CN108358456B - Method for preparing microcrystalline glass by using gold tailings and fluorite tailings - Google Patents
Method for preparing microcrystalline glass by using gold tailings and fluorite tailings Download PDFInfo
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- CN108358456B CN108358456B CN201810505791.1A CN201810505791A CN108358456B CN 108358456 B CN108358456 B CN 108358456B CN 201810505791 A CN201810505791 A CN 201810505791A CN 108358456 B CN108358456 B CN 108358456B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0063—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
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Abstract
The invention discloses a method for preparing microcrystalline glass by using gold tailings and fluorite tailings, which comprises the steps of heating and melting the gold tailings, the fluorite tailings and a modifier to obtain molten glass, carrying out water quenching treatment to form glass particles, carrying out crushing and screening treatment, selecting the glass particles, drying, paving the glass particles on a mold, sintering, crystallizing, carrying out heat preservation, annealing and cooling, and polishing and grinding the surface of a product to obtain the finished product microcrystalline glass. The method has the advantages of high comprehensive utilization rate of the gold tailings and the fluorite tailings, simple preparation method, convenient raw material source and low cost, and the prepared microcrystalline glass has excellent bending strength and microhardness, is free of fluoride leaching, has higher added value, provides a new way for resource comprehensive utilization of the gold tailings and the fluorite tailings, and has remarkable economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of building materials, relates to a method for preparing microcrystalline glass by taking industrial waste residues as raw materials, and particularly relates to a method for preparing microcrystalline glass by utilizing gold tailings and fluorite tailings.
Background
The microcrystal glass is also called glass ceramic, and is a composite material containing a large amount of microcrystal phases and uniformly distributed glass phases, which is prepared by performing certain heat treatment on base glass with a specific composition and controlling crystallization. The microcrystalline glass has adjustable thermal expansion coefficient, higher mechanical strength, obvious corrosion resistance, weathering resistance and good thermal stability, is a good substitute material for natural stone, and can be used in the fields of architectural decoration, aerospace, electronic and mechanical industries and the like.
The gold tailings are waste residues produced in the process of refining gold by a flotation method after crushing gold-containing ores. With the rapid development of gold extraction technology in China, the number, scale and yield of gold mines are increasing day by day, the mining intensity is increasing day by day, and the tailing amount is also increasing sharply. The gold tailings mainly comprise silicon dioxide, aluminum oxide and ferric oxide, and other valuable metals and minerals which can be comprehensively recovered, and have the characteristics of fine granularity, large quantity, high availability, low price, low treatment cost and the like, and are valuable secondary resources. At present, a large amount of gold tailings are accumulated, so that the ecological environment is adversely affected, and a series of environmental pollution problems are caused, for example, certain harmful gases in the tailings weathering process pollute the atmosphere, and in a flood season, the tailings and rainwater flow into farmland rivers to cause underground water pollution and the like.
Fluorite tailings mainly refer to floated ores, the main component of the fluorite tailings is silicon dioxide, and the fluorite tailings also contain a small amount of calcium fluoride, aluminum fluoride, calcium carbonate, iron oxide and other components, waste residues are fluorgypsum, and the main component of the waste residues is calcium sulfate. The stacking of fluorite tailings occupies a large amount of land, so that potential safety hazards are caused, and the ore dressing agent contained in the fluorite tailings can permeate underground to pollute underground water, thereby bringing a series of environmental problems.
The effective components in the gold tailings and the fluorite tailings are utilized to obtain a product with a higher added value, so that the economic benefit can be greatly improved, and the method has great significance for solving the problem of environmental pollution of the gold tailings and the fluorite tailings and realizing circular economy.
For example, chinese patent application CN103553468A (published as 2014, 2, 5) discloses a method for manufacturing aerated bricks by using gold mine tailings and fluorite tailings, which comprises: grinding the gold tailings, decyanating, finely grinding and uniformly mixing quicklime, fluorgypsum, fluorite tailings, silicon powder and cement to prepare mixed powder, mixing and stirring the decyanation slurry, the mixed powder, aluminum powder paste and water to obtain mixed slurry, pouring the mixed slurry into a blank mold, foaming a green blank, and cutting and autoclaving the green blank to obtain the finished product of the aerated brick.
For example, chinese patent application CN104071983A (published as 2014, 10 and 1) discloses a sintering process for producing a microcrystalline glass plate by using fluorite tailings, which comprises the following steps: after the fluorite tailings and the modifying agent are uniformly mixed, heating, melting and fully stirring are carried out to obtain molten glass, and after water quenching, grinding, screening, die filling and heat treatment are carried out, the microcrystalline glass plate is obtained.
For example, chinese patent application CN107459284A (published as 12.12.2017) discloses a composite board prepared from waste residues of fly ash, red mud, and fluorite tailings, and a preparation method thereof, wherein the waste residues of red mud, fly ash, fluorite tailings, etc. are used as raw materials, and are mixed with a base material and a heat stabilizer, and then are treated by a reasonable proportion and a preparation process, so that the prepared composite board has excellent performance, a large amount of waste residues to be mixed, and a low cost.
For example, chinese patent application CN107417123A (published as 2017, 12 and 1) discloses a method for preparing microcrystalline glass from stainless steel slag and fluorite tailings, which comprises: preparing fine stainless steel slag powder and fine fluorite tailing powder according to a certain mass ratio, uniformly mixing, melting the mixture in a resistance furnace to obtain a high-temperature melt, pouring the high-temperature melt onto a preheated steel plate, cooling the high-temperature melt along with the furnace to obtain mother glass, and performing heat treatment to obtain the microcrystalline glass.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing microcrystalline glass by using gold tailings and fluorite tailings, and simultaneously, the gold tailings and the fluorite tailings are reasonably used to improve the recycling rate of the gold tailings and the fluorite tailings.
Specifically, the method for preparing the microcrystalline glass by using the gold tailings and the fluorite tailings comprises the following steps of:
(1) preparing materials: the raw materials utilized by the method comprise gold tailings, fluorite tailings and a modifier; the content of the gold tailings is 25-30%, the content of the fluorite tailings is 20-30%, and the balance is a modifier, wherein the content is the mass percentage content;
the gold tailings mainly comprise the following chemical components in percentage by mass: 65-75% of silicon dioxide, 10-20% of aluminum oxide, 0-5% of calcium oxide, 4-7% of potassium oxide, 2-5% of sodium oxide, 1-3% of iron oxide and 0-2% of magnesium oxide, wherein the content of other components is less than 1% (the content of gold tailings is reduced to about 1-3%); preferably, the granularity of the gold tailings is more than 100 meshes.
The fluorite tailings mainly comprise the following chemical components in percentage by mass: 75-85% of silicon dioxide, 3-8% of aluminum oxide, 0-1% of calcium oxide, 1-3% of potassium oxide, 0-1% of sodium oxide, 1-3% of iron oxide, 0-1% of magnesium oxide, 2-5% of calcium fluoride, and the content of other components is less than 1% (the burning rate of fluorite tailings is reduced to about 1-3%); preferably, the fluorite tailings have a particle size of 100 meshes or more.
The modifier is selected from one or more of industrial quartz sand, alumina, calcite, potash feldspar, barium carbonate, zinc oxide and calcined soda, and mainly comprises the following components in percentage by mass: 30-50% of silicon dioxide, 25-45% of calcium oxide, 8-10% of barium oxide, 2-4% of zinc oxide, 8-10% of sodium oxide, and the content of other components is less than 1%; preferably, the modifier has a particle size of 200 mesh or more.
(2) Melting: uniformly mixing the gold tailings, the fluorite tailings and the modifier, heating for melting, and fully stirring to obtain molten glass; wherein the melting temperature is preferably kept between 1450 and 1550 ℃;
in the mixing process, a V-shaped mixer is adopted for mixing.
In the material melting process, the heat preservation time is 2-3 hours (h).
In the process of melting, stirring slurry is adopted for stirring uniformly.
(3) Water quenching: flowing the molten glass into a water quenching tank, and performing water quenching treatment to form glass particles;
in the water quenching process, the water temperature of the water quenching tank is normal temperature, and the glass solution is cooled to the normal temperature within 1-2 seconds after entering the water quenching tank.
(4) Grinding and screening: carrying out crushing and screening treatment on the glass particles, selecting the glass particles with proper granularity, and carrying out drying treatment; selecting glass particles with the granularity of 10-100 meshes, and achieving the best effect;
in the crushing process, the ceramic pot is added with ceramic balls or corundum balls for crushing.
(5) Die filling: after being dried, the glass particles are laid on a mould and sintered;
the material of the mould is high temperature resistant material such as alumina, zirconia or silicon carbide boron plate.
In the sintering process, the temperature is raised to 950-1000 ℃ at the rate of 5-10 ℃/min (min) and is kept for 0.5-1 h.
(6) And (3) heat treatment: comprises the steps of crystallization, heat preservation, annealing and cooling.
In the crystallization process, the temperature is raised to 1100-1200 ℃ at the temperature raising speed of 5-8 ℃/min and the temperature is preserved.
In the heat preservation process, the temperature is 1100-1200 ℃ and the heat preservation is carried out for 1-3 h.
In the annealing cooling process, the temperature is reduced to 700-800 ℃ at the cooling speed of 5-10 ℃/min, the temperature is kept for 1-2 h, and the temperature is reduced to below 100 ℃ at the cooling speed of 10-15 ℃/min.
(7) Grinding and polishing: and polishing and grinding the surface of the product to obtain the finished product of the microcrystalline glass.
The method has the advantages of high comprehensive utilization rate of the gold tailings and the fluorite tailings, simple preparation method, convenient raw material source and low cost, and the prepared microcrystalline glass has excellent bending strength and microhardness, is free of fluoride leaching, has higher added value, provides a new way for resource comprehensive utilization of the gold tailings and the fluorite tailings, and has remarkable economic and social benefits.
Detailed Description
Technical solutions in the embodiments of the present invention will be described in detail below, and it is apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The materials used in the following examples are available from the open market, unless otherwise specified.
Table 1 main components (mass% wt%) of gold tailings and fluorite tailings used in examples
Example 1
Table 2 main component (mass% wt%) of the modifier used in example 1
Table 3 composition of the raw materials of example 1
| Name (R) | Proportion (wt%) |
| Gold tailings | 30 |
| Fluorite tailings | 20 |
| Modifying agent | 50 |
Preparing the microcrystalline glass plate according to the raw material composition by adopting the following steps:
(1) crushing the gold tailings to obtain a granular material with the granularity of more than 100 meshes;
(2) crushing fluorite tailings to obtain a granular material with the granularity of more than 100 meshes;
(3) the particle size of the modifier is more than 200 meshes;
(4) drying and weighing the gold tailings, the fluorite tailings and the modifier granules, and mixing the dried and weighed materials in proportion;
(5) heating and melting the mixed raw materials, keeping the melting temperature at 1450-1500 ℃, and preserving the heat for 2.5 hours to obtain molten glass;
(6) enabling a molten glass discharge port to flow into a water quenching tank to obtain glass particles, crushing the glass particles, drying the glass particles, and screening the glass particles to obtain particles with the particle size of 10-100 meshes;
(7) flatly spreading particles with the granularity of 10-100 meshes into a mold, wherein the thickness of the particles is 10-20 mm;
(8) putting the paved die into a heating furnace;
(9) heating to 980 ℃ at the speed of 5-10 ℃/min, and preserving heat for 1 h;
(10) heating to 1110 ℃ at the speed of 5 ℃/min, and preserving heat for 1.5 h;
(11) reducing the temperature to 750 ℃ at the speed of 5 ℃/min, and preserving the heat for 1 h;
(12) cooling to below 100 ℃ at the speed of 10-15 ℃/min and discharging;
(13) and cutting, grinding and polishing the microcrystalline glass plate cooled to room temperature to obtain the finished microcrystalline glass plate.
Example 2
Table 4 main component (mass% wt%) of the modifier used in example 2
Table 5 raw material composition of example 2
| Name (R) | Proportion (wt%) |
| Gold tailings | 28 |
| Fluorite tailings | 24 |
| Modifying agent | 48 |
Preparing the microcrystalline glass plate according to the raw material composition by adopting the following steps:
(1) crushing the gold tailings to obtain a granular material with the granularity of more than 100 meshes;
(2) crushing fluorite tailings to obtain a granular material with the granularity of more than 100 meshes;
(3) the particle size of the modifier is more than 200 meshes;
(4) drying and weighing the gold tailings, the fluorite tailings and the modifier granules, and mixing the dried and weighed materials in proportion;
(5) heating and melting the mixed raw materials, keeping the melting temperature at 1450-1500 ℃, and preserving the heat for 2.5 hours to obtain molten glass;
(6) enabling a molten glass discharge port to flow into a water quenching tank to obtain glass particles, crushing the glass particles, drying the glass particles, and screening the glass particles to obtain particles with the particle size of 10-100 meshes;
(7) flatly spreading particles with the granularity of 10-100 meshes into a mold, wherein the thickness of the particles is 10-20 mm;
(8) putting the paved die into a heating furnace;
(9) heating to 980 ℃ at the speed of 5-10 ℃/min, and preserving heat for 1 h;
(10) heating to 1110 ℃ at the speed of 5 ℃/min, and preserving heat for 1.5 h;
(11) reducing the temperature to 750 ℃ at the speed of 5 ℃/min, and preserving the heat for 1 h;
(12) cooling to below 100 ℃ at the speed of 10-15 ℃/min and discharging;
(13) and cutting, grinding and polishing the microcrystalline glass plate cooled to room temperature to obtain the finished microcrystalline glass plate.
Example 3
Table 6 main component (mass% wt%) of the modifier used in example 3
Table 7 raw material composition of example 3
| Name (R) | Proportion (wt%) |
| Gold tailings | 25 |
| Fluorite tailings | 28 |
| Modifying agent | 47 |
Preparing the microcrystalline glass plate according to the raw material composition by adopting the following steps:
(1) crushing the gold tailings to obtain a granular material with the granularity of more than 100 meshes;
(2) crushing fluorite tailings to obtain a granular material with the granularity of more than 100 meshes;
(3) the particle size of the modifier is more than 200 meshes;
(4) drying and weighing the gold tailings, the fluorite tailings and the modifier granules, and mixing the dried and weighed materials in proportion;
(5) heating and melting the mixed raw materials, keeping the melting temperature at 1450-1500 ℃, and preserving the heat for 2.5 hours to obtain molten glass;
(6) enabling a molten glass discharge port to flow into a water quenching tank to obtain glass particles, crushing the glass particles, drying the glass particles, and screening the glass particles to obtain particles with the particle size of 10-100 meshes;
(7) flatly spreading particles with the granularity of 10-100 meshes into a mold, wherein the thickness of the particles is 10-20 mm;
(8) putting the paved die into a heating furnace;
(9) heating to 980 ℃ at the speed of 5-10 ℃/min, and preserving heat for 1 h;
(10) heating to 1110 ℃ at the speed of 5 ℃/min, and preserving heat for 1.5 h;
(11) reducing the temperature to 750 ℃ at the speed of 5 ℃/min, and preserving the heat for 1 h;
(12) cooling to below 100 ℃ at the speed of 10-15 ℃/min and discharging;
(13) and cutting, grinding and polishing the microcrystalline glass plate cooled to room temperature to obtain the finished microcrystalline glass plate.
TABLE 8 Properties of glass ceramics obtained in examples 1 to 3
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (1)
1. A method for preparing microcrystalline glass by using gold tailings and fluorite tailings is characterized by comprising the following steps:
s1, weighing raw materials according to a metering ratio, wherein the raw materials comprise 25-30 wt% of gold tailings, 20-30 wt% of fluorite tailings and the balance of modifier; the gold tailings have the granularity of more than 100 meshes and comprise the following components in percentage by mass: 65-75% of silicon dioxide, 10-20% of aluminum oxide, 0-5% of calcium oxide, 4-7% of potassium oxide, 2-5% of sodium oxide, 1-3% of iron oxide and 0-2% of magnesium oxide, wherein the content of other components is less than 1%; the fluorite tailings have the granularity of more than 100 meshes and comprise the following components in percentage by mass: 75-85% of silicon dioxide, 3-8% of aluminum oxide, 0-1% of calcium oxide, 1-3% of potassium oxide, 0-1% of sodium oxide, 1-3% of iron oxide, 0-1% of magnesium oxide, 2-5% of calcium fluoride, and the content of other components is less than 1%; the modifier is one or more of industrial quartz sand, alumina, calcite, potash feldspar, barium carbonate, zinc oxide and soda ash with the granularity of more than 200 meshes, and mainly comprises the following components in percentage by mass: 30-50% of silicon dioxide, 25-45% of calcium oxide, 8-10% of barium oxide, 2-4% of zinc oxide, 8-10% of sodium oxide, and the content of other components is less than 1%;
s2, uniformly mixing the raw materials, heating, melting and fully stirring to obtain molten glass, and keeping the temperature for 2-3 hours at the melting temperature of 1450-1550 ℃;
s3, performing water quenching treatment on the molten glass to form glass particles, wherein the water temperature is normal temperature during the water quenching treatment;
s4, crushing and screening the glass particles, drying the selected glass particles, and selecting the glass particles with the granularity of 10-100 meshes;
s5, paving the dried glass particles on a mold, sintering, and heating to 950-1000 ℃ at a heating rate of 5-10 ℃/min for sintering for 0.5-1 h;
s6, crystallizing the sinter, preserving heat, annealing and cooling; the crystallization process conditions are that the temperature is raised to 1100-1200 ℃ at the temperature raising speed of 5-8 ℃/min and is kept for 1-3 h; the annealing cooling process conditions are that the temperature is reduced to 700-800 ℃ at a cooling rate of 5-10 ℃/min, the temperature is preserved for 1-2 h, and the temperature is reduced to below 100 ℃ at a cooling rate of 10-15 ℃/min;
and S7, polishing and grinding the surface of the product to obtain the finished product of the microcrystalline glass.
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| CN109052967B (en) * | 2018-08-31 | 2021-08-24 | 贺州市骏鑫矿产品有限责任公司 | Method for preparing microcrystalline glass by using potassium feldspar tailings |
| CN111908796A (en) * | 2020-08-28 | 2020-11-10 | 江西鼎盛新材料科技有限公司 | Tailing slag microcrystalline glass and production method thereof |
| CN112390526B (en) * | 2020-11-17 | 2022-10-28 | 矿冶科技集团有限公司 | Method for harmlessly treating cyanided tailings in surface crystallization process of microcrystalline glass granules |
| CN113480325B (en) * | 2021-08-16 | 2023-04-07 | 苏州大学 | Building ceramsite based on fluorite tailings and preparation method thereof |
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| CN101696087A (en) * | 2009-11-12 | 2010-04-21 | 君达（凤县）环保资源无害化过程科技有限公司 | Black micro-crystalline glass plate made of gold ore tailings and manufacturing method thereof |
| CN104071983B (en) * | 2014-07-09 | 2016-06-22 | 北京璞晶科技有限公司 | A kind of sintering process method utilizing fluorite mine tailing to produce microcrystal glass plate |
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