obtained in the step (2) into an internal heating furnace, compacting the mixed raw material by using a heavy object, increasing the material density, and discharging redundant air; electrifying for melting, heating and decomposing the raw materials in an internal heating furnace, volatilizing the molten gas and carrying out chemical reaction, wherein the melting temperature is 1500-1550 ℃, and continuously adding the rest of the mixed raw materials prepared in the step (2) in the process to keep the reaction substances sufficient;
(4) when the added mixed raw materials are completely melted, adding a layer of return charge and powder with uniform thickness to the surface of the furnace, preserving heat for 5-8 hours, cooling to 1150-1450 ℃, and preserving heat for 1-2 hours;
(5) cutting off the power, and naturally cooling and crystallizing the materials in the furnace body;
(6) opening the furnace, and taking out the alkali metal-based fluorophlogopite sheet.
Preferably, the alkali metal fluoride is potassium fluoride or sodium fluoride.
More preferably, when the alkali metal fluoride is potassium fluoride, the starting material has the composition: 41-43% of quartz sand, 22-24% of seawater magnesia, 11-13% of alumina, 7-7.5% of magnesium fluoride and 12-14% of potassium fluoride.
More preferably, when the alkali metal fluoride is sodium fluoride, the composition of the starting material is: 42-45% of quartz sand, 23-25% of seawater magnesia, 12-14% of alumina, 7.5-8% of magnesium fluoride and 9-11% of sodium fluoride.
Preferably, the internal heating furnace is built by three-stage high-alumina refractory bricks.
Preferably, in the step (1), the raw materials are ground to be less than 100 meshes, and dried to ensure that the moisture of each component is less than or equal to 0.5%.
Compared with the prior art, the invention has the following technical advantages:
(1) the invention adopts seawater magnesite as one of the synthetic raw materials, the seawater magnesite is the sediment extracted from seawater by a chemical method, and the sintered magnesite produced by high-temperature sintering has higher chemical purity and volume density than the fused magnesite adopted in the prior art.
As shown in the figure 1, the structure of potassium fluorophlogopite sheet shows that magnesium plays a crystal nucleus role in crystal form, and Ca can be greatly weakened by adopting seawater magnesite2+The adverse effect of ions and the like on the sintering process enables the crystal form to grow more stably and improves the purity of the product.
(2) The potassium fluorophlogopite sheet prepared by the invention has excellent insulating property, and can still show excellent insulating property at 500 ℃ because the size of potassium ions is larger in the sheet layer, while the sodium fluorophlogopite sheet has excellent conductivity, because the sodium fluorophlogopite sheet has a multilayer composite interlayer cation structure and can be used as an excellent ion conductor, because the cation radius is smaller than that of potassium element and has more active electrical property, the conductivity is caused by the cation motion between the sheet layers, and the principle of the structural characteristic is similar to that of a conductor mechanism of β -alumina.
(3) The process for preparing the synthetic mica sheet has the advantages that the variety of required raw materials is few, substances such as sodium fluorophlogopite sheets and potassium fluorophlogopite sheets can be prepared by adjusting the proportion of the raw materials, the universality is strong, the purity of the synthetic product is high, byproducts are not generated basically, the ratio of the raw material formula to the converted finished product is effectively improved, the energy efficiency is saved, the use of potassium fluosilicate is reduced, the operation is simple, and the safety is high;
(4) the conductive sodium fluorophlogopite sheet prepared for the first time has the advantages of sheet structure, excellent conductivity, high appearance whiteness and high purity, is suitable for being used in the high-end electronic information field, and widens the application range of the fluorophlogopite sheet in the market.
Drawings
FIG. 1 is a structural view of potassium fluorophlogopite mica of technical advantage (1) in the present invention
FIG. 2 is an SEM image of a sodium fluorophlogopite sheet prepared by the present invention
FIG. 3 is an SEM image of potassium fluorophlogopite flake prepared according to the present invention
Detailed Description
The present invention will be further described with reference to the following detailed description and accompanying drawings.
The foundry returns in the invention are raw material mixtures which are not completely reacted and are adhered to the furnace wall after being sintered according to the preparation method disclosed in the invention, because the materials are heated to a reaction temperature, the materials are not completely crystallized, are not of a synthetic mica structure, but can be used as an insulating layer without polluting the raw material mixtures; the powder is a mixed reaction raw material, and because the density and the volume are changed in the synthesis reaction, the powder is used for supplementing the mixed raw material, the total reaction amount is increased, and the production efficiency of a single furnace is improved.
Example 1
A preparation method of a sodium fluorophlogopite sheet with conductivity comprises the following steps:
(1) after the raw materials are qualified, grinding the raw materials to 90 meshes by using a grinding machine, and drying the raw materials until the water content is 0.5 percent for later use;
(2) weighing the raw materials according to the mass ratio, wherein the raw materials comprise the following components: 45% of quartz sand, 25% of seawater magnesia, 13% of alumina, 8% of magnesium fluoride and 9% of sodium fluoride, and uniformly mixing and stirring the raw materials;
(3) adding the mixed raw material obtained in the step (2) into an internal heating furnace, and adding 2/3 in total amount; the internal heating furnace is built by three-level high-alumina refractory bricks, mixed raw materials are compacted by a heavy object, the material density is increased, and redundant air is discharged; electrifying for melting, heating and decomposing the raw materials in an internal heating furnace, volatilizing the molten gas and carrying out chemical reaction, wherein the melting temperature is 1400 ℃, and continuously adding the mixed raw materials prepared in the rest step (2) in the process to keep the sufficiency of reaction substances;
(4) when the added mixed raw materials are completely melted, adding a layer of return charge and powder with uniform thickness to the surface of the furnace, preserving heat for 5 hours, then cooling to 1150 ℃, and preserving heat for 1 hour;
(5) cutting off the power, and naturally cooling and crystallizing the materials in the furnace body;
(6) opening the furnace, and taking out the sodium fluorophlogopite sheet with the conductivity.
The prepared sodium fluorophlogopite sheet has the conductivity of 4.3 multiplied by 10 at 650 DEG C-4S/cm。
Example 2
A preparation method of potassium fluorophlogopite sheet with insulating property comprises the following steps:
(1) after the raw materials are qualified, grinding the raw materials to 80 meshes by using a grinder, and drying the raw materials until the water content is 0.4 percent for later use;
(2) weighing the raw materials according to the mass ratio, wherein the raw materials comprise the following components: 43% of quartz sand, 24% of seawater magnesia, 12% of alumina, 7% of magnesium fluoride and 14% of potassium fluoride, and uniformly mixing and stirring the raw materials;
(3) adding the mixed raw material obtained in the step (2) into an internal heating furnace, and adding 2/3 in total amount; the internal heating furnace is built by three-level high-alumina refractory bricks, mixed raw materials are compacted by a heavy object, the material density is increased, and redundant air is discharged; electrifying for melting, heating and decomposing the raw materials in an internal heating furnace, volatilizing the molten gas and carrying out chemical reaction, wherein the melting temperature is 1520 ℃, and continuously adding the mixed raw materials prepared in the rest step (2) in the process to keep the sufficiency of reaction substances;
(4) when the added mixed raw materials are completely melted, adding a layer of foundry returns and powder with uniform thickness to the surface of the furnace, preserving heat for 6 hours, then cooling to 1200 ℃, and preserving heat for 1.5 hours;
(5) cutting off the power, and naturally cooling and crystallizing the materials in the furnace body;
(6) opening the furnace, and taking out the potassium fluorophlogopite sheet with the insulating property.
Comparative example 1
The potassium fluorophlogopite flake of this comparative example was prepared as disclosed in patent CN 104876234B.
Measurement of Performance
The potassium fluorophlogopite platelets prepared in example 2 and comparative example 1 were subjected to property measurement, and the measurement results are shown in table 1;
TABLE 1 comparison table of insulation properties of potassium fluorophlogopite sheet
| Example 2 | Comparative example 1 | |
| Breakdown strength/kv/mm | 230 | 199 |
| Volume resistivity/omega. cm | 5.5×1015 | 4.2×1015 |
| Surface resistivity/omega | 3.3×1013 | 2.1×1013 |
Claims (6)
1. A preparation method of an alkali metal-based fluorophlogopite sheet is characterized by comprising the following steps:
(1) after the raw materials are qualified, grinding the raw materials by a grinding machine and then drying the raw materials for later use;
(2) weighing the raw materials according to the mass ratio, wherein the raw materials comprise the following components: 41-47% of quartz sand, 22-26% of seawater magnesia, 11-14% of alumina, 7-8.5% of magnesium fluoride and 5-14% of alkali metal fluoride, and mixing and uniformly stirring the raw materials;
(3) adding the mixed raw material part obtained in the step (2) into an internal heating furnace, compacting the mixed raw material by using a heavy object, increasing the material density, and discharging redundant air; electrifying for melting, heating and decomposing the raw materials in an internal heating furnace, volatilizing the molten gas and carrying out chemical reaction, wherein the melting temperature is 1500-1550 ℃, and continuously adding the rest of the mixed raw materials prepared in the step (2) in the process to keep the reaction substances sufficient;
(4) when the added mixed raw materials are completely melted, adding a layer of return charge and powder with uniform thickness to the surface of the furnace, preserving heat for 5-8 hours, cooling to 1150-1450 ℃, and preserving heat for 1-2 hours;
(5) cutting off the power, and naturally cooling and crystallizing the materials in the furnace body;
(6) opening the furnace, and taking out the alkali metal-based fluorophlogopite sheet.
2. The method for preparing an alkali metal-based fluorophlogopite flake according to claim 1, wherein: the alkali metal fluoride is potassium fluoride or sodium fluoride.
3. The method for preparing an alkali metal-based fluorophlogopite flake according to claim 2, wherein: when the alkali metal fluoride is potassium fluoride, the raw materials comprise the following components: 41-43% of quartz sand, 22-24% of seawater magnesia, 11-13% of alumina, 7-7.5% of magnesium fluoride and 12-14% of potassium fluoride.
4. The method for preparing an alkali metal-based fluorophlogopite flake according to claim 2, wherein: when the alkali metal fluoride is sodium fluoride, the composition of the starting material is: 42-45% of quartz sand, 23-25% of seawater magnesia, 12-14% of alumina, 7.5-8% of magnesium fluoride and 9-11% of sodium fluoride.
5. The method for preparing an alkali metal-based fluorophlogopite flake according to claim 1, wherein: the internal heating furnace is built by three-level high-alumina refractory bricks.
6. The method for preparing an alkali metal-based fluorophlogopite flake according to claim 1, wherein: in the step (1), the raw materials are ground to be below 100 meshes, and dried to ensure that the moisture of each component is less than or equal to 0.5 percent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826717A (en) * | 2020-07-14 | 2020-10-27 | 广东三宝新材料科技股份有限公司 | Artificially synthesized black mica crystal and crystallization method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0789713A (en) * | 1992-07-28 | 1995-04-04 | Mizusawa Ind Chem Ltd | Production of fluoromica |
| JP2004161612A (en) * | 2004-01-05 | 2004-06-10 | Kose Corp | Synthetic mica |
| CN101037208A (en) * | 2006-03-14 | 2007-09-19 | 中国科学院过程工程研究所 | Method for preparing swelled fluorine mica by kaoline |
| CN104876234A (en) * | 2015-04-16 | 2015-09-02 | 汕头保税区三宝光晶云母科技有限公司 | Preparation method for manually synthesized fluorophlogopite |
| CN104876233A (en) * | 2015-04-16 | 2015-09-02 | 汕头保税区三宝光晶云母科技有限公司 | Method for preparing artificially synthesized fluorophlogopite |
| CN109279617A (en) * | 2018-10-30 | 2019-01-29 | 安徽恒昊科技有限公司 | A kind of chemical synthesis process of mica |
-
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- 2019-07-25 CN CN201910676569.2A patent/CN110980752A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0789713A (en) * | 1992-07-28 | 1995-04-04 | Mizusawa Ind Chem Ltd | Production of fluoromica |
| JP2004161612A (en) * | 2004-01-05 | 2004-06-10 | Kose Corp | Synthetic mica |
| CN101037208A (en) * | 2006-03-14 | 2007-09-19 | 中国科学院过程工程研究所 | Method for preparing swelled fluorine mica by kaoline |
| CN104876234A (en) * | 2015-04-16 | 2015-09-02 | 汕头保税区三宝光晶云母科技有限公司 | Preparation method for manually synthesized fluorophlogopite |
| CN104876233A (en) * | 2015-04-16 | 2015-09-02 | 汕头保税区三宝光晶云母科技有限公司 | Method for preparing artificially synthesized fluorophlogopite |
| CN109279617A (en) * | 2018-10-30 | 2019-01-29 | 安徽恒昊科技有限公司 | A kind of chemical synthesis process of mica |
Non-Patent Citations (2)
| Title |
|---|
| 夏征农等: "《大辞海 第37卷 材料科学卷》", 31 December 2015, 上海辞书出版社 * |
| 李勇等: "《铜冶金用镁铬耐火材料》", 31 January 2014, 冶金工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111826717A (en) * | 2020-07-14 | 2020-10-27 | 广东三宝新材料科技股份有限公司 | Artificially synthesized black mica crystal and crystallization method thereof |
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Application publication date: 20200410 |