CN108585512B - Tailing MAS series glass ceramic insulating material and preparation method thereof - Google Patents
Tailing MAS series glass ceramic insulating material and preparation method thereof Download PDFInfo
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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
- C03C10/0036—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 SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—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 SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
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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
-
- 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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- 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
- 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
- C03C4/00—Compositions for glass with special properties
Abstract
The invention discloses a MAS series glass ceramic insulating material of tailings and a preparation method thereof, which is characterized in that solid wastes such as gold tailings, molybdenum tailings and the like are taken as main raw materials, the advantage of high content of silicon element and aluminum element in the molybdenum tailings and the gold tailings is utilized, and SiO is changed by changing the content of the silicon element and the aluminum element in the gold tailings2/Al2O3The method can reduce the cost of raw materials for preparing the glass ceramic, solve the pollution of metal tailings to the environment and provide a new idea for preparing the insulating glass ceramic material by utilizing solid wastes with single components. The sapphirine and enstatite phase insulating glass ceramic prepared by the invention has the advantages of excellent electrical insulating property, small dielectric loss, stable dielectric constant, high mechanical strength, high temperature resistance and good acid and alkali resistance. Can provide reference for the application of all silicate solid wastes in the field of functional materials represented by insulating materials. Has higher social and economic benefits.
Description
Technical Field
The invention relates to an insulating material, in particular to a tailing MAS series glass ceramic insulating material and a preparation method thereof.
Background
The insulating glass ceramic is used as one of a plurality of insulating materials, on one hand, the insulating glass ceramic inherits the characteristics of wide requirements of common oxide glass ceramic on basic glass components, high hardness, high wear resistance, good chemical stability and the like, and simultaneously has the characteristics of good heat resistance, adjustable thermal expansion coefficient, high mechanical strength, good insulating property, excellent dielectric property and the like, and can be widely applied to the power industry. On the other hand, the diversification of the components and the crystalline phase of the base glass lays a solid foundation for the modification and the performance development of the insulating glass ceramic.
The glass ceramic as a polycrystalline solid material composed of a crystal phase and a glass phase has the basic performance of common glass and the polycrystalline characteristic of a ceramic material, and the performance of the glass ceramic is generally superior to that of the same kind of glass and ceramic. For example MgO-Al2O3-SiO2The (MAS) glass ceramic can be used for preparing microcrystalline glass containing crystal phases such as sapphirine, enstatite, cordierite and the like by adjusting the components of the basic glass, has good mechanical properties, and more importantly, the MAS glass ceramic contains few alkali metal ions, so that the MAS glass ceramic has excellent electrical properties (such as low dielectric loss and high insulation resistivity), and is a good material for preparing insulators. However, studies on MAS-based glass ceramics have been mainly focused on cordierite dielectric materials, and few reports have been made on these materials as insulating materials.
The metal tailings can cause great harm to human life and ecological environment, and the method for preparing the glass ceramic by utilizing the tailings is a practical and effective way, so that the raw material cost for preparing the glass ceramic can be reduced, and the environmental problem can be solved. Researchers have successfully prepared glass ceramics with pyroxene phase as the main crystal phase by using steel slag and metal tailings as main raw materials, and the glass ceramics have good mechanical properties and chemical stability. The molybdenum tailings and the gold tailings have high silicon element and aluminum element contents, and provide main components for preparing MAS series insulating glass ceramic materials. In addition, the contents of alkali metal element (K, Na), alkaline earth metal element (Ca) and Fe which are not beneficial to the insulating property are low, so that a basic condition is provided for preparing the insulating glass ceramic material by utilizing tailings, and a new idea is provided for preparing the insulating glass ceramic material by utilizing solid wastes with single components.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a MAS series glass ceramic insulating material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a tailing MAS series glass ceramic insulating material comprises the following raw materials in parts by weight: 30-60 parts of metal tailings, 2-14 parts of quartz sand, 13-25 parts of aluminum oxide, 8-16 parts of magnesium oxide, 0-10 parts of borax and 0-3 parts of sodium carbonate; and adding titanium dioxide accounting for 3-14% of the total weight of the raw materials.
The metal tailings are selected from one of gold tailings and molybdenum tailings. The quartz sand is high-purity quartz sand.
The basic glass ceramic formula comprises: SiO 22 39～51％、Al2O3 24～36％、MgO 10～14％、B2O3 0～4％、Na2O0～3％、TiO2 3～14％。
SiO in the base glass-ceramic component2/Al2O3＝1.02～2.8。
When SiO is present2/Al2O3When the crystal phase is less than 2.0, the main crystal phase of the glass ceramic insulating material is as follows: sapphirine phase.
When SiO is present2/Al2O3When the crystal phase is more than 2.0, the main crystal phases of the glass ceramic insulating material are as follows: an enstatite phase.
A preparation method of a tailing MAS series glass ceramic insulating material comprises the following steps:
(1) weighing according to the formula of the raw materials, and uniformly mixing;
(2) adding the uniformly mixed raw materials into a tank furnace or an electric furnace, heating and melting to be clear, and preparing molten glass;
(3) casting the molten glass into a preheated mould for forming, and then demoulding;
(4) annealing, nucleating and crystallizing;
(5) cooling to room temperature to obtain the final product.
The specific method of the step (2) is to add the uniformly mixed raw materials into a tank furnace or an electric furnace, heat the raw materials to 1400 ℃ and 1500 ℃, and preserve heat for 2-4h to prepare the glass liquid.
The preheating temperature in the step (3) is 500-600 ℃.
In the step (4), the annealing is carried out for 2-3h at the temperature of 500-; the nucleation is carried out for heat preservation for 1-3h at 750-820 ℃; crystallization is carried out by keeping the temperature at 850-1050 ℃ for 1-3 h.
The invention has the beneficial effects that:
1. the invention utilizes the advantage of high content of silicon element and aluminum element in molybdenum tailings and gold tailings, prepares the MAS series glass ceramic insulating material by taking the metal tailings as the main raw material, can reduce the raw material cost for preparing the insulating glass ceramic, can solve the problem of environmental pollution caused by the metal tailings, and provides a new idea for preparing the insulating glass ceramic material by utilizing solid wastes with single components.
2. The product prepared by the method has the advantages of high temperature resistance, small dielectric loss, stable dielectric constant, excellent electrical insulation, corrosion resistance, acid and alkali resistance and high mechanical strength.
3. The addition of the molybdenum tailings and the gold tailings reduces the melt viscosity, is favorable for realizing the casting molding of a complex special-shaped workpiece, and can realize the integrated production of the melting, molding, annealing, nucleating and crystallizing processes of a glass ceramic insulating device taking sapphirine and enstatite as main crystalline phases.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is an XRD pattern of MAS series glass ceramic insulating material prepared by the method of example 1.
Figure 2 is an SEM image of MAS series glass ceramic insulating material prepared by the tailing example 1 of the invention.
FIG. 3 is an XRD pattern of MAS series glass ceramic insulating material prepared by example 2 of the invention.
Figure 4 is an SEM image of MAS series glass ceramic insulating material prepared by the example 2 of the invention.
FIGS. 1 and 3 show that the glass ceramic insulating materials of examples 1 and 2 have sapphirine phase as a main crystal phase and a small amount of perovskite phase is precipitated.
FIGS. 2 and 4 show that the crystal morphology of the sapphirine phase glass ceramic insulating material is mainly rod-shaped crystal, and a certain amount of block-shaped crystal is precipitated, and the crystal size is about 250nm to 600 nm. With SiO2/Al2O3The mass ratio is increased, the short rod-shaped crystals gradually grow into rod-shaped crystals, and the crystal grain size of the block-shaped crystals finally reaches about 600nm and is arranged in a hexagonal disordered manner.
FIG. 5 is an XRD pattern of MAS series glass ceramic insulating material prepared by example 3 of the invention.
Figure 6 is an SEM image of MAS series glass ceramic insulating material prepared by the example 3 of the invention.
FIG. 7 is an XRD pattern of MAS series glass ceramic insulating material prepared by example 4 of the invention.
Figure 8 is an SEM image of MAS series glass ceramic insulating material prepared by the example 5 of the invention.
FIGS. 5 and 7 show that the main crystal phase of the glass ceramic insulating materials of examples 3 and 4 is enstatite phase, and a small amount of magnetite phase is precipitated.
FIGS. 6 and 8 show that with SiO2/Al2O3The mass ratio is increased, the appearance of the enstatite crystal is gradually changed into dendritic crystal from granular crystal, the size of the crystal grain is about 0.3 mu m, the crystal grains are arranged in a staggered interlocking mode, and the gaps among the crystal grains are small.
Detailed Description
The following examples further illustrate the embodiments of the present invention in detail.
The main chemical components of the raw materials of the gold tailings and the molybdenum tailings are shown in the table 1.
Table 1 main chemical composition (wt.%) of raw gold and molybdenum tailings of the present invention
Example 1
TABLE 2 chemical composition of inner Mongolia gold tailings (wt.%)
A tailing MAS series glass ceramic insulating material comprises the following raw materials in parts by weight: 49.7 parts of inner Mongolia gold tailings, 5.2 parts of quartz sand, 22.7 parts of aluminum oxide, 8.6 parts of magnesium oxide, 7.1 parts of borax and 6.6 parts of titanium dioxide; SiO 22/Al2O3＝1.27。
SiO2/Al2O3The calculating method of (2):
SiO2: 49.7 (gold tailing part) × 59.4% (SiO)2Content) +5.2 (SiO added)234.72 parts
Al2O3: 49.7 (gold tailing portion) × 9.33% (Al)2O3Content) +22.7 (added Al)2O3Number of shares) ═ 27.33
SiO2/Al2O3＝34.72/27.33＝1.27
The preparation method comprises the following steps:
(1) weighing according to the formula of the raw materials, and uniformly mixing;
(2) adding the uniformly mixed raw materials into an electric furnace, heating to 1400 ℃, preserving heat for 4 hours, melting and clarifying to obtain glass liquid;
(3) casting the molten glass into a mold preheated to 500 ℃ for molding, and then demolding;
(4) putting the demoulded sample into an electric furnace, and keeping the temperature for 3 hours at 500 ℃ for annealing; keeping the temperature at 750 ℃ for 2h for nucleation; keeping the temperature at 880 ℃ for 2h, and crystallizing;
(5) naturally cooling to room temperature in an electric furnace to obtain the MAS glass ceramic insulating material, wherein the main crystal phase is a sapphirine phase.
The XRD pattern and the SEM pattern of the MAS series glass ceramic insulating material prepared by the embodiment are shown in figure 1 and figure 2.
Example 2
TABLE 3 main chemical composition (wt.%) of inner Mongolia molybdenum tailings
A tailing MAS series glass ceramic insulating material comprises the following raw materials in parts by weight: 40.9 parts of inner Mongolia molybdenum tailings, 7.7 parts of quartz sand, 20.2 parts of aluminum oxide, 8.6 parts of magnesium oxide, 7.1 parts of borax and 6.6 parts of titanium dioxide; SiO 22/Al2O3＝1.42。
The preparation method comprises the following steps:
(1) weighing according to the formula of the raw materials, and uniformly mixing;
(2) adding the uniformly mixed raw materials into an electric furnace, heating to 1400 ℃, preserving heat for 2 hours, melting and clarifying to obtain glass liquid;
(3) casting the molten glass into a mold preheated to 550 ℃ for molding, and then demolding;
(4) placing the demoulded sample into an electric furnace, preserving heat for 2 hours at 550 ℃, and annealing; keeping the temperature at 800 ℃ for 1h for nucleation; keeping the temperature at 920 ℃ for 2h for crystallization;
(5) naturally cooling to room temperature in an electric furnace to obtain the MAS glass ceramic insulating material, wherein the main crystal phase is a sapphirine phase.
The XRD pattern and the SEM pattern of the MAS series glass ceramic insulating material prepared by the embodiment are shown in figure 3 and figure 4 respectively.
Example 3
A MAS series glass-ceramic insulating material is prepared from the following raw materials (by weight portion)Material preparation: 54.8 parts of inner Mongolia gold tailings, 11.3 parts of quartz sand, 15 parts of aluminum oxide, 13.2 parts of magnesium oxide, 2 parts of soda ash and 3.7 parts of titanium dioxide; SiO 22/Al2O3＝2.39。
The preparation method comprises the following steps:
(1) weighing according to the formula of the raw materials, and uniformly mixing;
(2) adding the uniformly mixed raw materials into an electric furnace, heating to 1450 ℃, preserving heat for 3 hours, melting and clarifying to obtain glass liquid;
(3) casting the molten glass into a mold preheated to 550 ℃ for molding, and then demolding;
(4) putting the demoulded sample into an electric furnace, preserving heat for 3 hours at 550 ℃, and annealing; keeping the temperature at 820 ℃ for 1h for nucleation; keeping the temperature at 950 ℃ for 3h, and crystallizing;
(5) naturally cooling to room temperature in an electric furnace to obtain the MAS series glass ceramic insulating material, wherein the main crystal phase is as follows: an enstatite phase.
The XRD pattern and the SEM pattern of the MAS series glass ceramic insulating material prepared by the embodiment are shown in figure 5 and figure 6.
Example 4
A tailing MAS series glass ceramic insulating material comprises the following raw materials in parts by weight: 56.2 parts of inner Mongolia molybdenum tailings, 11.3 parts of quartz sand, 13.2 parts of aluminum oxide, 13.2 parts of magnesium oxide, 2 parts of soda ash and 3.7 parts of titanium dioxide; SiO 22/Al2O3＝2.44。
The preparation method comprises the following steps:
(1) weighing according to the formula of the raw materials, and uniformly mixing;
(2) adding the uniformly mixed raw materials into an electric furnace, heating to 1450 ℃, preserving heat for 3 hours, melting and clarifying to obtain glass liquid;
(3) casting the molten glass into a mold preheated to 600 ℃ for molding, and then demolding;
(4) placing the demoulded sample into an electric furnace, and keeping the temperature for 2 hours at 600 ℃ for annealing; keeping the temperature at 800 ℃ for 2h for nucleation; keeping the temperature at 980 ℃ for 2h, and crystallizing;
(5) naturally cooling to room temperature in an electric furnace to obtain the MAS series glass ceramic insulating material, wherein the main crystal phase is as follows: an enstatite phase.
The XRD pattern and the SEM pattern of the MAS series glass ceramic insulating material prepared by the embodiment are shown in figure 7 and figure 8 respectively.
Performance analysis:
1. product performance detection
The properties of MAS series glass ceramic insulating materials of the tailings of examples 1 to 4 were examined and compared with aluminum porcelain (GB/T8411.3-2009 ceramic and glass insulating material part 3: material properties), and the results are shown in tables 4 and 5.
TABLE 4 mechanical and physicochemical properties of the product
The results in Table 4 show that the MAS series glass ceramic insulating material prepared by using the metal tailings as the main raw material has the advantages of high bending strength, small thermal expansion coefficient, good acid and alkali resistance and the like, has physical and chemical properties superior to various indexes of aluminum ceramics, and can meet the use requirements of the insulating material.
TABLE 5 Electrical Properties of the products
The results in Table 5 show that the MAS series glass ceramic insulating material prepared by using the metal tailings as the main raw material has the advantages of high volume resistivity, low dielectric loss, excellent high-temperature performance and the like, the electrical performance is superior to various indexes of aluminum ceramics, and the use requirement of the insulating material can be met.
The foregoing description is only a preferred embodiment of the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The MAS series glass ceramic insulating material is characterized by comprising the following raw materials in parts by weight: 30-60 parts of metal tailings, 2-14 parts of quartz sand, 13-25 parts of aluminum oxide, 8-16 parts of magnesium oxide, 0-10 parts of borax and 0-3 parts of sodium carbonate; adding titanium dioxide accounting for 3-14% of the total weight of the raw materials; the metal tailings are selected from one of gold tailings and molybdenum tailings; SiO in the base glass-ceramic component2/Al2O31.02-2.8; SiO in the base glass-ceramic component2/Al2O3When the crystal phase is less than 2.0, the main crystal phase of the glass ceramic insulating material is as follows: sapphirine phase; SiO in the base glass-ceramic component2/Al2O3When the crystal phase is more than 2.0, the main crystal phases of the glass ceramic insulating material are as follows: an enstatite phase.
2. The preparation method of the tailing MAS series glass ceramic insulating material as claimed in claim 1, which is characterized by comprising the following steps:
(1) weighing according to the formula of the raw materials, and uniformly mixing;
(2) adding the uniformly mixed raw materials into a tank furnace or an electric furnace, heating and melting to be clear, and preparing molten glass;
(3) casting the molten glass into a preheated mould for forming, and then demoulding;
(4) annealing, nucleating and crystallizing;
(5) cooling to room temperature to obtain the final product.
3. The preparation method of MAS series glass ceramic insulating material as claimed in claim 2, wherein the step (2) comprises charging the uniformly mixed raw materials into a tank furnace or an electric furnace, heating to 1400 ℃ and 1500 ℃, and maintaining the temperature for 2-4h to obtain molten glass.
4. The method for preparing MAS series glass ceramic insulating material as claimed in claim 2, wherein the preheating temperature in step (3) is 500-600 ℃.
5. The preparation method of the MAS system glass ceramic insulating material as claimed in claim 2, wherein the annealing in the step (4) is carried out at 500-600 ℃ for 2-3 h; the nucleation is carried out for heat preservation for 1-3h at 750-820 ℃; crystallization is carried out by keeping the temperature at 850-1050 ℃ for 1-3 h.
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| CN101734857A (en) * | 2009-12-30 | 2010-06-16 | 陕西乾盛环保建材工程有限公司 | Method for manufacturing black microcrystalline glass plates from molybdenum tailings |
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| CN107580590A (en) * | 2015-03-09 | 2018-01-12 | 法商圣高拜欧洲实验及研究中心 | For repairing the unformed product of glass-melting furnace |
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| JP3346693B2 (en) * | 1995-11-24 | 2002-11-18 | 京セラ株式会社 | Glass-ceramic sintered body and wiring board using the same |
| CN1246463A (en) * | 1998-09-02 | 2000-03-08 | 东北大学钎具开发研究中心 | Process for preparing microcrystalline glass insulator and its products |
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